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Sample records for surfactant-enhanced emulsification microextraction

  1. Ultrasound-assisted surfactant-enhanced emulsification microextraction for the determination of Cd and Ni in tea and water samples.

    PubMed

    Ezoddin, Maryam; Taghizadeh, Tayebeh; Majidi, Behrooz

    2014-01-01

    A microextraction method based on ultrasound-assisted surfactant-enhanced emulsification using solidification of a floating organic droplet (UASEME-SFO) was evaluated for simultaneous determination of Cd and Ni in water and tea samples followed by flame atomic absorption spectrometry. In the UASEME-SFO technique, Triton X-100 was used as an emulsifier to accelerate the emulsification of the extraction solvent into a sample solution and hasten the mass transfer of the analytes. Analytes form a complex and are extracted into 1-dodecanol which was used as an extraction solvent. Some parameters such as type and volume of the extraction solvent, the type and concentration of the surfactant, ultrasound extraction time, reagent concentration, centrifuge conditions and salt concentration were investigated. Under optimum conditions, calibration curves were linear in the range of 0.3-100 and 0.6-180 microg L(-1) with detection limits of 0.11 and 0.20 microg L(-1) for Cd and Ni, respectively. The accuracy of the method was confirmed by parallel analyses using the certified reference material of water and tea samples. The recoveries of the analytes in tea leaves, tea infusions and water samples were in the range of 96.5-105.1%. PMID:25145194

  2. Rapid screening of five phthalate esters from beverages by ultrasound-assisted surfactant-enhanced emulsification microextraction coupled with gas chromatography.

    PubMed

    Yan, Hongyuan; Cheng, Xiaoling; Yan, Kuo

    2012-10-21

    A rapid ultrasound-assisted surfactant-enhanced emulsification microextraction (UASEME) method coupled with gas chromatography-flame ionization detection (GC-FID) is proposed for the rapid screening of five phthalate esters in bottled beverages. In the UASEME procedure, a nonionic surfactant (Triton X-100) was used as the emulsifier, without application of any organic dispersive solvents typically required in dispersive liquid-liquid microextraction. Triton X-100 as the emulsifier accelerated the formation of fine droplets from the extraction solvent in the sample solution under ultrasound radiation, thus combining the advantages of dispersive liquid-liquid microextraction (DLLME) and ultrasound-assisted emulsification microextraction (UAEME). Under the optimum conditions, the enrichment factors of the five analytes ranged from 230 to 288 fold and the recoveries ranged from 89.3% to 100.1%. The limits of detection (LODs) based on signal to noise of 3 were 0.41-0.79 μg L(-1). Intra-assay and inter-assay precision, expressed as the relative standard deviation (RSD), were ≤5.46% and 5.81%, respectively. The proposed UASEME-GC/FID method was demonstrated to be simple, practical and environmentally friendly for the determination of trace phthalate esters in beverage samples. PMID:22932997

  3. Vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction for the determination of carbamates in juices by micellar electrokinetic chromatography tandem mass spectrometry.

    PubMed

    Moreno-González, David; Huertas-Pérez, José F; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2015-07-01

    A new method based on vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction has been developed for the extraction of carbamate pesticides in juice samples prior to their determination by micellar electrokinetic chromatography coupled to tandem mass spectrometry. This sample treatment allowed the satisfactory extraction and the extract clean-up of 25 carbamates from different fruit and vegetal juices (banana, tomato, and peach). In this study, the addition of ammonium perfluorooctanoate in the aqueous sample in combination with vortex agitation, provided very clean extracts with short extraction times. Under optimized conditions, recoveries of the proposed method for these pesticides from fortified juice samples ranged from 81% to 104%, with relative standard deviations lower than 15%. Limits of quantification were between 2.3µgkg(-)(1) and 4.7µgkg(-)(1), showing the high sensitivity of this fast and simple method. PMID:25882424

  4. Vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction for the determination of triazine herbicides in water samples by microemulsion electrokinetic chromatography.

    PubMed

    Li, Ran-Hong; Liu, Dong-Hui; Yang, Zhong-Hua; Zhou, Zhi-Qiang; Wang, Peng

    2012-07-01

    A novel method based on the combination of microemulsion electrokinetic chromatography (MEEKC) and vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction (VSLLME) was developed for the determination of five triazine herbicides (simazine, atrazine, ametryn, prometryn, and terbutryn) in water samples. The five triazine herbicides were baseline separated by using the microemulsion buffer containing a 10 mmol/L borate buffer at pH 9.5, 2.5% (w/v) SDS as surfactant, 0.8% (w/v) ethyl acetate as oil phase, and 6.0% (w/v) 1-butanol as cosurfactant. The optimum extraction conditions of VSLLME were as follows: 100 μL chloroform was used as extraction solvent, 5.0 × 10⁻⁵ mol/L Tween-20 was chosen as the surfactant to enhance the emulsification, and the extraction process was carried out by vortex mixing for 3 min. Under these optimum experimental conditions, the calibration curve was linear in the range of 2.0-200.0 ng/mL, with the correlation coefficients (r²) varying from 0.9927 to 0.9958. The detection limits of the method varied from 0.41 to 0.62 ng/mL. The purposed method was applied to the determination of five triazine herbicides in real water samples, and the recoveries were between 80.6 and 107.3%. PMID:22821495

  5. Vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction of biogenic amines in fermented foods before their simultaneous analysis by high-performance liquid chromatography.

    PubMed

    Donthuan, Jaruwan; Yunchalard, Sirinda; Srijaranai, Supalax

    2014-11-01

    A simple, rapid, sensitive, and environmentally friendly method, based on modified dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography was developed for the simultaneous determination of five biogenic amines in fermented food samples. Biogenic amines were derivatized with 9-fluorenylmethyl chloroformate, extracted by vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction, and then analyzed by high-performance liquid chromatography. Five biogenic amine compounds were separated within 30 min using a C18 column and gradient elution with acetonitrile and 1% acetic acid. Factors influencing the derivatization and extraction efficiency such as type and volume of extraction solvent, type, and concentration of surfactant, pH, salt addition, and vortex time were optimized. Under the optimum conditions, the method provided the enrichment factors in the range of 161-553. Good linearity was obtained from 0.002-0.5 mg/L for cadaverine and tyramine, 0.003-1 mg/L for tryptamine and histamine, and 0.005-1 mg/L for spermidine with coefficient of determination (R(2) ) > 0.992. The limits of detection ranged from 0.0010 to 0.0026 mg/L. The proposed method was successfully applied to analysis of biogenic amines in fermented foods such as fermented fish (plaa-som), wine and beer where good recoveries were obtained in the range of 83.2-112.5% PMID:25142110

  6. Ionic-liquid-based, manual-shaking- and ultrasound-assisted, surfactant-enhanced emulsification microextraction for the determination of three fungicide residues in juice samples.

    PubMed

    Chen, Xiaochu; You, Xiangwei; Liu, Fengmao; Hou, Fan; Zhang, Xu

    2015-01-01

    A novel manual-shaking- and ultrasound-assisted surfactant-enhanced emulsification microextraction method was developed for the determination of three fungicides in juice samples. In this method, the ionic liquid, 1-ethyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide, instead of a volatile organic solvent was used as the extraction solvent. The surfactant, NP-10, was used as an emulsifier to enhance the dispersion of the water-immiscible ionic liquid into an aqueous phase, which accelerated the mass transfer of the analytes. Organic dispersive solvent typically required in common dispersive liquid-liquid microextraction methods was not necessary. In addition, manual shaking for 15 s before ultrasound to preliminarily mix the extraction solvent and the aqueous sample could greatly shorten the time for dispersing the ionic liquid into aqueous solution by ultrasound irradiation. Several experimental parameters affecting the extraction efficiency, including type and volume of extraction solvent, type and concentration of surfactant, extraction time, and pH, were optimized. Under the optimized conditions, good linearity with the correlation coefficients (γ) higher than 0.9986 and high sensitivity with the limit of detection ranging from 0.4 to 1.6 μg/L were obtained. The average recoveries ranged from 61.4 to 86.0% for spiked juice, with relative standard deviations from 1.8 to 9.7%. The proposed method was demonstrated to be a simple, fast, and efficient method for the analysis of the target fungicides in juice samples. PMID:25394281

  7. Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop combined with high performance liquid chromatography for determination of naproxen and nabumetone.

    PubMed

    Asadi, Mohammad; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Bijan

    2015-12-18

    A novel, rapid, simple and green vortex-assisted surfactant-enhanced emulsification microextraction method based on solidification of floating organic drop was developed for simultaneous separation/preconcentration and determination of ultra trace amounts of naproxen and nabumetone with high performance liquid chromatography-fluorescence detection. Some parameters influencing the extraction efficiency of analytes such as type and volume of extractant, type and concentration of surfactant, sample pH, KCl concentration, sample volume, and vortex time were investigated and optimized. Under optimal conditions, the calibration graph exhibited linearity in the range of 3.0-300.0ngL(-1) for naproxen and 7.0-300.0ngL(-1) for nabumetone with a good coefficient of determination (R(2)>0.999). The limits of detection were 0.9 and 2.1ngL(-1). The relative standard deviations for inter- and intra-day assays were in the range of 5.8-10.1% and 3.8-6.1%, respectively. The method was applied to the determination of naproxen and nabumetone in urine, water, wastewater and milk samples and the accuracy was evaluated through recovery experiments. PMID:26627589

  8. Determination of Lead in Water Samples Using a New Vortex-Assisted, Surfactant-Enhanced Emulsification Liquid-Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry.

    PubMed

    Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Pan, Weiliang; Tang, Xiaohui; Zhou, Guangming; Mao, Yufeng; Su, Xaioxuan

    2016-04-01

    A low toxic solvent-based vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction (LT-VSLLME) combined with graphite furnace atomic absorption spectrometry was developed for the extraction and determination of lead (Pb) in water samples. In the LT-VSLLME method, the extraction solvent was dispersed into the aqueous samples by the assistance of vortex agitator. Meanwhile, the addition of a surfactant, which acted as an emulsifier, could enhance the speed of the mass-transfer from aqueous samples to the extraction solvent. The influences of analytical parameters, including extraction solvent type and its volume, surfactant type and its volume, pH, concentration of chelating agent, salt effect and extraction time were investigated. Under the optimized conditions, a good relative standard deviation of 3.69% at 10 ng L(-1) was obtained. The calibration graph showed a linear pattern in the ranges of 5-30 ngL(-1), with a limit of detection of 0.76 ng L(-1). The linearity was obtained by five points in the concentration range of 5-30 ngL(-1). The enrichment factor was 320. The procedure was applied to wastewater and river water, and the accuracy was assessed through the analysis of the recovery experiments. PMID:26614355

  9. Vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction with solidification of floating organic droplet combined with HPLC for the determination of neonicotinoid pesticides.

    PubMed

    Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax

    2013-12-15

    A microextraction procedure based on vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction with solidification of floating organic droplet (VSLLME-SFO) for preconcentration of neonicotinoid pesticides, including acetamiprid, clotianidin, nitenpyram, imidacloprid, and thiamethoxam, has been developed. In VSLLME-SFO process, the addition of surfactant (as an emulsifier), could be enhance the mass-transfer from the aqueous solution into the extraction solvent. The extraction solvent could be dispersed into the aqueous by vortex process. Other experimental parameters affected the extraction efficiency, including the kind and concentration of salt, concentration and volume of HCl, kind and concentration of surfactant and its volume, kind and volume of extraction solvent, vortex time and the centrifugation extraction time, were also optimized. The optimum extraction conditions of VSLLME-SFO were 10.00 mL of sample, 0.3% (w/v) Na2SO4, 50 µL of 0.050 mol L(-1) SDS, 1.0 mol L(-1) HCl (400 µL), 150 µL of octanol, vortex time 1 min and centrifugation time 10 min. The sediment phase was analyzed by subjecting it to HPLC using a mobile phase of 25% acetonitrile in water, at a flow rate of 1.0 mL min(-1), and photodiode array detection at 254 nm. Under the optimum extraction conditions, high enrichment factors (20-100 fold) and low limit of detection (0.1-0.5 μg L(-1)) could be obtained. This method provided high sensitivity, low toxic organic solvents used, and simplicity of the extraction processes. The proposed method was successfully applied in the analysis of neonicotinoids in fruit juice and water samples. PMID:24209333

  10. Vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction with solidification of floating organic droplet combined with flame atomic absorption spectrometry for the fast determination of cadmium in water samples.

    PubMed

    Peng, Guilong; Lu, Ying; He, Qiang; Mmereki, Daniel; Tang, Xiaohui; Zhong, Zhihui; Zhao, Xiaolong

    2016-01-01

    A novel vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction with solidification of floating organic droplet (VSLLME-SFO) was developed for the fast, simple and efficient determination of cadmium (Cd) in water samples followed by flame atomic absorption spectrometry (FAAS). In the VSLLME-SFO process, the addition of surfactant (as an emulsifier), could enhance the mass transfer from the aqueous solution into the extraction solvent. The extraction solvent could be dispersed into the aqueous phase under vigorous shaking with the vortex. In this paper, we investigated the influences of analytical parameters, including pH, extraction solvent type and its volume, surfactant type and its volume, concentration of chelating agent, salt effect and vortex time, on the extraction efficiency of Cd. Under the optimized conditions, the limit of detection was 0.16 μg/L. The analyte enrichment factor was 37.68. The relative standard deviation was 3.2% (10 μg/L, n = 10) and the calibration graph was linear, ranging from 0.5 to 30 μg/L. The proposed method was successfully applied for the analysis of ultra-trace Cd in river water and wastewater samples. PMID:27232416

  11. Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop followed by electrothermal atomic absorption spectrometry for speciation of antimony (ΙΙΙ, V).

    PubMed

    Eftekhari, Mohammad; Chamsaz, Mahmoud; Arbab-Zavar, Mohammad Hossein; Eftekhari, Ali

    2015-01-01

    Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop (VASEME-SFO) was used for preconcentration and speciation of antimony (ΙΙΙ, V) followed by electrothermal atomic absorption spectrometry (ETAAS). In this procedure, Triton X-114 was used as emulsifier and 1-undecanol was used as extraction solvent. This method is based on the complexation of Sb(ΙΙΙ) with dithizone (as complexing agent) at pH 2 and extraction of the resulting hydrophobic complex into the extraction solvent (1-undecanol) with vortex-assisted liquid phase microextraction, whereas Sb(V) remained in solution. Sb(ΙΙΙ) in extraction solvent was directly analyzed by ETAAS after dilution with ethanol, and Sb(V) was calculated by subtracting Sb(ΙΙΙ) from the total antimony after reducing Sb(V) to Sb(ΙΙΙ) by L-cysteine. Under the optimized condition, the calibration curve was linear in the range of 0.4-8 μg L(-1) of Sb(ΙΙΙ) with a correlation coefficient of 0.9995. The detection limit based on three times of the standard deviation of the blank (n = 8) was 0.09 μg L(-1). The validation and the recovery of the proposed method were performed by the analysis of a certified reference material and spike method. The obtained results were in very good agreements with certified values. The proposed method was successfully applied for the determination of antimony species at trace levels in different water samples. PMID:25404541

  12. Ultrasound-assisted surfactant-enhanced emulsification microextraction based on the solidification of a floating organic droplet used for the simultaneous determination of six fungicide residues in juices and red wine.

    PubMed

    You, Xiangwei; Wang, Suli; Liu, Fengmao; Shi, Kaiwei

    2013-07-26

    A novel ultrasound-assisted surfactant-enhanced emulsification microextraction technique based on the solidification of a floating organic droplet followed by high performance liquid chromatography with diode array detection was developed for simultaneous determination of six fungicide residues in juices and red wine samples. The low-toxicity solvent, 1-dodecanol, was used as an extraction solvent. For its low density and proper melting point near room temperature, the extractant droplet was collected easily by solidifying it at a low temperature. The surfactant, Tween 80, was used as an emulsifier to enhance the dispersion of the water-immiscible extraction solvent into an aqueous phase, which hastened the mass-transfer of the analytes. Organic dispersive solvent typically required in common dispersive liquid-liquid microextraction methods was not used in the proposed method. Some parameters (e.g., the type and volume of extraction solvent, the type and concentration of surfactant, ultrasound extraction time, salt addition, and volume of samples) that affect the extraction efficiency were optimized. The proposed method showed a good linearity within the range of 5μgL(-1)-1000μgL(-1), with the correlation coefficients (γ) higher than 0.9969. The limits of detection for the method ranged from 0.4μgL(-1) to 1.4μgL(-1). Further, this simple, practical, sensitive, and environmentally friendly method was successfully applied to determine the target fungicides in juice and red wine samples. The recoveries of the target fungicides in red wine and fruit juice samples were 79.5%-113.4%, with relative standard deviations that ranged from 0.4% to 12.3%. PMID:23473514

  13. Comparison of air-agitated liquid-liquid microextraction and ultrasound-assisted emulsification microextraction for polycyclic aromatic hydrocarbons determination in hookah water.

    PubMed

    Rajabi, Maryam; Bazregar, Mohammad; Daneshfar, Ali; Asghari, Alireza

    2015-07-01

    In this work, two disperser-free microextraction methods, namely, air-agitated liquid-liquid microextraction and ultrasound-assisted emulsification microextraction are compared for the determination of a number of polycyclic aromatic hydrocarbons in aqueous samples, followed by gas chromatography with flame ionization detection. The effects of various experimental parameters upon the extraction efficiencies of both methods are investigated. Under the optimal conditions, the enrichment factors and limits of detection were found to be in the ranges of 327-773 and 0.015-0.05 ng/mL for air-agitated liquid-liquid microextraction and 406-670 and 0.015-0.05 ng/mL for ultrasound-assisted emulsification microextraction, respectively. The linear dynamic ranges and extraction recoveries were obtained to be in the range of 0.05-120 ng/mL (R(2) ≥ 0.995) and 33-77% for air-agitated liquid-liquid microextraction and 0.05-110 ng/mL (R(2) ≥ 0.994) and 41-67% for ultrasound-assisted emulsification microextraction, respectively. To investigate this common view among some people that smoking hookah is healthy due to the passage of smoke through the hookah water, samples of both the hookah water and hookah smoke were analyzed. PMID:25989415

  14. Ultrasound-assisted emulsification-microextraction for the determination of phenolic compounds in olive oils.

    PubMed

    Reboredo-Rodríguez, P; Rey-Salgueiro, L; Regueiro, J; González-Barreiro, C; Cancho-Grande, B; Simal-Gándara, J

    2014-05-01

    A reliable, sensitive and effective method based on ultrasound-assisted emulsification-microextraction (USAEME) coupled to HPLC-DAD has been developed to identify and quantify several target phenolic compounds from extra virgin olive oils (EVOO). This approach is based on the emulsification of a microvolume of polar organic extractant in a non-polar liquid sample by ultrasound radiation and further separation of both liquid phases by centrifugation. The percentage of methanol/water (v/v) in the extractant, the volume of extractant, and the extraction time as three effective parameters on the extraction were optimised by a central composite design (Box-Behnken response surface) method. The optimised method presented recoveries in EVOO between 91% and 115% for the target analytes (except vanillin with 65%) and a satisfactory precision with relative standard deviations (RSD%) lower than 8.4% for repeatability and reproducibility. The method showed good linearity and limits of detection and quantification were in the range 0.001-0.14 and 0.004-0.47mg/kg, respectively. After method validation, it was successfully applied to the analysis of three EVOO samples. All target compounds were detected in all analysed samples. Tyrosol and hydroxytyrosol were the major phenolic compounds, followed by pinoresinol and luteolin. PMID:24360429

  15. Determination of melamine in soil samples using surfactant-enhanced hollow fiber liquid phase microextraction followed by HPLC–UV using experimental design

    PubMed Central

    Sarafraz Yazdi, Ali; Raouf Yazdinezhad, Samaneh; Heidari, Tahereh

    2014-01-01

    Surfactant-enhanced hollow fiber liquid phase (SE-HF-LPME) microextraction was applied for the extraction of melamine in conjunction with high performance liquid chromatography with UV detection (HPLC–UV). Sodium dodecyl sulfate (SDS) was added firstly to the sample solution at pH 1.9 to form hydrophobic ion-pair with protonated melamine. Then the protonated melamine–dodecyl sulfate ion-pair (Mel–DS) was extracted from aqueous phase into organic phase immobilized in the pores and lumen of the hollow fiber. After extraction, the analyte-enriched 1-octanol was withdrawn into the syringe and injected into the HPLC. Preliminary, one variable at a time method was applied to select the type of extraction solvent. Then, in screening step, the other variables that may affect the extraction efficiency of the analyte were studied using a fractional factorial design. In the next step, a central composite design was applied for optimization of the significant factors having positive effects on extraction efficiency. The optimum operational conditions included: sample volume, 5 mL; surfactant concentration, 1.5 mM; pH 1.9; stirring rate, 1500 rpm and extraction time, 60 min. Using the optimum conditions, the method was analytically evaluated. The detection limit, relative standard deviation and linear range were 0.005 μg mL−1, 4.0% (3 μg mL−1, n = 5) and 0.01–8 μg mL−1, respectively. The performance of the procedure in extraction of melamine from the soil samples was good according to its relative recoveries in different spiking levels (95–109%). PMID:26644934

  16. A new coupling of spectrophotometric determination with ultrasound-assisted emulsification dispersive liquid-liquid microextraction of trace silver.

    PubMed

    Wen, Xiaodong; Kong, Lamei; Chen, Meihui; Deng, Qingwen; Zhao, Xia; Guo, Jie

    2012-11-01

    In this work, a new coupling of spectrophotometric determination with preconcentration method named as ultrasound-assisted emulsification dispersive liquid-liquid microextraction (UAE-DLLME) for trace silver was firstly established. Disperser solvent in traditional DLLME was substituted by ultrasound-assisted emulsification, which could afford more effective emulsification and make the extraction method greener. The extraction was accomplished efficiently in only 3 min during ultrasound-assisted emulsification. Compared to traditional DLLME, the established pretreatment was simpler, greener and more effective. The UAE-DLLME technique was effectively coupled with ordinary spectrophotometer to improve the analytical performance and expand the application of spectrophotometric determination. The factors influencing UAE-DLLME, such as concentration of chelating agent, kind and volume of extractant, pH, conditions of phase separation, ultrasound extraction time and instrumental conditions, were studied in detail. Under the optimal conditions, the limit of detection (LOD) for silver was 0.45 μg L(-1), with sensitivity enhancement factor (EF) of 35. The established method was applied to the determination of trace silver in real and certified reference samples with satisfactory analytical results. PMID:22902575

  17. A new coupling of spectrophotometric determination with ultrasound-assisted emulsification dispersive liquid-liquid microextraction of trace silver

    NASA Astrophysics Data System (ADS)

    Wen, Xiaodong; Kong, Lamei; Chen, Meihui; Deng, Qingwen; Zhao, Xia; Guo, Jie

    2012-11-01

    In this work, a new coupling of spectrophotometric determination with preconcentration method named as ultrasound-assisted emulsification dispersive liquid-liquid microextraction (UAE-DLLME) for trace silver was firstly established. Disperser solvent in traditional DLLME was substituted by ultrasound-assisted emulsification, which could afford more effective emulsification and make the extraction method greener. The extraction was accomplished efficiently in only 3 min during ultrasound-assisted emulsification. Compared to traditional DLLME, the established pretreatment was simpler, greener and more effective. The UAE-DLLME technique was effectively coupled with ordinary spectrophotometer to improve the analytical performance and expand the application of spectrophotometric determination. The factors influencing UAE-DLLME, such as concentration of chelating agent, kind and volume of extractant, pH, conditions of phase separation, ultrasound extraction time and instrumental conditions, were studied in detail. Under the optimal conditions, the limit of detection (LOD) for silver was 0.45 μg L-1, with sensitivity enhancement factor (EF) of 35. The established method was applied to the determination of trace silver in real and certified reference samples with satisfactory analytical results.

  18. Novel coupling of surfactant assisted emulsification dispersive liquid-liquid microextraction with spectrophotometric determination for ultra trace nickel

    NASA Astrophysics Data System (ADS)

    Deng, Qingwen; Chen, Meihui; Kong, Lamei; Zhao, Xia; Guo, Jie; Wen, Xiaodong

    2013-03-01

    In this work, dispersive liquid-liquid microextraction (DLLME) was improved and the preconcentration method named as surfactant assisted emulsification dispersive liquid-liquid microextraction (SAE-DLLME) was established for ultra trace nickel preconcentration and spectrophotometric determination. Non-ionic surfactant Triton X-100 (TX-100) was used as emulsifier and Triton X-114 (TX-114) was investigated as comparison. Disperser solvent was substituted by surfactant, which could afford more effective emulsification and make the extraction relatively greener. The extraction was accomplished efficiently in only 1 min during manual shaking. Compared to traditional DLLME, the developed SAE-DLLME pretreatment was simple, rapid and effective. The improved extraction technique was firstly coupled with traditional spectrophotometer to improve the analytical performance and expand the application of spectrophotometric determination. The influence factors relevant to SAE-DLLME including extraction parameters and instrumental conditions, were studied in detail. Under the optimal conditions, the limit of detection (LOD) for nickel was 0.24 μg L-1, with sensitivity enhancement factor (EF) of 23.

  19. Development of ultrasound-assisted emulsification microextraction for determination of thiocynate ion in human urine and saliva samples.

    PubMed

    Hashemi, Mahdi; Daryanavard, Seyed Mosayeb; Abdolhosseini, Sana

    2013-02-15

    Ultrasound-assisted emulsification microextraction (USAE-ME) procedure coupled with UV-vis spectrophotometric measurement has been developed for determination of thiocyanate ion (SCN(-)) in water and biological fluids samples. The method is based on protonation of SCN(-) ions in acidic medium and extraction of thiocyanic acid into fine droplets of chloroform as an extraction solvent contains rhodamine B (RhB). The RhB was protonated in presence of thiocynanic acid to form highly colored ion-pair complex of [thiocynate][RhBH(+)] in chloroform, which used for subsequent spectrophotometric determination of SCN(-) ions. Experimental parameters for both spectrophotometric reaction and USAE-ME procedure have been optimized. Under optimized conditions the calibration curve for SCN(-) showed good linearity in the range of 38.0-870.0ngmL(-1) (R(2)=0.9967). The limit of detection (S/N=3) and preconcentration factor were 5.0ngmL(-1) and 40, respectively. Relative standard deviation for determination of 200ngmL(-1) of SCN(-) was 2.8% (n=5). The proposed method has been successfully applied for determination of SCN(-) ion in tap water, mineral bottled water and human saliva and urine samples with an average recovery of 99.2%. PMID:23353810

  20. Development of ultrasound-assisted emulsification microextraction based on solidification of a floating organic droplet for determination of organochlorine pesticides in water samples.

    PubMed

    Shu, Bin; Yang, Zhaoguang; Lee, Hsiaowan; Qiu, Bo; Li, Haipu

    2016-02-01

    An ultrasound-assisted emulsification microextraction based on the solidification of a floating organic droplet followed by gas chromatography with electron capture detection was developed for the simultaneous determination of 13 organochlorine pesticides in water samples. In the proposed method, ultrasound was applied to achieve the emulsification without addition of any dispersive solvent. In consequence, the volume of extraction phase remained unaffected by the ion strength of aqueous phase and high extraction recoveries were obtained. It was also found that dilution of the floating phase with acetone was necessary for preventing peak splitting in chromatogram. Under optimal conditions, the proposed method provided good sensitivity (the detection limits of organochlorine pesticides ranged from 1.3 to 3.9 ng/L) and good repeatability of extraction (below 6.5%, n = 5). The recoveries in reservoir and river water samples were between 75.8% and 96.9%. PMID:26631905

  1. Ionic liquid-based ultrasound-assisted emulsification microextraction coupled with high performance liquid chromatography for the determination of four fungicides in environmental water samples.

    PubMed

    Liang, Pei; Wang, Fang; Wan, Qin

    2013-02-15

    A highly efficient and environmentally friendly sample preparation method termed ionic liquid-based ultrasound-assisted emulsification microextraction (IL-USAEME) combined with high performance liquid chromatography has been developed for the determination of four fungicides (azoxystrobin, diethofencarb, pyrimethanil and kresoxim-methyl) in water samples. In this novel approach, ionic liquid (IL) was used as extraction solvent in place of the organic solvent used in conventional USAEME assay, and there is no need for using organic dispersive solvent which is typically required in the common dispersive liquid-liquid microextraction method. Various parameters that affect the extraction efficiency, such as the kind and volume of IL, ultrasound emulsification time, extraction temperature and salt addition were investigated and optimized. Under the optimum extraction condition, the linearities of calibration curves were in the range from 3 to 5000 ng mL(-1) for target analytes with the correlation coefficient higher than 0.9992. The enrichment factors and the limits of detection were in the range of 88-137 and 0.73-2.2 ng mL(-1), depending on the analytes. The environmental water samples were successfully analyzed using the proposed method, and the relative recoveries at fortified levels of 50 and 100 ng mL(-1) were in the range of 83.9%-116.2%. PMID:23597988

  2. Development of an ultrasound-assisted emulsification microextraction method for the determination of chlorpyrifos and organochlorine pesticide residues in honey samples using gas chromatography with mass spectrometry.

    PubMed

    Mousavi, Mir-Michael; Arefhosseini, Seyedrafie; Alizadeh Nabili, Ali Akbar; Mahmoudpour, Mansour; Nemati, Mahboob

    2016-07-01

    A simple, rapid, and efficient ultrasound-assisted emulsification microextraction method followed by gas chromatography mass spectrometry in selected ion monitoring mode was developed for the determination of organochlorine pesticides in honey samples. The type and volume of organic extraction solvent, pH, effect of added salt content, and centrifuging time and speed were investigated. Under the optimum extraction conditions, 30 μL of 1, 2-dibromoethane (extraction solvent) was immersed into an ultrasonic bath for 1 min at 40°C. The limits of detection and quantification for all target pesticides were 0.003-0.06 and 0.01-0.2 ng/g, respectively. The extraction recovery was 91-100% and the enrichment factors were 168-192. The relative standard deviation for the method was <6% for intraday (n = 6) and <8% for interday precision (n = 4). The proposed method was successfully applied for the analysis of organochlorine pesticides in honey samples. PMID:27214344

  3. Ultrasound-assisted emulsification microextraction with simultaneous derivatization coupled to fibre optics-based cuvetteless UV-vis micro-spectrophotometry for formaldehyde determination in cosmetic samples.

    PubMed

    Lavilla, Isela; Cabaleiro, Noelia; Pena, Francisco; de la Calle, Inmaculada; Bendicho, Carlos

    2010-07-26

    In this work, ultrasound-assisted emulsification microextraction in combination with fibre optics-based cuvetteless UV-vis micro-spectrophotometry has been proposed as a novel method for the determination of formaldehyde in water-based cosmetics such as shampoo, conditioner and shower gel. The use of a powerful cup-horn sonoreactor allows simultaneous extraction and derivatization of the samples without any pre-treatment. The type and volume of organic extractant solvent, need for a disperser solvent, sonication conditions (sonication time and amplitude), ionic strength and centrifuging time have been carefully studied. Matrix effects were also evaluated. The European official method for quantification of formaldehyde in cosmetic products was used for comparison purposes. An important improvement in sensitivity and sample throughput as well as miniaturization was achieved. A limit of detection of 0.02 microg g(-1) of formaldehyde and a repeatability expressed as relative standard deviation of 5.9% were obtained. PMID:20638500

  4. Ionic liquid-based totally organic solvent-free emulsification microextraction coupled with high performance liquid chromatography for the determination of three acaricides in fruit juice.

    PubMed

    Zhang, Jiaheng; Liang, Zhe; Guo, Hao; Gao, Peng; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

    2013-10-15

    A novel, totally organic solvent-free emulsification microextraction (TEME) technique using ionic liquids (ILs) is proposed in this study. Seven bis(trifluoromethylsulfonyl)imide ionic liquids were synthesized. After comparing the physicochemical properties of the ionic liquids and their application to microextraction experiments, 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([C6MIM][NTf2]), which has moderate surface tension and viscosity, was selected as the extraction solvent. The dispersion of ILs and mass transfer were accelerated by ultrasound irradiation and temperature control processes. Therefore, no dispersive organic solvent was needed. Several variables, such as ionic liquid volume, duration of the ultrasound extraction, dispersion temperature, ionic strength and centrifugation time were investigated and optimized. Under the optimum conditions, the calibration curve was linear in the range of 0.1-600 μg L(-1) for chlorfenapyr and fenpyroximate and 0.5-600 μg L(-1) for spirodiclofen, with correlation coefficients of 0.9994-0.9999. The enrichment factors were between 261 and 285. The limits of detection (LODs) were 0.02-0.06 μg L(-1). Real fruit juice samples (at fortified levels of 10 μg L(-1) and 30 μg L(-1)) were successfully analyzed using the proposed method. The relative recoveries and enrichment factors were in the range of 92-104%. PMID:24054632

  5. Ultrasound-Assisted Emulsification Microextraction Based on Solidification Floating Organic Drop Trace Amounts of Manganese Prior to Graphite Furnace Atomic Absorption Spectrometry Determination

    PubMed Central

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

    In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn+2 at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50–10.0 ng mL−1 with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL−1 was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

  6. Ultrasound-assisted emulsification microextraction based on solidification floating organic drop trace amounts of manganese prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

    In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn(+2) at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50-10.0 ng mL(-1) with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL(-1) was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

  7. In situ emulsification microextraction using a dicationic ionic liquid followed by magnetic assisted physisorption for determination of lead prior to micro-sampling flame atomic absorption spectrometry.

    PubMed

    Shokri, Masood; Beiraghi, Asadollah; Seidi, Shahram

    2015-08-19

    For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L(-1) lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf2], was added into the sample solution containing 100 μL of 1.0 mol L(-1) 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl2, to form a water immiscible ionic liquid, [pbmim][NTf2]2. This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe3O4 magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf2]2, physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L(-1). Good linearity was obtained in the range of 2.5-150 μg L(-1) with determination coefficient (r(2)) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L(-1) was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples. PMID:26343434

  8. Ultrasound-assisted temperature-controlled ionic liquid emulsification microextraction coupled with capillary electrophoresis for the determination of parabens in personal care products.

    PubMed

    Ma, Teng; Li, Zheng; Jia, Qiong; Zhou, Weihong

    2016-07-01

    We developed a CE and ultrasound-assisted temperature-controlled ionic liquid emulsification microextraction method for the determination of four parabens (methyl paraben, ethyl paraben, propyl paraben, and butyl paraben) in personal care products including mouthwash and toning lotion. In the proposed extraction procedure, ionic liquid (IL, 1-octyl-3-methylimidazolium hexafluorophosphate) was used as extraction solvent, moreover, no disperser solvent was needed. Parameters affecting the extraction efficiency including volume of IL, heating temperature, ultrasonic time, extraction time, sample pH, ionic strength, and centrifugation time were optimized. Under the optimized conditions, the method was found to be linear over the range of 3-500 ng/mL with coefficient of determination (R(2) ) in the range of 0.9990-0.9998. The LODs and LOQs for the four parabens were 0.45-0.72 ng/mL and 1.50-2.40 ng/mL, respectively. Intraday and interday precisions (RSDs, n = 5) were in the range of 5.4-6.8% and 7.0-8.7%, respectively. The recoveries of parabens at different spiked levels ranged from 71.9 to 119.2% with RSDs less than 9.5%. PMID:26990303

  9. Ultrasound-assisted emulsification solidified floating organic drops microextraction of ultra trace amount of Te (IV) prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Fathirad, Fariba; Afzali, Daryoush; Mostafavi, Ali; Ghanbarian, Maryam

    2012-01-15

    In the present study, a new, simple and efficient method for the preconcentration of ultra trace amounts of Te (IV) is developed using ultrasound-assisted emulsification solidified floating organic drops microextraction (USAE-SFODME) before graphite furnace atomic absorption spectrometry determination. In this method, tellurium is extracted into the fine droplets of 1-undecanol after chelate formation with the water soluble ligand, ammonium pyrrolidinedithiocarbamate (APDC). Several factors such as pH, chelating agent amount, type and volume of the extracting solvent, sonication and centrifuging time that influence the extraction and complex formation are optimized. Under the optimum conditions, the calibration graph is linear in the range of 0.01-0.24ngmL(-1) of tellurium in the original solution, with limit of detection of 0.003ngmL(-1). The relative standard deviation (RSD) for seven replicated determinations of tellurium ion at 0.08ngmL(-1) concentration level is calculated as 3.4%. The proposed method was successfully applied to the determination of Te (IV) in a standard soil and several water samples. PMID:22265571

  10. Evaluation of the contamination of spirits by polycyclic aromatic hydrocarbons using ultrasound-assisted emulsification microextraction coupled to gas chromatography-mass spectrometry.

    PubMed

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2016-01-01

    The concentration of twelve polycyclic aromatic hydrocarbons (PAHs), included in the list of priority pollutants, in different spirits has been obtained by means of a rapid and sensitive method based on gas chromatography and mass spectrometry (GC-MS). The environmentally friendly ultrasound-assisted emulsification microextraction (USAEME) technique allowed the easy and effective preconcentration of the PAHs from the sample matrices. Several parameters affecting the extraction efficiency, such as the nature and volume of the extractant solvent, and the addition of salt, as well as the sonication parameters were investigated and optimized. The absence of matrix effects under the optimized conditions allowed the sample quantification against aqueous standards. Detection limits ranged between 1.8 and 6.3 ng L(-1), depending on the compound. Different spirit samples were successfully analyzed using the proposed method, and contents of up to 0.9 μg L(-1) were found. Relative recoveries at fortified levels of 0.2 and 1 μg L(-1) were in the range 84-118%. PMID:26212977

  11. Development of an ultrasound-assisted emulsification-microextraction method for the determination of the main compounds causing cork taint in wines.

    PubMed

    Pizarro, C; Sáenz-González, Cristina; Pérez-del-Notario, Nuria; González-Sáiz, José María

    2012-03-16

    In this work, an ultrasound-assisted emulsification-microextraction method has been optimised for the determination in wine of haloanisoles (2,4,6-trichloranisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloranisole (PCA)) responsible for the so-called cork taint. Their halophenolic precursors (2,4,6-trichlorophenol (TCP), 2,3,4,6-tetrachlorophenol (TeCP), 2,4,6-tribromophenol (TBP) and pentachlorophenol (PCP)) have also been simultaneously determined. For this purpose, parameters affecting the USAEME-derivatisation procedure were exhaustively investigated. Firstly, extraction solvent, basic conditions and extraction time were selected to, subsequently, employ experimental design methodology for the simultaneous optimisation of the volumes of acetic anhydride and extraction solvent, temperature and ionic strength conditions. Once optimised, the evaluation of the analytical performance of the method confirmed its suitability for the determination of the studied compounds in wines. The proposed method showed satisfactory linearity (correlation coefficients over 0.981), repeatability (below 10.9%) and inter-day precision (below 11.0%). Detection limits obtained were similar or even lower than previously reported. In addition, the proposed method was successfully applied to the analysis of real samples. To our knowledge, this is the first time that USAME method has been optimised for the simultaneous determination of haloanisoles and halophenols in wine. PMID:22326186

  12. Determination of personal care products and hormones in leachate and groundwater from Polish MSW landfills by ultrasound-assisted emulsification microextraction and GC-MS.

    PubMed

    Kapelewska, Justyna; Kotowska, Urszula; Wiśniewska, Katarzyna

    2016-01-01

    Determination of the endocrine disrupting compounds (EDCs) in leachate and groundwater samples from the landfill sites is very important because of the proven harmful effects of these compounds on human and animal organisms. A method combining ultrasound-assisted emulsification microextraction (USAEME) and gas chromatography-mass spectrometry (GC-MS) was developed for simultaneous determination of seven personal care products (PCPs): methylparaben (MP), ethylparaben (EP), propylparaben (PP), buthylparaben (BP), benzophenone (BPh), 3-(4-methylbenzylidene)camphor (4-MBC), N,N-diethyltoluamide (DEET), and two hormones: estrone (E1) and β-estradiol (E2) in landfill leachate and groundwater samples. The limit of detection (LOD)/limit of quantification (LOQ) values in landfill leachate and groundwater samples were in the range of 0.003-0.083/0.009-0.277 μg L(-1) and 0.001-0.015/0.002-0.049 μg L(-1), respectively. Quantitative recoveries and satisfactory precision were obtained. All studied compounds were found in the landfill leachates from Polish municipal solid waste (MSW) landfills; the concentrations were between 0.66 and 202.42 μg L(-1). The concentration of pollutants in groundwater samples was generally below 0.1 μg L(-1). PMID:26381788

  13. Rapid analysis of chlorinated anilines in environmental water samples using ultrasound assisted emulsification microextraction with solidification of floating organic droplet followed by HPLC-UV detection.

    PubMed

    Ramkumar, Abilasha; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

    2012-08-15

    The present study demonstrates a simple, rapid and efficient method for the determination of chlorinated anilines (CAs) in environmental water samples using ultrasonication assisted emulsification microextraction technique based on solidification of floating organic droplet (USAEME-SFO) coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection. In this extraction method, 1-dodecanol was used as extraction solvent which is of lower density than water, low toxicity, low volatility, and low melting point (24 °C). After the USAEME, extraction solvent could be collected easily by keeping the extraction tube in ice bath for 2 min and the solidified organic droplet was scooped out using a spatula and transferred to another glass vial and allowed to thaw. Then, 10 μL of extraction solvent was diluted with mobile phase (1:1) and taken for HPLC-UV analysis. Parameters influencing the extraction efficiency, such as the kind and volume of extraction solvent, volume of sample, ultrasonication time, pH and salt concentration were thoroughly examined and optimized. Under the optimal conditions, the method showed good linearity in the concentration range of 0.05-500 ng mL(-1) with correlation coefficients ranging from 0.9948 to 0.9957 for the three target CAs. The limit of detection based on signal to noise ratio of 3 ranged from 0.01 to 0.1 ng mL(-1). The relative standard deviations (RSDs) varied from 2.1 to 6.1% (n=3) and the enrichment factors ranged from 44 to 124. The proposed method has also been successfully applied to analyze real water samples and the relative recoveries of environmental water samples ranged from 81.1 to 116.9%. PMID:22841080

  14. Chemometric-based determination of polycyclic aromatic hydrocarbons in aqueous samples using ultrasound-assisted emulsification microextraction combined to gas chromatography-mass spectrometry.

    PubMed

    Ahmadvand, Mohammad; Sereshti, Hassan; Parastar, Hadi

    2015-09-25

    In the present research, ultrasonic-assisted emulsification-microextraction (USAEME) coupled with gas chromatography-mass spectrometry (GC-MS) has been proposed for analysis of thirteen environmental protection agency (EPA) polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Tetrachloroethylene was selected as extraction solvent. The main parameters of USAEME affecting the efficiency of the method were modeled and optimized using a central composite design (CCD). Under the optimum conditions (9μL for extraction solvent, 1.15% (w/v) NaCl (salt concentration) and 10min for ultrasonication time), preconcentration factor (PF) of the PAHs was in the range of 500-950. In order to have a comprehensive analysis, multivariate curve resolution-alternating least squares (MCR-ALS) as a second-order calibration algorithm was used for resolution, identification and quantification of the target PAHs in the presence of uncalibrated interferences. The regression coefficients and relative errors (REs, %) of calibration curves of the PAHs were in the satisfactory range of 0.9971-0.9999 and 1.17-6.59%, respectively. Furthermore, analytical figures of merit (AFOM) for univariate and second-order calibrations were obtained and compared. As an instance, the limit of detections (LODs) of target PAHs were in the range of 1.87-18.9 and 0.89-6.49ngmL(-1) for univariate and second-order calibration, respectively. Finally, the proposed strategy was used for determination of target PAHs in real water samples (tap and hookah waters). The relative recoveries (RR) and the relative standard deviations (RSDs) were 68.4-109.80% and 2.15-6.93%, respectively. It was concluded that combination of multivariate chemometric methods with USAEME-GC-MS can be considered as a new insight for the analysis of target analytes in complex sample matrices. PMID:26319375

  15. Application of ultrasound-assisted emulsification microextraction for simultaneous determination of aminophenol isomers in human urine, hair dye, and water samples using high-performance liquid chromatography.

    PubMed

    Asghari, Alireza; Fazl-Karimi, Hamidreza; Barfi, Behruz; Rajabi, Maryam; Daneshfar, Ali

    2014-08-01

    Aminophenol isomers (2-, 3-, and 4-aminophenols) are typically classified as industrial pollutants with genotoxic and mutagenic effects due to their easy penetration through the skin and membranes of human, animals, and plants. In the present study, a simple and efficient ultrasound-assisted emulsification microextraction procedure coupled with high-performance liquid chromatography with ultraviolet detector was developed for preconcentration and determination of these compounds in human fluid and environmental water samples. Effective parameters (such as type and volume of extraction solvent, pH and ionic strength of sample, and ultrasonication and centrifuging time) were investigated and optimized. Under optimum conditions (including sample volume: 5 mL; extraction solvent: chloroform, 80 µL; pH: 6.5; without salt addition; ultrasonication: 3.5 min; and centrifuging time: 3 min, 5000 rpm min(-1)), the enrichment factors and limits of detection were ranged from 42 to 51 and 0.028 to 0.112 µg mL(-1), respectively. Once optimized, analytical performance of the method was studied in terms of linearity (0.085-157 µg mL(-1), r (2) > 0.998), accuracy (recovery = 88.6- 101.7%), and precision (repeatability: intraday precision < 3.98%, and interday precision < 5.12%). Finally, applicability of the method was evaluated by the extraction and determination of these compounds in human urine, hair dye, and real water samples. PMID:24275645

  16. Sensitive determination of 2,4,6-trichloroanisole in water samples by ultrasound assisted emulsification microextraction prior to gas chromatography-tandem mass spectrometry analysis.

    PubMed

    Fontana, Ariel R; Altamirano, Jorgelina C

    2010-06-15

    A novel application of an ultrasound assisted emulsification microextraction (USAEME) technique is proposed for the extraction and preconcentration of 2,4,6-trichloroanisole (2,4,6-TCA) from water samples prior to its determination by gas chromatography-tandem mass spectrometry (GC-MS/MS). USAEME employs a non-polar high-density solvent (extractant solvent), which forms an oil-in-water emulsion (O/W) in the aqueous sample bulk assisted by ultrasonic radiation. Several factors including, solvent type and volume, extraction time, extraction temperature, shaking mode and matrix modifiers were studied and optimized over the relative recovery of the target analyte. An aliquot of 5mL water sample was conditioned by adding 150microL 6.15molL(-1) sodium chloride and 300microL 0.05molL(-1) phosphate buffer (pH 6), and finally extracted with 40microL chloroform by using USAEME technique. Under the optimal experimental conditions 2,4,6-TCA was quantitatively extracted achieving an enrichment factor (EF) of 555. The detection limit (LOD), calculated as three times the signal-to-noise ratio (S/N), was 0.2ngL(-1) and the RSD was 6.3% (n=5) when 1ngL(-1) 2,4,6-TCA standard mixture was analyzed. The coefficients of estimation of the calibration curves obtained following the proposed methodology was >or=0.997 and the linear working range was 1-5000ngL(-1). Finally, the proposed technique was successfully applied for extraction and determination of the 2,4,6-TCA in water samples. Recovery studies lead values >or=94%, which showed a successfully robustness of the analytical methodology for determination of nanogram per liter of 2,4,6-TCA in water samples. PMID:20441935

  17. Emulsification liquid-liquid microextraction based on deep eutectic solvent: An extraction method for the determination of benzene, toluene, ethylbenzene and seven polycyclic aromatic hydrocarbons from water samples.

    PubMed

    Khezeli, Tahere; Daneshfar, Ali; Sahraei, Reza

    2015-12-18

    In this study, for the first time, a simple, inexpensive and sensitive method named emulsification liquid-liquid microextraction based on deep eutectic solvent (ELLME-DES) was used for the extraction of benzene, toluene, ethylbenzene (BTE) and seven polycyclic aromatic hydrocarbons (PAHs) from water samples. In a typical experiment, 100μL of DES (as water-miscible extraction solvent) was added to 1.5mL of sample solution containing target analytes. A homogeneous solution was formed immediately. Injection of 100μL of THF (as emulsifier agent) into homogeneous solution provided a turbid state. After extraction, phase separation (aqueous phase/DES rich phase) was performed by centrifugation. DES rich phase was withdrawn by a micro-syringe and submitted to isocratic reverse-phase HPLC with UV detection. Under optimum conditions obtained by response surface methodology (RSM) and desirability function (DF), the calibration graphs were linear in the concentration range from 10 to 200μg/L for benzene, 10-400μg/L for toluene, 1-400μg/L for ethylbenzene, biphenyl, chrysene and fluorene, and 0.1-400μg/L for anthracene, benzo[a]pyrene, phenanthrene and pyrene. The coefficients of determination (r(2)) and limits of detection were 0.9924-0.9997 and 0.02-6.8μg/L, respectively. This procedure was successfully applied to the determination of target analytes in spiked water samples. The relative mean recoveries ranged from 93.1 to 103.3%. PMID:26614169

  18. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A.

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v- 1 of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L- 1 with a limit of detection of 4.9 μg L- 1 and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L- 1 Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials.

  19. Novel solvent-free microwave-assisted extraction coupled with low-density solvent-based in-tube ultrasound-assisted emulsification microextraction for the fast analysis of organophosphorus pesticides in soils.

    PubMed

    Su, Yi-Song; Yan, Cheing-Tong; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

    2013-07-01

    A novel and rapid solventless microwave-assisted extraction coupled with low-density solvent-based in-tube ultrasound-assisted emulsification microextraction has been developed for the efficient determination of nine organophosphorus pesticides in soils by GC analysis with microelectron capture detection. A specially designed, homemade glass tube inbuilt with a scaled capillary tube was used as an extraction device to collect and measure the separated extractant phase easily. Parameters affecting the efficiencies of the developed method were thoroughly investigated. From experimental results, the following conditions were selected for the extraction of organophosphorus pesticides from 1.0 g of soil sample to 5 mL of aqueous solution under 226 W of microwave irradiation for 2.5 min followed by ultrasound-assisted emulsification microextraction with 20 μL toluene for 30 s and then centrifugation at 3200 rpm for 3 min. Detections were linear in the range of 0.25-10 ng/g with detection limits between 0.04 and 0.13 ng/g for all target analytes. The applicability of the method to real samples was assessed on agricultural contaminated soils and the recoveries ranged between 91.4 and 101.3%. Compared to other methods, the present method was shown to be highly competitive in terms of sensitivity, cost, eco-friendly nature, and analysis speed. PMID:23681938

  20. Surfactant-enhanced alkaline flooding for light oil recovery. Annual report, 1992--1993

    SciTech Connect

    Wasan, D.T.

    1994-08-01

    In this report, the authors present the results of experimental and theoretical studies in surfactant-enhanced alkaline flooding for light oil recovery. The overall objective of this work is to develop a very cost-effective method for formulating a successful surfactant-enhanced alkaline flood by appropriately choosing mixed alkalis which form inexpensive buffers to obtain the desired pH (between 8.5 and 12.0) for ultimate spontaneous emulsification and ultralow interfacial tension. In addition, the authors have (1) developed a theoretical interfacial activity model for determining equilibrium interfacial tension, (2) investigated the mechanisms for spontaneous emulsification, (3) developed a technique to monitor low water content in oil, and (4) developed a technique to study water-in-oil emulsion film properties.

  1. Surfactant-enhanced aquifier remediation

    SciTech Connect

    Fountain, J.C.

    1996-12-31

    Surfactants can be used to rapidly remove NAPL from contaminated aquifers. They are effective for virtually any organic contaminant. Use in LNAPL contaminated sites requires adequate hydraulic conductivity and control of flow using either hydraulic or physical methods. The presence of DNAPL requires consideration of vertical mobility; a competent confining layer (aquitard) is required if additional aquifers are present at greater depths. Surfactant processes, whether based upon mobilization or solubilization, can be effective at mass removal, but cannot be expected to provide resortation to drinking water standards. The fraction of mass removal, and the cost of remediation using surfactants are dependent upon a sites hydrogeology. Both minimization of cost and maximization of NAPL removal requires detailed characterization of sites contaminant distribution and hydrogeology. Assessment of the feasibility of surfactant-enhanced remediation is dependent upon a detailed site characterization.

  2. Ultrasound assisted-deep eutectic solvent based on emulsification liquid phase microextraction combined with microsample injection flame atomic absorption spectrometry for valence speciation of chromium(III/VI) in environmental samples.

    PubMed

    Yilmaz, Erkan; Soylak, Mustafa

    2016-11-01

    A new type of deep eutectic solvents (DESs) have been prepared and used as extraction solvents for ultrasound assisted-deep eutectic solvent based emulsification liquid phase microextraction method (UA-DES-ELPME) for the determination and speciation of total chromium, chromium(III) and chromium(VI). The chromium concentration in DES rich phase (extraction phase) was determined by using microsample injection flame atomic absorption spectrometer (FAAS). The detection limit (LOD), the quantification limit (LOQ), preconcentration factor and relative standard deviation were found as 5.5µgL(-1), 18.2µgL(-1), 20 and 6%, respectively. The accuracy of the developed method was evaluated by the analysis of water the certified reference materials (TMDA-53.3 Fortified environmental water and TMDA-54.4 Fortified Lake Water) and addition-recovery tests for water samples. PMID:27591663

  3. Ligandless, ion pair-based and ultrasound assisted emulsification solidified floating organic drop microextraction for simultaneous preconcentration of ultra-trace amounts of gold and thallium and determination by GFAAS.

    PubMed

    Fazelirad, Hamid; Taher, Mohammad Ali

    2013-01-15

    In the present work, a new, simple and efficient method for simultaneous preconcentration of ultra-trace amounts of gold and thallium is developed using an ion pair based-ultrasound assisted emulsification-solidified floating organic drop microextraction procedure before graphite furnace atomic absorption spectrometry determination. This methodology was used to preconcentrate the ion pairs formed between AuCl(4)(-) and TlCl(4)(-) and [C(23)H(42)]N(+) in a microliter-range volume of 1-undecanol. Several factors affecting the microextraction efficiency, such as HCl volume, type and volume of extraction solvent, sonication time, sample volume, temperature, ionic strength and [C(23)H(42)]NCl volume were investigated and optimized. Under the optimized conditions, the enrichment factor of 441 and 443 and calibration graphs of 2.2-89 and 22.2-667 ng L(-1) for gold and thallium were obtained, respectively. The intra- and inter-day precision of ± 4.4 and ± 4.9% for Au and ± 4.8 and ± 5.4% for Tl were obtained. The detection limit was 0.66 ng L(-1) for Au and 4.67 ng L(-1) for Tl. The results show that the liquid-liquid pretreatment using ion pair forming, is sensitive, rapid, simple and safe method for the simultaneous preconcentration of gold and thallium. The method was successfully applied for determination of gold and thallium in natural water and hair samples. PMID:23200402

  4. Surfactant-enhanced alkaline flooding for light oil recovery. [Annual report], 1993--1994

    SciTech Connect

    Wasan, D.T.

    1995-03-01

    In this report, we present the results of our experimental and theoretical studies in surfactant-enhanced alkaline flooding for light oil recovery. The overall objective of this work is to develop a very cost-effective method for formulating a successful surfactant-enhanced alkaline flood by appropriately choosing mixed alkalis which form inexpensive buffers to obtain the desired pH (between 8.5 and 12.0) for ultimate spontaneous emulsification and ultralow interfacial tension. In addition, we have (1) investigated the effect of surfactant on the equilibrium and transient interfacial tension, (2) investigated the kinetics of oil removal from a silica surface, and (3) developed a theoretical interfacial activity model for determining equilibrium interfacial tension. The results of the studies conducted during the course of this project are presented.

  5. Surfactant-enhanced alkaline flooding for light oil recovery. Quarterly report, April 1, 1995--June 30, 1995

    SciTech Connect

    Wasan, D.T.

    1995-09-01

    The overall objective of this project is to develop a very cost-effective method for formulating a successful surfactant-enhanced alkaline flood by appropriately choosing mixed alkalis which form inexpensive buffers to obtain the desired pH (between 8.5 and 12.0) for ultimate spontaneous emulsification and ultra-low tension. In addition, the novel concept of pH gradient design to optimize flood water conditions will be tested.

  6. A new 1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate ionic liquid based ultrasound-assisted emulsification microextraction for the determination of organic ultraviolet filters in environmental water samples.

    PubMed

    Ge, Dandan; Lee, Hian Kee

    2012-08-17

    A novel microextraction approach termed ionic liquid based ultrasound-assisted emulsification microextraction (IL-USAEME) combined with high-performance liquid chromatography-ultraviolet (HPLC-UV) was developed for the preconcentration and detection of organic ultraviolet (UV) filters in environmental water samples. An ionic liquid (IL) was used in place of an organic solvent as in conventional USAEME. In the study, orthogonal array designs (OAD) were employed for the optimization of the extraction parameters: type of IL, pH of the sample, extraction volume, ultrasonic time and salt concentration. In the first step, a mixed level OAD matrix, OA(16) (4(1) × 2(12)) was employed for the initial optimization. Based on the results of the first step, an ultra-hydrophobic IL, 1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate was chosen as the IL extractant and sample pH was set at a value of 3. Ultrasonic time, extraction volume and salt concentration were further optimized in the second step by an OA(16) (4(5)) matrix. Under the latter optimized conditions, calibration curves with coefficients of estimation higher than 0.997 over the concentration range of 5 and 1000 ng/ml, and the relative standard deviations for six replicates of the extraction from 2.6 to 6.6% were obtained. The limits of detection for four organic UV filters were between 0.5 and 1 ng/ml. The validated technique was applied to the analysis of organic UV filters in environmental water samples. PMID:22771059

  7. SIMULATION OF SURFACTANT-ENHANCED AQUIFER REMEDIATION

    EPA Science Inventory

    Surfactant-enhanced aquifer remediation (SEAR) is currently under active investigation as one of the most promising alternatives to conventional pump-and-treat remediation for aquifers contaminated by dense nonaqueous phase organic liquids. An existing three-dimensional finite-di...

  8. Surfactant-enhanced alkaline flooding for light oil recovery. Final report

    SciTech Connect

    Wasan, D.T.

    1996-05-01

    In this report, we present the results of our experimental and theoretical studies in surfactant-enhanced alkaline flooding for light oil recovery. The overall objective of this work is to develop a very cost-effective method for formulating a successful surfactant-enhanced alkaline flood by appropriately choosing mixed alkalis which form inexpensive buffers to obtain the desired pH (between 8.5 and 12. 0) for ultimate spontaneous emulsification and ultralow interfacial tension. In addition, we have (1) developed a theoretical interfacial activity model for determining equilibrium interfacial tension, (2) investigated the mechanisms for spontaneous emulsification, (3) developed a technique to monitor low water content in oil and (4) developed a technique to study water-in-oil emulsion film properties, (5) investigated the effect of surfactant on the equilibrium and transient interfacial tension, (6) investigated the kinetics of oil removal from a silica surface, and (7) developed a theoretical interfacial activity model for determining equilibrium interfacial tension, accounting for added surfactant. The results of the studies conducted during the course of this project are discussed.

  9. Surfactant-enhanced alkaline flooding for light oil recovery. Final report 1994--1995

    SciTech Connect

    Wasan, D.T.

    1995-12-01

    In this report, the authors present the results of their experimental and theoretical studies in surfactant-enhanced alkaline flooding for light oil recovery. The overall objective of this work is to develop a very cost-effective method for formulating a successful surfactant-enhanced alkaline flood by appropriately choosing mixed alkalis which form inexpensive buffers to obtain the desired pH (between 8.5 and 12.0) for ultimate spontaneous emulsification and ultralow interfacial tension. In addition, the authors have (1) developed a theoretical interfacial activity model for determining equilibrium interfacial tension, (2) investigated the mechanisms for spontaneous emulsification, (3) developed a technique to monitor low water content in oil, and (4) developed a technique to study water-in-oil emulsion film properties, (5) investigated the effect of surfactant on the equilibrium and transient interfacial tension, (6) investigated the kinetics of oil removal from a silica surface, and (7) developed a theoretical interfacial activity model for determining equilibrium interfacial tension, accounting for added surfactant. The results of the studies conducted during the course of this project are summarized.

  10. Surfactant-enhanced alkaline flooding field project

    SciTech Connect

    French, T.R.

    1991-10-01

    The Tucker sand of Helper (KS) field is a candidate for surfactant-enhanced alkaline flooding. The geology of the Helper site is typical of many DOE Class I reservoirs. The Tucker sand of Helper field was deposited in a fluvial dominated deltaic environment. Helper oil can be mobilized with either chemical system 2 or chemical system 3, as described in this report. Oil fields in the Gulf Coast region are also good candidates for surfactant-enhanced alkaline flooding. The results from laboratory tests conducted in Berea sandstone cores with oil brine from Helper (KS) field are encouraging. The crude oil is viscous and non-acidic and, yet, was mobilized by the chemical formulations described in this report. Significant amounts of the oil were mobilized under simulated reservoir conditions. The results in Berea sandstone cores were encouraging and should be verified by tests with field core. Consumption of alkali, measured with field core, was very low. Surfactant loss appeared to be acceptable. Despite the good potential for mobilization of Helper oil, certain reservoir characteristics such as low permeability, compartmentalization, and shallow depth place constraints on applications of any chemical system in the Tucker sand. These constraints are typical of many DOE Class I reservoirs. Although Hepler field is not a perfect reservoir in which to apply surfactant- enhanced alkaline flooding, Hepler oil is particularly amenable to mobilization by surfactant-enhanced alkaline systems. A field test is recommended, dependent upon final evaluation of well logs and cores from the proposed pilot area. 14 refs., 21 figs., 10 tabs.

  11. SURFACTANT ENHANCED AQUIFER REMEDIATION WITH SURFACTANT REGENERATION/REUSE

    EPA Science Inventory

    A demonstration of surfactant-enhanced aquifer remediation was conducted during the spring of 1999 at Marine Corps Base, Camp LeJeune, NC. A PCE-DNAPL zone was identified and delineated by extensive soil sampling in 1997, and was further characteized by a partitioning interwell t...

  12. MEASUREMENT OF MASS TRANSFER RATES FOR SURFACTANT-ENHANCED SOLUBILIZATION OF NONAQUEOUS PHASE LIQUIDS. (R825405)

    EPA Science Inventory

    Surfactant-enhanced solubilization of residual, nonaqueous-phase liquid (NAPL) contaminants is an emerging, subsurface remediation technology. The potential for nonequilibrium conditions is investigated for surfactant-enhanced solubilization of a NAPL, trichloroethylene (TCE), in...

  13. Practical Considerations and Challenges Involved in Surfactant Enhanced Bioremediation of Oil

    PubMed Central

    Mohanty, Sagarika; Jasmine, Jublee

    2013-01-01

    Surfactant enhanced bioremediation (SEB) of oil is an approach adopted to overcome the bioavailability constraints encountered in biotransformation of nonaqueous phase liquid (NAPL) pollutants. Fuel oils contain n-alkanes and other aliphatic hydrocarbons, monoaromatics, and polynuclear aromatic hydrocarbons (PAHs). Although hydrocarbon degrading cultures are abundant in nature, complete biodegradation of oil is rarely achieved even under favorable environmental conditions due to the structural complexity of oil and culture specificities. Moreover, the interaction among cultures in a consortium, substrate interaction effects during the degradation and ability of specific cultures to alter the bioavailability of oil invariably affect the process. Although SEB has the potential to increase the degradation rate of oil and its constituents, there are numerous challenges in the successful application of this technology. Success is dependent on the choice of appropriate surfactant type and dose since the surfactant-hydrocarbon-microorganism interaction may be unique to each scenario. Surfactants not only enhance the uptake of constituents through micellar solubilization and emulsification but can also alter microbial cell surface characteristics. Moreover, hydrocarbons partitioned in micelles may not be readily bioavailable depending on the microorganism-surfactant interactions. Surfactant toxicity and inherent biodegradability of surfactants may pose additional challenges as discussed in this review. PMID:24350261

  14. Surfactant-enhanced alkaline flooding field project. Annual report, Revision

    SciTech Connect

    French, T.R.

    1991-10-01

    The Tucker sand of Helper (KS) field is a candidate for surfactant-enhanced alkaline flooding. The geology of the Helper site is typical of many DOE Class I reservoirs. The Tucker sand of Helper field was deposited in a fluvial dominated deltaic environment. Helper oil can be mobilized with either chemical system 2 or chemical system 3, as described in this report. Oil fields in the Gulf Coast region are also good candidates for surfactant-enhanced alkaline flooding. The results from laboratory tests conducted in Berea sandstone cores with oil brine from Helper (KS) field are encouraging. The crude oil is viscous and non-acidic and, yet, was mobilized by the chemical formulations described in this report. Significant amounts of the oil were mobilized under simulated reservoir conditions. The results in Berea sandstone cores were encouraging and should be verified by tests with field core. Consumption of alkali, measured with field core, was very low. Surfactant loss appeared to be acceptable. Despite the good potential for mobilization of Helper oil, certain reservoir characteristics such as low permeability, compartmentalization, and shallow depth place constraints on applications of any chemical system in the Tucker sand. These constraints are typical of many DOE Class I reservoirs. Although Hepler field is not a perfect reservoir in which to apply surfactant- enhanced alkaline flooding, Hepler oil is particularly amenable to mobilization by surfactant-enhanced alkaline systems. A field test is recommended, dependent upon final evaluation of well logs and cores from the proposed pilot area. 14 refs., 21 figs., 10 tabs.

  15. Surfactant-enhanced low-pH alkaline flooding

    SciTech Connect

    Peru, D.A. and Co., Columbia, MD . Research Div.); Lorenz, P.B. )

    1990-08-01

    This paper reports sodium bicarbonate investigated as a potential alkaline agent in surfactant-enhanced alkaline flooding because it has very little tendency to dissolve silicate minerals. In experiments performed with Wilmington, CA, crude oil and three types of surfactants, the bicarbonate/surfactant combination caused a marked lowering of interfacial tension (IFT). Bicarbonate protected the surfactant against divalent cations and reduced adsorption of surfactant and polymer on various minerals. Coreflood test confirm that sodium bicarbonate plus surfactant can be an effective alternative to the high-pH flooding process.

  16. Surfactant-enhanced alkaline flooding for light oil recovery. Quarterly report, January 1--March 31, 1994

    SciTech Connect

    Wasan, D.T.

    1994-06-01

    The overall objective of this project is to develop a very cost-effective method for formulating a successful surfactant-enhanced alkaline flood by appropriately choosing mixed alkalis which form inexpensive buffers to obtain the desired pH (between 8.5 and 12.0) for ultimate spontaneous emulsification and ultra-low tension. In addition, the novel concept of pH gradient design to optimize flood water conditions will be tested. Last quarter we investigated the phase behavior and the regions where in the middle phase occurs. The optimum phase was found to go through a maximum with pH, sodium concentration and surfactant concentration. The optimum pH is about 12.0 to 13.5, the optimum sodium concentration is about 0.513 mol/liter, and the optimum surfactant concentration is about 0.2%. The effect of surfactant type was also investigated. Petrostep B-105 was found to give the most middle phase production. This quarter, we investigated the contact angle of Long Beach oil, Adena oil, and a model oil on a solid glass surface in contact with an aqueous alkaline solution both with and without added preformed surfactant. The contact angle with Long Beach and Adena oils showed oil-wet conditions, whereas the model oil showed both oil-wet and water-wet conditions depending on the pH of the aqueous phase. The addition of surfactant to the alkaline solution resulted in making the system less oil-wet. Spreading of the oil on the glass surface was observed in all three systems investigated.

  17. Optimization of modified dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the simultaneous preconcentration and determination of nitrazepam and midazolam drugs: An experimental design.

    PubMed

    Goudarzi, Nasser; Farsimadan, Sahar; Chamjangali, Mansour Arab; Bagherian, Ghadam Ali

    2015-05-01

    A simple, sensitive, and rapid microextraction method, namely, ultrasound-assisted surfactant-enhanced emulsification microextraction based on the solidification of floating organic droplet method coupled with high-performance liquid chromatography was developed for the simultaneous preconcentration and determination of nitrazepam and midazolam. The significant parameters affecting the extraction efficiency were considered using Plackett-Burman design as a screening method. To obtain the optimum conditions with consideration of the selected significant variables, a Box-Behnken design was used. The microextraction procedure was performed using 29.1 μL of 1-undecanol, 1.36% (w/v) of NaCl, 10.0 μL of sodium dodecyl sulfate (25.0 μg mL(-1)), and 1.0 μL of Tween80 (25.0 μg mL(-1)) as an emulsifier in an extraction time of 20.0 min at pH 7.88. In order to investigate the validation of the developed method, some validation parameters including the linear dynamic range, repeatability, limit of detection, and recoveries were studied under the optimum conditions. The detection limits of the method were 0.017 and 0.086 ng mL(-1) for nitrazepam and midazolam, respectively. The extraction recovery percentages for the drugs studied were above 91.0 with acceptable relative standard deviation. The proposed methodology was successfully applied for the determination of these drugs in a number of human serum samples. PMID:25755221

  18. Surfactant-enhanced spreading: Experimental achievements and possible mechanisms.

    PubMed

    Kovalchuk, N M; Trybala, A; Arjmandi-Tash, O; Starov, V

    2016-07-01

    Surfactants are broadly used to improve wetting properties of aqueous formulations. The improvement is achieved by essential reduction of liquid/air and solid/liquid interfacial tensions resulting in the decrease of contact angle. For moderately hydrophobic substrates, there is a range of surfactants providing complete wetting of substrate. With the decrease of substrate surface energy, this range of surfactants reduces very quickly and only trisiloxane surfactant solutions are capable to wet completely such highly hydrophobic substrates as polypropylene and parafilm. That is why these surfactants are referred to as superspreaders. The most intriguing feature of wetting surfactant solutions is their ability to spread much faster than pure liquids with spread area, S, being proportional to time, t, S~t, as compared to S~t(0.2) for pure liquids, which wet completely the solid substrate. Trisiloxane surfactant solutions spread faster than other aqueous surfactant solutions, which also provide complete wetting, being superspreaders in the sense of spreading rate as well. The mechanism of fast spreading of surfactant solutions on hydrophobic substrates and much higher spreading rates for trisiloxane solutions are to be explained. Below the available experimental data on superspreading and surfactant-enhanced spreading are analysed/summarised, and possible mechanisms governing the fast spreading are discussed. PMID:26282600

  19. Beyond dispersive liquid-liquid microextraction.

    PubMed

    Leong, Mei-I; Fuh, Ming-Ren; Huang, Shang-Da

    2014-03-28

    Dispersive liquid-liquid microextraction (DLLME) and other dispersion liquid-phase microextraction (LPME) methods have been developed since the first DLLME method was reported in 2006. DLLME is simple, rapid, and affords high enrichment factor, this is due to the large contact surface area of the extraction solvent. DLLME is a method suitable for the extraction in many different water samples, but it requires using chlorinated solvents. In recent years, interest in DLLME or dispersion LPME has been focused on the use of low-toxicity solvents and more conveniently practical procedures. This review examines some of the most interesting developments in the past few years. In the first section, DLLME methods are separated in two categories: DLLME with low-density extraction solvent and DLLME with high-density extraction solvent. Besides these methods, many novel special devices for collecting low-density extraction solvent are also mentioned. In addition, various dispersion techniques with LPME, including manual shaking, air-assisted LPME (aspirating and injecting the extraction mixture by syringe), ultrasound-assisted emulsification, vortex-assisted emulsification, surfactant-assisted emulsification, and microwave-assisted emulsification are described. Besides the above methods, combinations of DLLME with other extraction techniques (solid-phase extraction, stir bar sorptive extraction, molecularly imprinted matrix solid-phase dispersion and supercritical fluid extraction) are introduced. The combination of nanotechnique with DLLME is also introduced. Furthermore, this review illustrates the application of DLLME or dispersion LPME methods to separate and preconcentrate various organic analytes, inorganic analytes, and samples. PMID:24582396

  20. SURFACTANT-ENHANCED SOLUBILIZATION OF RESIDUAL DODECANE IN SOIL COLUMNS - 2. MATHEMATICAL MODELING

    EPA Science Inventory

    A mathematical model is developed to describe surfactant-enhanced solubilization of nonaqueous-phase liquids (NAPLs) in porous media. The model incorporates aqueous-phase transport equations for organic and surfactant components as well as a mass balance for the organic phase. Ra...

  1. FIELD DEMONSTRATION STUDIES OF SURFACTANT-ENHANCED SOLUBILIZATION AND MOBILIZATION AT HILL AIR FORCE BASE, UTAH

    EPA Science Inventory

    Surfactant-enhanced subsurface remediation can dramatically improve contaminant removal rates compared to the traditional pump-and-treat technology. Surfactants can be used to significantly enhance the solubilization of non-aqueous phase liquids (NAPL) constituents, or they can b...

  2. SURFACTANT ENHANCED SOLUBILIZATION OF RESIDUAL DODECANE IN SOIL COLUMNS 1. MATHEMATICAL MODELING

    EPA Science Inventory

    A mathematical model is developed to describe surfactant enhanced solubilization of nonaqueous phase liquids (NAPLS) in porous media. he model incorporates aqueous phase transport equations for organic and surfactant components as well as a mass balance on the organic phase. ate-...

  3. Streamline simulation of surfactant enhanced aquifer remediation. Master`s thesis

    SciTech Connect

    Tunison, D.I.

    1996-12-01

    Nonaqueous Phase Liquids (NAPLs) are a recognized source of groundwater contamination. Surfactant Enhanced Aquifer Remediation (SEAR) shows promise in increasing the efficiency and effectiveness over traditional `pump and treat` NAPL remediation processes. Laboratory results are not always consistent with the effects observed in field applications because of the complex interactions that occur in the subsurface. Mathematical modeling is required to enable accurate prediction and understanding of SEAR.

  4. Modeling surfactant-enhanced nonaqueous-phase liquid remediation of porous media

    SciTech Connect

    White, M.D.; Oostrom, M.

    1998-12-01

    A mathematical model is developed to investigate the main processes associated with surfactant-enhanced nonaqueous-phase liquid (NAPL) remediation of porous media. The model couples four nonlinear mass balance conservation equations (i.e., water, NAPL-phase organic, aqueous-phase organic, and aqueous-phase surfactant) that incorporate aqueous- and NAPL-phase migration and transport of aqueous-phase dissolved surfactant and organics. Rate-limited solubilization of the organic into the aqueous phase is represented by a linear driving force expression and is dependent on the surfactant-enhanced equilibrium concentration. Surfactant-enhanced mobilization of the NAPL phase is incorporated using surfactant concentration-dependent interfacial tension lowering, scaled relative permeability-saturation-capillary pressure relations, and trapping number-dependent effective residual saturations for the nonwetting liquid. Sorption of surfactant is assumed to conform to a Langmuir isotherm model, whereas organic sorption is modeled using a linear isotherm with a surfactant and soil-organic content-dependent retardation coefficient. The model is used to simulate experiments described by Pennel et al. (1996) in which the NAPL perchloroethylene was flushed from sand columns using different surfactant solutions.

  5. Measurement of mass-transfer rates for surfactant-enhanced solubilization of nonaqueous phase liquids

    SciTech Connect

    Mayer, A.S.; Zhong, L.; Pope, G.A.

    1999-09-01

    Surfactant-enhanced solubilization of residual, non-aqueous-phase liquid (NAPL) contaminants is an emerging, subsurface remediation technology. The potential for nonequilibrium conditions is investigated for surfactant-enhanced solubilization of a NAPL, trichlorethylene (TCE), in a model porous medium. The surfactant formulation consists of an anionic surfactant, sodium dihexyl sulfosuccinate, an alcohol, and an electrolyte in aqueous solution. Batch solubilization experiments are conducted to assess the significant of chemical rate limitations. Surfactant flood experiments are conducted in packed columns with residual TCE. Mass-transfer rate coefficients are determined as a function of aqueous-phase pore velocity, NAPL volumetric fraction, and surfactant concentration. A correlation for predicting mass-transfer rate coefficients as a function of system properties is developed. The mass-transfer rate coefficients and correlation are obtained by fitting a transport simulator to the column effluent concentration results. Significant differences are found between the correlation developed here and correlations developed for other NAPL--surfactant systems. The correlation predicts near-linear dependences of mass-transfer rates on the NAPL volumetric fraction and pore velocity. Using the Damkohler number, the degree of nonequilibrium behavior in surfactant-enhanced NAPL solubilization is analyzed for a range of conditions. Nonequilibrium conditions are found to be significant at relatively low NAPL volumetric fractions.

  6. Application of Optimized Vortex-Assisted Surfactant-Enhanced DLLME for Preconcentration of Thymol and Carvacrol, and Their Determination by HPLC-UV: Response Surface Methodology.

    PubMed

    Ghaedi, Mehrorang; Roosta, Mostafa; Khodadoust, Saeid; Daneshfar, Ali

    2015-08-01

    A novel vortex-assisted surfactant-enhanced dispersive liquid-liquid microextraction combined with high-performance liquid chromatography (VASEDLLME-HPLC) was developed for the determination of thymol and carvacrol (phenolic compound). In this method, the extraction solvent (CHCl3) was dispersed into the aqueous samples via a vortex agitator and addition of the surfactant (Triton X-100). The preliminary experiments were undertaken to select the best extraction solvent and surfactant. The influences of effective variables were investigated using a Plackett-Burman 2(7-4) screening design and then, the significant variables were optimized by using a central composite design combined with desirability function. Working under optimum conditions specified as: 140 µL CHCl3, 0.08% (w/v, Triton X-100), 3 min extraction time, 6 min centrifugation at 4,500 rpm, pH 7, 0.0% (w/v) NaCl permit achievement of high and reasonable linear range over 0.005-4.0 mg L(-1) with R(2) = 0.9998 (n = 10). The separation of thymol and carvacrol was achieved in <14 min using a C18 column and an isocratic binary mobile phase acetonitrile-water (55:45, v/v) with a flow rate of 1.0 mL min(-1). The VASEDLLME is applied for successful determination of carvacrol and thymol in different thyme and pharmaceutical samples with relative standard deviation <4.7% (n = 5). PMID:25637132

  7. A comparison of various modes of liquid-liquid based microextraction techniques: determination of picric acid.

    PubMed

    Burdel, Martin; Šandrejová, Jana; Balogh, Ioseph S; Vishnikin, Andriy; Andruch, Vasil

    2013-03-01

    Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples. PMID:23381802

  8. Remediation of Nitrobenzene Contaminated Soil by Combining Surfactant Enhanced Soil Washing and Effluent Oxidation with Persulfate

    PubMed Central

    Yan, Jingchun; Gao, Weiguo; Qian, Linbo; Han, Lu; Chen, Yun; Chen, Mengfang

    2015-01-01

    The combination of surfactant enhanced soil washing and degradation of nitrobenzene (NB) in effluent with persulfate was investigated to remediate NB contaminated soil. Aqueous solution of sodium dodecylbenzenesulfonate (SDBS, 24.0 mmol L-1) was used at a given mass ratio of solution to soil (20:1) to extract NB contaminated soil (47.3 mg kg-1), resulting in NB desorption removal efficient of 76.8%. The washing effluent was treated in Fe2+/persulfate and Fe2+/H2O2 systems successively. The degradation removal of NB was 97.9%, being much higher than that of SDBS (51.6%) with addition of 40.0 mmol L-1 Fe2+ and 40.0 mmol L-1 persulfate after 15 min reaction. The preferential degradation was related to the lone pair electron of generated SO4•−, which preferably removes electrons from aromatic parts of NB over long alkyl chains of SDBS through hydrogen abstraction reactions. No preferential degradation was observed in •OH based oxidation because of its hydrogen abstraction or addition mechanism. The sustained SDBS could be reused for washing the contaminated soil. The combination of the effective surfactant-enhanced washing and the preferential degradation of NB with Fe2+/persulfate provide a useful option to remediate NB contaminated soil. PMID:26266532

  9. Effect of surfactant phase behavior on emulsification.

    PubMed

    Kaizu, Kazuhiro; Alexandridis, Paschalis

    2016-03-15

    In order to improve our understanding of the effects that the equilibrium phase behavior and structure of amphiphiles have on the emulsification process and the properties of emulsions stabilized by these amphiphiles, we have exploited the known phase behavior of polyoxyethylene-polyoxypropylene-polyoxyethylene (POE-POP-POE) amphiphilic block copolymers (Pluronics) in the presence of two immiscible solvents. Specifically, we considered ternary systems consisting of Pluronic F38, L64, P84, P104, or L121 with water and p-xylene which exhibit a very rich phase behavior, including a variety of water-continuous and oil-continuous lyotropic liquid crystalline (LLC) phases. We prepared emulsions having the same (final) compositions but through different emulsification paths, and evaluated the emulsions on the basis of homogeneity and droplet size. We found finer and more homogenous emulsions to result when O/lamellar gel structures (as revealed by small-angle X-ray scattering) were formed during the emulsification process, or when the emulsification path traversed the lamellar LLC phase. This can be attributed to the favorable properties of the lamellar structure: high oil solubilization capacity with concurrent facile dispersibility in water, relatively low interfacial tension, and relatively low viscosity. The findings reported here are relevant to the preparation of emulsions for diverse applications such as skin-care products, pharmaceuticals, food products, coatings, inks, agrochemicals, oil dispersants, and nanomaterials synthesis. PMID:26724700

  10. Visualization of surfactant enhanced NAPL mobilization and solubilization in a two-dimensional micromodel

    SciTech Connect

    ZHONG,LIRONG; MAYER,ALEX; GLASS JR.,ROBERT J.

    2000-03-08

    Surfactant-enhanced aquifer remediation is an emerging technology for aquifers contaminated with nonaqueous phase liquids (NAPLs). A two-dimensional micromodel and image capture system were applied to observe NAPL mobilization and solubilization phenomena. In each experiment, a common residual NAPL field was established, followed by a series of mobilization and solubilization experiments. Mobilization floods included pure water floods with variable flow rates and surfactant floods with variations in surfactant formulations. At relatively low capillary numbers (N{sub ca}<10{sup {minus}3}), the surfactant mobilization floods resulted in higher NAPL saturations than for the pure water flood, for similar N{sub ca}.These differences in macroscopic saturations are explained by differences in micro-scale mobilization processes. Solubilization of the residual NAPL remaining after the mobilization stage was dominated by the formation of dissolution fingers, which produced nonequilibrium NAPL solubilization. A macroemulsion phase also as observed to form spontaneously and persist during the solubilization stage of the experiments.

  11. SURFACTANT ENHANCED RECOVERY OF TETRACHLOROETHYLENE FROM A POROUS MEDIUM CONTAINING LOW PERMEABILITY LENSES. 2. NUMERICAL SIMULATION. (R825409)

    EPA Science Inventory

    Abstract

    A numerical model of surfactant enhanced solubilization was developed and applied to the simulation of nonaqueous phase liquid recovery in two-dimensional heterogeneous laboratory sand tank systems. Model parameters were derived from independent, small-scale, ...

  12. Membrane emulsification to produce perfume microcapsules

    NASA Astrophysics Data System (ADS)

    Pan, Xuemiao

    Microencapsulation is an efficient technology to deliver perfume oils from consumer products onto the surface of fabrics. Microcapsules having uniform size/mechanical strength, may provide better release performance. Membrane emulsification in a dispersion cell followed by in-situ polymerization was used to prepare narrow size distribution melamine-formaldehyde (MF) microcapsules containing several types of oil-based fragrances or ingredients. Investigated in this study are the parameters impacting to the size and size distribution of the droplets and final MF microcapsules. A pilot plant-scale cross-flow membrane system was also used to produce MF microcapsules, demonstrating that the membrane emulsification process has potential to be scaled up for industrial applications. In this study, health and environmental friendly poly (methyl methacrylate) (PMMA) microcapsules with narrow size distribution were also prepared for the first time using the dispersion cell membrane emulsification system. Characterization methods previously used for thin-shell microcapsules were expanded to analyse microcapsules with thick shells. The intrinsic mechanical properties of thick shells were determined using a micromanipulation technique and finite element analysis (FEM). The microcapsules structure was also considered in the determination of the permeability and diffusivity of the perfume oils in good solvents..

  13. Partitioning of phenanthrene into surfactant hemi-micelles on the bacterial cell surface and implications for surfactant-enhanced biodegradation.

    PubMed

    Lanzon, Jacquelyn B; Brown, Derick G

    2013-09-01

    Recent studies have suggested that the ability of a surfactant to enhance the bioavailability of hydrophobic organic compounds (HOC) requires the formation of surfactant hemi-micelles on the bacterial cell surface and subsequent partitioning of HOC into the hemi-micelles. However, the studies did not provide direct evidence of HOC partitioning into surfactant hemi-micelles on the bacterial cell surface. In this study, direct evidence is provided to demonstrate that the nonionic surfactant Brij 30 forms hemi-micelles on the bacterial cell surface and that phenanthrene sorption at the bacterial surface is enhanced by the surfactant. These results are in agreement with the current theory describing surfactant-enhanced HOC bioavailability. This enhanced bioavailability is put into context with microbial kinetics and system partitioning processes, and it is demonstrated that the addition of surfactant can enhance, have no effect, or inhibit HOC biodegradation depending upon surfactant concentration and microbial growth rate. Understanding these non-linear relationships between surfactant-enhanced HOC bioavailability, biodegradation kinetics, and system partitioning will assist in the design and implementation of surfactant-enhanced bioremediation programs. PMID:23764610

  14. DEMONSTRATION OF PILOT-SCALE PERVAPORATION SYSTEMS FOR VOLATILE ORGANIC COMPOUND REMOVAL FROM A SURFACTANT ENHANCED AQUIFER REMEDIATION FLUID. II. HOLLOW FIBER MEMBRANE MODULES

    EPA Science Inventory

    Pilot-scale demonstration of pervaporation-based removal of volatile organic compounds from a surfactant enhanced aquifer remediation (SEAR) fluid has been conducted at USEPA's Test & Evaluation Facility using hollow fiber membrane modules. The membranes consisted of microporous...

  15. Field demonstration of surfactant-enhanced solubilization of DNAPL at Dover Air Force Base, Delaware

    NASA Astrophysics Data System (ADS)

    Childs, Jeffrey; Acosta, Edgar; Annable, Michael D.; Brooks, Michael C.; Enfield, Carl G.; Harwell, Jeffrey H.; Hasegawa, Mark; Knox, Robert C.; Rao, P. Suresh C.; Sabatini, David A.; Shiau, Ben; Szekeres, Erika; Wood, A. Lynn

    2006-01-01

    This study reports on a surfactant-based flood for tetrachloroethylene (PCE) removal from a control test cell at the Dover National Test Site. The surfactant formulation (sodium dihexyl sulfosuccinate (Aerosol-MA® or AMA), isopropanol and calcium chloride) was able to achieve a high concentration of PCE in swollen micelles (supersolubilization) without vertical PCE migration. The hydraulic system included eight screened wells that were operated in both vertical circulation and line drive configurations. After 10 pore volumes of flushing, the overall PCE removal was 68% (65% of which corresponded to the surfactant flooding alone). In addition, the residual PCE saturation was reduced from 0.7% to 0.2%, and the concentration of PCE in the groundwater was reduced from 37-190 mg/L before the flushing to 7.3 mg/L after flooding. Recycling the surfactant solution reduced the required surfactant mass (and thus cost, and waste) by 90%. Close to 80% of the total PCE removal was obtained during the first five pore volumes which were operated in an upward vertical circulation flow scheme. No free oil phase was observed during the test. Further analysis of multilevel sampler data suggests that most of the trapped oil remaining in the cell was likely localized in secluded regions of the aquifer, which helps explain the lower PCE groundwater concentration after remedial activities. In summary, this field study demonstrated the feasibility of surfactant-enhanced remediation to reduce the mass in the source zone and significantly reduce the PCE aqueous concentration and therefore the risk associated with the contaminant plume.

  16. Nano-encapsulated PCM via Pickering Emulsification

    NASA Astrophysics Data System (ADS)

    Wang, Xuezhen; Zhang, Lecheng; Yu, Yi-Hsien; Jia, Lisi; Sam Mannan, M.; Chen, Ying; Cheng, Zhengdong

    2015-08-01

    We designed a two-step Pickering emulsification procedure to create nano-encapsulated phase changing materials (NEPCMs) using a method whose simplicity and low energy consumption suggest promise for scale-up and mass production. Surface-modified amphiphilic zirconium phosphate (ZrP) platelets were fabricated as the Pickering emulsifiers, nonadecane was chosen as the core phase change material (PCM), and polystyrene, the shell material. The resultant capsules were submicron in size with remarkable uniformity in size distribution, which has rarely been reported. Differential scanning calorimetry (DSC) characterization showed that the capsulation efficiency of NEPCMs, and they were found to be thermal stable, as characterized by the DSC data for the sample after 200 thermal cycles. NEPCMs exhibit superior mechanical stability and mobility when compared with the well-developed micro-encapsulated phase change materials (MEPCMs). NEPCMs find useful applications in thermal management, including micro-channel coolants; solar energy storage media; building temperature regulators; and thermal transfer fabrics.

  17. Effect of cation exchange on surfactant-enhanced solubilization of trichloroethene

    NASA Astrophysics Data System (ADS)

    Field, J. A.; Sawyer, T. E.; Schroth, M. H.; Humphrey, M. D.; Istok, J. D.

    2000-11-01

    The objective of this study was to develop the single-well push-pull test as a diagnostic tool for assessing the potential for cation exchange to adversely affect the phase behavior of sodium dihexyl sulfosuccinate surfactant (Aerosol MA 80-I) and its solubilization of trichloroethene (TCE) in the subsurface. Laboratory push-pull tests were conducted on a model natural aquifer sediment collected from a TCE-contaminated field site and a test solution consisting of 36,800 mg/l (3.7 wt.%) sulfosuccinate, 100,000 mg/l (10 wt.%) isopropanol, and 3200 mg/l (0.32 wt.%) KBr. Laboratory experiments were designed to simulate conditions occurring during single-well, "push-pull" tests. In batch experiments conducted in the presence of excess TCE, the test solution gave a Winsor Type I system with an enhanced aqueous TCE solubility of 26,700 mg/l and a solution density of 1.000 g/cm 3. The sulfosuccinate surfactant was transported conservatively in sediment packs containing no TCE. However, increasing concentrations of Ca 2+ and Mg 2+ resulting from cation exchange caused the TCE solubilization potential of the injected surfactant to exceed values predicted from the solubilization isotherm. Sulfosuccinate surfactant transport was strongly retarded in sediment packs containing 5 vol.% residual TCE because cation exchange resulted in the formation of a Winsor Type II system, which resulted in the partitioning of the sulfosuccinate surfactant into the residual TCE phase. Conservative sulfosuccinate transport was observed in a separate sediment pack containing 5 vol.% residual TCE when a 130 meq/l Na + pre-flush was used to reduce quantities of Ca 2+ and Mg 2+ in the sediment pack prior to sulfosuccinate injection. The results of this study emphasize the importance of cation exchange on the performance of surfactant-enhanced TCE solubilization and demonstrate the utility of the push-pull test for predicting the potentially deleterious effects of cation exchange on surfactant phase

  18. Low-frequency ac electro-flow-focusing microfluidic emulsification

    NASA Astrophysics Data System (ADS)

    He, Peng; Kim, Haejune; Luo, Dawei; Marquez, Manuel; Cheng, Zhengdong

    2010-04-01

    Applications of electric field, using either dc or high-frequency ac field, have shown many advantages in emulsification. We further develop this technique by a detailed study on low-frequency ac electro-flow-focusing (EFF) microfluidic emulsification. Counter-intuitively, the droplet size variation is not monotonic with the electric field, in contrary to the dc-EFF emulsification. This phenomenon originates from a relaxation oscillation of flow rate through the Taylor cone. Particularly, a continuous droplet size decrease was obtained at the voltage ramp-up stage. This emulsification process was modeled in analog to the accumulation and release of charges in an RC electric circuit with an adjustable resistor.

  19. Nano-encapsulated PCM via Pickering Emulsification.

    PubMed

    Wang, Xuezhen; Zhang, Lecheng; Yu, Yi-Hsien; Jia, Lisi; Sam Mannan, M; Chen, Ying; Cheng, Zhengdong

    2015-01-01

    We designed a two-step Pickering emulsification procedure to create nano-encapsulated phase changing materials (NEPCMs) using a method whose simplicity and low energy consumption suggest promise for scale-up and mass production. Surface-modified amphiphilic zirconium phosphate (ZrP) platelets were fabricated as the Pickering emulsifiers, nonadecane was chosen as the core phase change material (PCM), and polystyrene, the shell material. The resultant capsules were submicron in size with remarkable uniformity in size distribution, which has rarely been reported. Differential scanning calorimetry (DSC) characterization showed that the capsulation efficiency of NEPCMs, and they were found to be thermal stable, as characterized by the DSC data for the sample after 200 thermal cycles. NEPCMs exhibit superior mechanical stability and mobility when compared with the well-developed micro-encapsulated phase change materials (MEPCMs). NEPCMs find useful applications in thermal management, including micro-channel coolants; solar energy storage media; building temperature regulators; and thermal transfer fabrics. PMID:26278332

  20. Nano-encapsulated PCM via Pickering Emulsification

    PubMed Central

    Wang, Xuezhen; Zhang, Lecheng; Yu, Yi-Hsien; Jia, Lisi; Sam Mannan, M.; Chen, Ying; Cheng, Zhengdong

    2015-01-01

    We designed a two-step Pickering emulsification procedure to create nano-encapsulated phase changing materials (NEPCMs) using a method whose simplicity and low energy consumption suggest promise for scale-up and mass production. Surface-modified amphiphilic zirconium phosphate (ZrP) platelets were fabricated as the Pickering emulsifiers, nonadecane was chosen as the core phase change material (PCM), and polystyrene, the shell material. The resultant capsules were submicron in size with remarkable uniformity in size distribution, which has rarely been reported. Differential scanning calorimetry (DSC) characterization showed that the capsulation efficiency of NEPCMs, and they were found to be thermal stable, as characterized by the DSC data for the sample after 200 thermal cycles. NEPCMs exhibit superior mechanical stability and mobility when compared with the well-developed micro-encapsulated phase change materials (MEPCMs). NEPCMs find useful applications in thermal management, including micro-channel coolants; solar energy storage media; building temperature regulators; and thermal transfer fabrics. PMID:26278332

  1. Pentachlorophenol removal from water using surfactant-enhanced filtration through low-pressure thin film composite membranes.

    PubMed

    Kumar, Yogesh; Popat, K M; Brahmbhatt, H; Ganguly, B; Bhattacharya, A

    2008-06-15

    Removal of pentachlorophenol from water is investigated using the surfactant-enhanced cross-flow membrane filtration technique in which anionic surfactant; sodium dodecyl sulfate (SDS) is the carrier of pentachlorophenol. The separation performances are studied by varying SDS concentrations (

  2. DEMONSTRATION OF PILOT-SCALE PREVAPORATION SYSTEMS FOR VOLATILE ORGANIC COMPOUND REMOVAL FROM A SURFACTANT ENHANCED AQUIFER REMEDIATION FLUID. I. SPIRAL WOUND MEMBRANE MODULES

    EPA Science Inventory

    During the summer of 1996, a pilot-scale demonstration of a surfactant enhanced aquifer remediation (SEAR) process for removal of dense non-aqueous phase liquids (DNAPLs) from soils was conducted at Hill Air Force Base in Layton, Utah. Five thousand gallons of the extracted DNAP...

  3. Researches and applications of the ultrasonic emulsifications and dispersions.

    PubMed

    Quanlu, Li; Yinhong, Zhang; Jing, Wu

    2013-11-01

    This paper defines power ultrasonics and their two important directions: Ultrasonic emulsification and dispersion from a practical point of view, brief reports on recent research results are ultrasonic emulsification to be used for the preparation of composite electrorheological fluid, and ultrasonic dispersion to be used dispersion as a new type cold cloud catalytic agent metaldehyde [CH3CH]4-6 (this is used for artificial rain), etc., and produce good results or gain progress. Then, the principle and applications of power ultrasonics (including magnetostriction type ultrasonic transducer and piezoelectric type ultrasonic transducer) in the emulsification or dispersion, are pointed out. Also, ultrasonic extensive applications in chemistry, materials, and life sciences are briefly introduced. PMID:24180765

  4. Fabrication of a uniformly sized fenofibrate microemulsion by membrane emulsification.

    PubMed

    Pradhan, Roshan; Lee, Dong Won; Choi, Han-Gon; Yong, Chul Soon; Kim, Jong Oh

    2013-01-01

    Fenofibrate-loaded microemulsions composed of Labrafil M 1944 CS, Capryol PGMC and fenofibrate as the dispersed phase and Labrasol in demineralised water as the continuous phase were prepared by utilising a Shirasu-porous-glass (SPG) membrane emulsification technique. The process parameters were optimised by adjusting the feed pressure (15-45 kPa), agitator speed (250-800 rpm) and temperature of the continuous phase (25-45°C). As a result, narrowly distributed microemulsions were obtained via SPG membrane emulsification at an agitator speed of 250 rpm, a feed pressure of 30 kPa and a continuous phase temperature of 25°C. Furthermore, TEM images clearly showed that the microemulsion prepared by SPG membrane emulsification had a uniform, spherical morphology with a narrow size distribution. Our results indicated that the SPG membrane emulsification technique is highly efficient for the preparation of narrowly distributed microemulsions with relatively smaller particle sizes compared with the common stirring method. PMID:22657749

  5. Structured microparticles with tailored properties produced by membrane emulsification.

    PubMed

    Vladisavljević, Goran T

    2015-11-01

    This paper provides an overview of membrane emulsification routes for fabrication of structured microparticles with tailored properties for specific applications. Direct (bottom-up) and premix (top-down) membrane emulsification processes are discussed including operational, formulation and membrane factors that control the droplet size and droplet generation regimes. A special emphasis was put on different methods of controlled shear generation on membrane surface, such as cross flow on the membrane surface, swirl flow, forward and backward flow pulsations in the continuous phase and membrane oscillations and rotations. Droplets produced by membrane emulsification can be used for synthesis of particles with versatile morphology (solid and hollow, matrix and core/shell, spherical and non-spherical, porous and coherent, composite and homogeneous), which can be surface functionalised and coated or loaded with macromolecules, nanoparticles, quantum dots, drugs, phase change materials and high molecular weight gases to achieve controlled/targeted drug release and impart special optical, chemical, electrical, acoustic, thermal and magnetic properties. The template emulsions including metal-in-oil, solid-in-oil-in-water, oil-in-oil, multilayer, and Pickering emulsions can be produced with high encapsulation efficiency of encapsulated materials and narrow size distribution and transformed into structured particles using a variety of solidification processes, such as polymerisation (suspension, mini-emulsion, interfacial and in-situ), ionic gelation, chemical crosslinking, melt solidification, internal phase separation, layer-by-layer electrostatic deposition, particle self-assembly, complex coacervation, spray drying, sol-gel processing, and molecular imprinting. Particles fabricated from droplets produced by membrane emulsification include nanoclusters, colloidosomes, carbon aerogel particles, nanoshells, polymeric (molecularly imprinted, hypercrosslinked, Janus and core

  6. Investigation of surfactant-enhanced dissolution of entrapped nonaqueous phase liquid chemicals in a two-dimensional groundwater flow field.

    PubMed

    Saba, T; Illangasekare, T H; Ewing, J

    2001-09-01

    Because of their low solubility, waste chemicals in the form of nonaqueous phase liquids (NAPLs) that are entrapped in subsurface formations act as long-term sources of groundwater contamination. In the design of remediation schemes that use surfactants, it is necessary to estimate the mass transfer rate coefficients under multi-dimensional flow fields that exit at field sites. In this study, we investigate mass transfer under a two-dimensional flow field to obtain an understanding of the basic mechanisms of surfactant-enhanced dissolution and to quantify the mass transfer rates. Enhanced dissolution experiments in a two-dimensional test cell were conducted to measure rates of mass depletion from entrapped NAPLs to a flowing aqueous phase containing a surfactant. In situ measurement of transient saturation changes using a gamma attenuation system revealed dissolution patterns that are affected by the dimensionality of the groundwater flow field. Numerical modeling of local flow fields that changed with time, due to depletion of NAPL sources, enabled the examination of the basic mechanisms of NAPL dissolution in complex groundwater systems. Through nonlinear regression analysis, mass transfer rates were correlated to porous media properties, NAPL saturation and aqueous phase velocity. Results from the experiments and numerical analyses were used to identify deficiencies in existing methods of analysis that uses assumptions of one-dimensional flow, homogeneity of aquifer properties, local equilibrium and idealized transient mass transfer. PMID:11530927

  7. Shifts in microbial community structure during in situ surfactant-enhanced bioremediation of polycyclic aromatic hydrocarbon-contaminated soil.

    PubMed

    Wang, Lingwen; Li, Feng; Zhan, Yu; Zhu, Lizhong

    2016-07-01

    This study aims to reveal the microbial mechanism of in situ surfactant-enhanced bioremediation (SEBR). Various concentrations of rhamnolipids, Tween 80, and sodium dodecyl benzenesulfonate (SDBS) were separately sprayed onto soils contaminated with polycyclic aromatic hydrocarbons (PAHs) for years. Within 90 days, the highest level of degradation (95 %) was observed in the soil treated with rhamnolipids (10 mg/kg), followed by 92 % degradation with Tween 80 (50 mg/kg) and 90 % degradation with SDBS (50 mg/kg). The results of the microbial phospholipid fatty acids (PLFAs) suggest that bacteria dominated the enhanced PAH biodegradation (94 % of the maximum contribution). The shift of bacterial community structure during the surfactant treatment was analyzed by using the 16S rRNA gene high-throughput sequencing. In the presence of surfactants, the number of the operational taxonomic units (OTUs) associated with Bacillus, Pseudomonas, and Sphingomonas increased from 2-3 to 15-30 % at the end of the experiment (two to three times of control). Gene prediction with phylogenetic investigation of communities by reconstruction of unobserved states (PICRUSt) shows that the PAH-degrading genes, such as 1-hydroxy-2-naphthoate dioxygenase and PAH dioxygenase large subunit, significantly increased after the surfactant applications (p < 0.05). The findings of this study provide insights into the surfactant-induced shifts of microbial community, as well as critical factors for efficient bioremediation. PMID:27068902

  8. The effect of polymer-surfactant interaction on the rheological properties of surfactant enhanced alkaline flooding formulations

    SciTech Connect

    French, T.R.; Josephson, C.B.

    1993-02-01

    Surfactant-enhanced, lower pH (weak) alkaline chemicals are effective for mobilizing residual oil. Polymer is used for mobility control because if mobility control is lost, then oil recovery is reduced. The ability to maintain mobility control during surfactant-alkaline flooding can be adversely affected by chemical interaction. In this work, interaction between polymers and surfactants was shown to be affected by pH, ionic strength, crude oil, and the properties of the polymers and surfactants. Polymer-surfactant interaction (phase separation, precipitation, and viscosity loss) occurred between most of the polymers and surfactants that were tested. Polymer-surfactant interaction is difficult to eliminate, and no method was found for completely eliminating interaction. Polymer-surfactant interaction occurred at optimal salinity and below optimal salinity. Polymer-surfactant interaction had an adverse effect on polymer rheology; however, the adverse effect of interaction on polymer rheology was lessened when oil was present. Increasing the pH of chemical systems further reduced the adverse effects of interaction on polymer rheology.

  9. Emulsification in turbulent flow: 3. Daughter drop-size distribution.

    PubMed

    Tcholakova, Slavka; Vankova, Nina; Denkov, Nikolai D; Danner, Thomas

    2007-06-15

    Systematic set of experiments is performed to clarify the effects of several factors on the size distribution of the daughter drops, which are formed as a result of drop breakage during emulsification in turbulent flow. The effects of oil viscosity, etaD, interfacial tension, sigma, and rate of energy dissipation in the turbulent flow, epsilon, are studied. As starting oil-water premixes we use emulsions containing monodisperse oil drops, which have been generated by membrane emulsification. By passing these premixes through a narrow-gap homogenizer, working in turbulent regime of emulsification, we monitor the changes in the drop-size distribution with the emulsification time. The experimental data are analyzed by using a new numerical procedure, which is based on the assumption (supported by the experimental data) that the probability for formation of daughter drops with diameter smaller than the maximum diameter of the stable drops, demulsification time. We found that the breakage of a single "mother" drop leads to the formation of multiple daughter drops, and that the number and size distribution of these daughter drops depend strongly on the viscosity of the dispersed phase. Different scaling laws are found to describe the experimental results for the oils of low and high viscosity. The obtained results for the daughter drop-size distribution are in a reasonably good agreement with the experimental results reported by other authors. In contrast, the comparison with several basic model functions, proposed in the literature, does not show good agreement and the possible reasons are discussed. The proposed numerical procedure allows us to describe accurately the evolution of all main characteristics of the drop-size distribution during emulsification, such as the number and volume averaged diameters, and the distributive and cumulative functions by

  10. Methodological aspects of sample preparation for the determination of carbamate residues: a review.

    PubMed

    Santaladchaiyakit, Yanawath; Srijaranai, Supalax; Burakham, Rodjana

    2012-09-01

    This review covers recent developments in sample preparations and analytical techniques for determination of residues of carbamate pesticides. Special attention is paid to the newly established microextraction techniques, including cloud-point extraction, dispersive liquid-liquid microextraction, and ultrasound-assisted surfactant-enhanced emulsification microextraction. In addition, extractions using a variety of solvents, as well as miniaturized and on-line sample preparation systems, are discussed. Applications of the different methods for the determination of carbamate pesticide residues in food and environmental matrices are included. PMID:22997028

  11. Effect of back pressure on emulsification of lipid nanodispersions in a high-pressure homogenizer.

    PubMed

    Saheki, Akira; Seki, Junzo; Nakanishi, Takeo; Tamai, Ikumi

    2012-01-17

    We examined the effect of 0-20% back pressure, which functions as a resistance to emulsification in a high-pressure homogenizer, on emulsification of lipid nanodispersions (emulsion and liposomes) less than 100 nm in diameter. Back pressure in the range of 0.9-3.8% of the emulsification pressure enhanced the emulsification, and the particle diameter of lipid nanodispersion was the smallest at 2% back pressure. The back pressure effect was independent of the actual pressure, which was regarded as the difference between the emulsification and the back pressures. The mechanism of the back pressure effect was considered to be enhancement of emulsification by suppression of collapse cavitation in the high-pressure emulsification module. This back pressure effect appeared in emulsification of emulsion and liposomes, and was seen predominantly in the early emulsification phase (within 10 passages). The particles of lipid nanodispersions prepared at 2% back pressure with adequate re-circulation achieved physicochemically optimal diameter with a narrow size distribution, and were more stable at 60°C for 7 days than particles prepared with 20% back pressure. Our results indicate that emulsification with a low level of back pressure is effective for production of stable lipid nanodispersions with narrow size distribution. PMID:22108638

  12. Coalescence during emulsification. 2. Role of small molecule surfactants.

    PubMed

    Lobo, Lloyd; Svereika, Aileen

    2003-05-15

    An oil-soluble hexadecyl pyrene (HDP) probe is used to monitor coalescence of hexadecane oil-in-water emulsions, during emulsification, in stirred systems and in a high-pressure homogenizer (microfluidizer), when small molecule surfactants are used as emulsifiers. The effect of sodium dodecyl sulfate concentration and salt concentration on the amount of coalescence and final drop size is studied. The behavior of oil-soluble surfactants and mixtures of oil-soluble and water-soluble surfactants on emulsification performance is also discussed. For high-pressure homogenizers, the drop sizes obtained are found to depend mostly on the ability of surfactants to stabilize the drops against coalescence, rather than their ability to reduce the interfacial tension. Increasing oil phase fractions increase the coalescence rate, because of the increase in collision frequency, which, in turn, impacts the drop size of the homogenized emulsion. PMID:16256561

  13. Emulsification in turbulent flow 2. Breakage rate constants.

    PubMed

    Vankova, Nina; Tcholakova, Slavka; Denkov, Nikolai D; Vulchev, Vassil D; Danner, Thomas

    2007-09-15

    Systematic experimental study of the effects of several factors on the breakage rate constant, k(BR), during emulsification in turbulent flow is performed. These factors are the drop size, interfacial tension, viscosity of the oil phase, and rate of energy dissipation in the flow. As starting oil-water premixes we use emulsions containing monodisperse oil drops, which have been generated by the method of membrane emulsification. By passing these premixes through a narrow-gap homogenizer, working in turbulent regime of emulsification, we study the evolution of the number concentration of the drops with given diameter, as a function of the emulsification time. The experimental data are analyzed by a kinetic scheme, which takes into account the generation of drops of a given size (as a result of breakage of larger drops) and their disappearance (as a result of their own breakage process). The experimental results for k(BR) are compared with theoretical expressions from the literature and their modifications. The results for all systems could be described reasonably well by an explicit expression, which is a product of: (a) the frequency of collisions between drops and turbulent eddies of similar size, and (b) the efficiency of drop breakage, which depends on the energy required for drop deformation. The drop deformation energy contains two contributions, originating from the drop surface extension and from the viscous dissipation inside the breaking drop. In the related subsequent paper, the size distribution of the daughter drops formed in the process of drop breakage is analyzed for the same experimental systems. PMID:17553511

  14. Controlled double emulsification utilizing 3D PDMS microchannels

    NASA Astrophysics Data System (ADS)

    Chang, Fu-Che; Su, Yu-Chuan

    2008-06-01

    This paper presents a PDMS emulsification device that is capable of generating water-in-oil-in-water double emulsions in a controlled manner. Specially designed 3D microchannels are utilized to steer the independently driven water- and oil-phase flows (especially to restrict the attachment of the middle oil-phase flow on the channel surfaces), and to break the continuous flows into monodisperse double emulsions. In addition to channel geometries and fluid flow rates, surfactants and osmotic agents are employed to facilitate the breakup process and stabilize the resulting emulsion structures. In the prototype demonstration, two-level SU-8 molds were fabricated to duplicate PDMS microstructures, which were surface treated and bonded irreversibly to form 3D microchannels. Throughout the emulsification trials, dripping was intentionally induced to generate monodisperse double emulsions with single or multiple aqueous droplets inside each oil drop. It is found that the overall and core sizes of the resulting double emulsions could be adjusted independently, mainly by varying the outer and inner fluid flow rates, respectively. As such, the presented double emulsification device could potentially realize the controllability on emulsion structure and size distribution, which is desired for a variety of biological and pharmaceutical applications.

  15. Thin-film microextraction.

    PubMed

    Bruheim, Inge; Liu, Xiaochuan; Pawliszyn, Janusz

    2003-02-15

    The properties of a thin sheet of poly(dimethylsiloxane) (PDMS) membrane as an extraction phase were examined and compared to solid-phase microextraction (SPME) PDMS-coated fiber for application to semivolatile analytes in direct and headspace modes. This new PDMS extraction approach showed much higher extraction rates because of the larger surface area to extraction-phase volume ratio of the thin film. Unlike the coated rod formats of SPME using thick coatings, the high extraction rate of the membrane SPME technique allows larger amounts of analytes to be extracted within a short period of time. Therefore, higher extraction efficiency and sensitivity can be achieved without sacrificing analysis time. In direct membrane SPME extraction, a linear relationship was found between the initial rate of extraction and the surface area of the extraction phase. However, for headspace extraction, the rates were somewhat lower because of the resistance to analyte transport at the sample matrix/headspace barrier. It was found that the effect of this barrier could be reduced by increasing either agitation, temperature, or surface area of the sample matrix/headspace interface. A method for the determination of PAHs in spiked lake water samples was developed based on the membrane PDMS extraction coupled with GC/MS. A linearity of 0.9960 and detection limits in the low-ppt level were found. The reproducibility was found to vary from 2.8% to 10.7%. PMID:12622398

  16. Microextraction of priority pollutants

    SciTech Connect

    Leepipatriboon, S.

    1984-01-01

    Some of the priority pollutants, e.g., aromatic hydrocarbons, halogenated aromatic hydrocarbons and halogenated alkanes and alkenes have been studied by a microextraction technique. The compounds studied were benzene, toluene, and ethylbenzene for aromatic hydrocarbons; chlorobenzene, m-dichlorobenzene, p-dichlorobenzene, and o-dichlorobenzene for halogenated aromatic hydrocarbons; and trans-1,2-dichloroethylene, 1,1-dichloroethane, 1,1,2,2-tetrachloroethane, choloroform, ethylene chloride, 1,1,1-trichloroethane, carbon tetrachloride, methylene chloride, bromodichloromethane, 1,2-dichloropropane, trichloroethylene and bromoform for halogenated alkanes and alkenes. The organic solvent-to-water sample ratios of study were 1:9, 5:5 and 8:2, respectively. Solvent extractability effect of carbon disulfide, methylene chloride and hexane or iso-octane and the effect of salts, e.g., saturated sodium chloride solution, saturated sodium sulfate solution, 2.00 g of sodium chloride and 2.00 g of sodium sulfate on the percent recovery were investigated in this study. This technique is based on the extraction into an organic solvent phase followed by the measurement of the peak area by a flame ionization detector. Gas chromatography and the internal standard technique were used throughout the stud. The gas chromatographic conditions for each system of study were reported. The standard deviation of this study ranged from 1-16%. The distribution constant, K{sub D}, and the results of percent recovery for each compound are discussed.

  17. Tandem dispersive liquid-liquid microextraction as an efficient method for determination of basic drugs in complicated matrices.

    PubMed

    Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Saffarzadeh, Zahra; Asghari, Alireza

    2016-01-15

    A simple and efficient approach is introduced for the improvement of the clean-up and applicability of the dispersive liquid-liquid microextraction (DLLME) method in complicated matrices. For this purpose, two dispersive microextraction methods were combined, and the tandem dispersive liquid-liquid microextraction (TDLLME) method was provided. At first, using the ultrasound-assisted emulsification microextraction (USAEME) method, the tricyclic anti-depressant (TCA) drugs nortriptyline, imipramine, and amitriptyline, as the model compounds, contained in an aqueous sample solution (8.0 mL), were extracted into an organic solvent (35 μL). Then by utilizing the air-agitated liquid-liquid microextraction (AALLME) method, these analytes were simply back-extracted into 50 μL of an aqueous acceptor phase. By performing this convenient extraction method, a high sample clean-up was obtained; the overall extraction time was 7 min. The back-extraction step could be performed in less than 2 min, and very simple tools were required for this purpose. The response surface methodology (RSM) was used for the optimization of the experimental parameters so that the volumes 95 and 50 μL were obtained for the organic solvent and the acceptor phase, respectively, and the pH values of 11.25 and 1.75 were obtained for the donor and acceptor phases, respectively, as the optimal extraction conditions. Under the optimized conditions, TDLLME-HPLC-UV provided a good linearity in the range of 2.5-5000 ng mL(-1), low limits of detection (0.7-1.0 ng mL(-1)), good extraction repeatabilities (relative standard deviations below 6.2%, n=5), and enrichment factors (EFs) of 50-101. Finally, the developed method was successfully used for the determination of the mentioned drugs in the wastewater and human plasma samples. PMID:26711155

  18. Surfactant-enhanced bioremediation

    SciTech Connect

    Churchill, P.F.; Dudley, R.J.; Churchill, S.A.

    1995-12-31

    This study was undertaken to examine the effect of three structurally related, non-ionic surfactants, Triton X-45, Triton X-100 and Triton X-165, as well as the oleophilic fertilizer, Inipol EAP 22, on the rate of biodegradation of phenanthrene by pure bacterial cultures. Each surfactant dramatically increased the apparent aqueous solubility of phenanthrene. Model studies were conducted to investigate the ability of these surfactants to enhance the rate of transport and uptake of polycyclic aromatic hydrocarbons into bacterial cells, and to assess the impact that increasing the aqueous solubility of hydrocarbons has on their rate of biodegradation. The results indicate that increasing the apparent aqueous solubility of hydrocarbons can lead to enhanced biodegradation rates by two Pseudomonas saccharophila strains. However, the experiments also suggest that some surfactants can inhibit aromatic hydrocarbon biodegradation by certain bacteria. The data also support the hypothesis that surface-active components present in the oleophilic fertilizer formulation, Inipol EAP 22, may have significantly contributed to the positive results reported in tests of remedial agent impact on bioremediation, which was used as a supplemental clean-up technology on Exxon Valdez crude oil-contaminated Alaskan beaches.

  19. Dispersive suspended microextraction.

    PubMed

    Yang, Zhong-Hua; Liu, Yu; Lu, Yue-Le; Wu, Tong; Zhou, Zhi-Qiang; Liu, Dong-Hui

    2011-11-14

    A novel sample pre-treatment technique termed dispersive suspended microextraction (DSME) coupled with gas chromatography-flame photometric detection (GC-FPD) has been developed for the determination of eight organophosphorus pesticides (ethoprophos, malathion, chlorpyrifos, isocarbophos, methidathion, fenamiphos, profenofos, triazophos) in aqueous samples. In this method, both extraction and two phases' separation process were performed by the assistance of magnetic stirring. After separating the two phases, 1 μL of the suspended phase was injected into GC for further instrument analysis. Varieties of experiment factors which could affect the experiment results were optimized and the following were selected: 12.0 μL p-xylene was selected as extraction solvent, extraction speed was 1200 rpm, extraction time was 30 s, the restoration speed was 800 rpm, the restoration time was 8 min, and no salt was added. Under the optimum conditions, limits of detections (LODs) varied between 0.01 and 0.05 μg L(-1). The relative standard deviation (RSDs, n=6) ranged from 4.6% to 12.1%. The linearity was obtained by five points in the concentration range of 0.1-100.0 μg L(-1). Correlation coefficients (r) varied from 0.9964 to 0.9995. The enrichment factors (EFs) were between 206 and 243. In the final experiment, the developed method has been successfully applied to the determination of organophosphorus pesticides in wine and tap water samples and the obtained recoveries were between 83.8% and 101.3%. Compared with other pre-treatment methods, DSME has its own features and could achieve satisfied results for the analysis of trace components in complicated matrices. PMID:22023861

  20. Some Physicochemical Remarks on Spontaneous Emulsification of Vitreal Tamponades

    PubMed Central

    dell'Omo, Roberto; Zeppa, Lucio; Bufalo, Gennaro; Cardone, Michele; Romano, Mario; Ambrosone, Luigi

    2014-01-01

    The importance of gravitational instability in determining the emulsification of vitreal tamponades is discussed. Theoretical results and numerical simulations indicate that the spontaneous formation of water-silicon oil is a rare event and that the very low concentration of surface active agents cannot justify the systematic formation of emulsions. The gravitational instabilities seem to play the main role. Our theoretical results seem in agreement with the experimental evidences; furthermore they indicate a future research line for the improvement of endotamponades. Indeed, the use of biodegradable antifoam may avoid the formation of bubbles and delay the formation of emulsions. PMID:25133159

  1. Some physicochemical remarks on spontaneous emulsification of vitreal tamponades.

    PubMed

    Costagliola, Ciro; Semeraro, Francesco; dell'Omo, Roberto; Zeppa, Lucio; Bufalo, Gennaro; Cardone, Michele; Romano, Mario; Ambrosone, Luigi

    2014-01-01

    The importance of gravitational instability in determining the emulsification of vitreal tamponades is discussed. Theoretical results and numerical simulations indicate that the spontaneous formation of water-silicon oil is a rare event and that the very low concentration of surface active agents cannot justify the systematic formation of emulsions. The gravitational instabilities seem to play the main role. Our theoretical results seem in agreement with the experimental evidences; furthermore they indicate a future research line for the improvement of endotamponades. Indeed, the use of biodegradable antifoam may avoid the formation of bubbles and delay the formation of emulsions. PMID:25133159

  2. Ultrasound-assisted liquid-phase microextraction based on a nanostructured supramolecular solvent.

    PubMed

    Moradi, Morteza; Yamini, Yadollah; Tayyebi, Moslem; Asiabi, Hamid

    2013-05-01

    Novel ultrasonically enhanced supramolecular solvent microextraction (USESSM) then high-performance liquid chromatography with ultraviolet detection have been used for extraction and determination of phthalates in water and cosmetics. Coacervates consisting of decanoic acid-based nano-structured aggregates, specifically reverse micelles, have been used the first time as solvents for ultrasound-assisted emulsification microextraction (USAEME). Sonication accelerated mass transfer of the target analytes into the nano-structured solvent from the aqueous sample, thus reducing extraction time. Several conditions affecting extraction efficiency, for example the concentrations of major components of the supramolecular solvent (tetrahydrofuran and decanoic acid), sample solution pH, salt addition, and ultrasonication time, were investigated and optimized. Under the optimum conditions, preconcentration of the analytes ranged from 176 to 412-fold and the linear range was 0.5-100 μg L(-1), with correlation coefficients (R(2)) ≥ 0.9984. The detection sensitivity of the method was excellent, with limits of detection (LOD, S/N = 3) in the range 0.10-0.70 μg L(-1) and precision in the range 4.1-11.7 % (RSD, n = 5). This method was successfully used for analysis of phthalates in water and cosmetics, with good recovery of spiked phthalates (91.0-108.5 %). PMID:23417551

  3. Manufacture of poly(methyl methacrylate) microspheres using membrane emulsification.

    PubMed

    Bux, Jaiyana; Manga, Mohamed S; Hunter, Timothy N; Biggs, Simon

    2016-07-28

    Accurate control of particle size at relatively narrow polydispersity remains a key challenge in the production of synthetic polymer particles at scale. A cross-flow membrane emulsification (XME) technique was used here in the preparation of poly(methyl methacrylate) microspheres at a 1-10 l h(-1) scale, to demonstrate its application for such a manufacturing challenge. XME technology has previously been shown to provide good control over emulsion droplet sizes with careful choice of the operating conditions. We demonstrate here that, for an appropriate formulation, equivalent control can be gained for a precursor emulsion in a batch suspension polymerization process. We report here the influence of key parameters on the emulsification process; we also demonstrate the close correlation in size between the precursor emulsion and the final polymer particles. Two types of polymer particle were produced in this work: a solid microsphere and an oil-filled matrix microcapsule.This article is part of the themed issue 'Soft interfacial materials: from fundamentals to formulation'. PMID:27298430

  4. Liquid Phase Micro-Extraction of Linear Alkylbenzene Sulfonate Anionic Surfactants in Aqueous Samples

    PubMed Central

    Larsson, Niklas; Otrembska, Paulina; Villar, Mercedes; Jönsson, Jan Åke

    2011-01-01

    Hollow fiber liquid phase micro-extraction (LPME) of linear alkylbenzene sulfonates (LAS) from aqueous samples was studied. Ion pair extraction of C10, C11, C12 and C13 homologues was facilitated with trihexylamine as ion-pairing agent, using di-n-hexylether as solvent for the supported liquid membrane (SLM). Effects of extraction time, acceptor buffer concentration, stirring speed, sample volume, NaCl and humic acids were studied. At 10–50 μg L−1 linear R2-coefficients were 0.99 for C10 and C11 and 0.96 for C12. RSD was typically ∼15%. Three observations were especially made. Firstly, LPME for these analytes was unusually slow with maximum enrichment observed after 15–24 h (depending on sample volume). Secondly, the enrichment depended on LAS sample concentration with 35–150 times enrichment below ∼150 μg L−1 and 1850–4400 times enrichment at 1 mg L−1. Thirdly, lower homologues were enriched more than higher homologues at low sample concentrations, with reversed conditions at higher concentrations. These observations may be due to the fact that LAS and the amine counter ion themselves influence the mass transfer at the water-SLM interface. The observations on LPME of LAS may aid in LPME application to other compounds with surfactant properties or in surfactant enhanced membrane extraction of other compounds. PMID:24957870

  5. Influence of post-emulsification drying processes on the microencapsulation of human serum albumin.

    PubMed

    Lane, Majella E; Brennan, Fiona S; Corrigan, Owen I

    2006-01-01

    In the present work, methods used to microencapsulate Human Serum Albumin (HSA) in a biodegradable polymer were compared for their effects on the physicochemical characteristics of HSA-loaded microparticles and on the release and integrity of encapsulated HSA. The polymer used was poly(D,L-lactide-co-glycolide) (75:25) (PLGA) (Boehringer Ingelheim, Resomer RG 752, MW 20,900). Microparticles were formulated by (i) w/o/w emulsification and freeze-drying (EFD) or (ii) w/o/w emulsification and spray-drying (ESD). Particle morphology and size were evaluated by scanning electron microscopy and by laser diffraction analysis. Loading, encapsulation efficiency and protein release were determined using a commercial protein assay kit. Protein integrity was evaluated by sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis. Particles produced by emulsification/spray-drying exhibited greater diversity in shape than those produced by emulsification/freeze-drying. Additionally, protein loading values were significantly higher for particles produced by emulsification/spray-drying rather than particles produced by emulsification/freeze-drying. The structural integrity of encapsulated protein was confirmed for particles produced by both processes. The fraction of HSA released was similar for both formulations. The emulsification/spray-drying technique described appears to be a rapid and efficient method for the preparation of PLGA microparticles loaded with a model protein. PMID:16274944

  6. Solid phase microextraction field kit

    DOEpatents

    Nunes, Peter J.; Andresen, Brian D.

    2005-08-16

    A field kit for the collection, isolation and concentration of trace amounts of high explosives (HE), biological weapons (BW) and chemical weapons (CW) residues in air, soil, vegetation, swipe, and liquid samples. The field kit includes a number of Solid Phase Microextraction (SPME) fiber and syringe assemblies in a hermetically sealed transportation container or tubes which includes a sampling port, a number of extra SPME fiber and syringe assemblies, the fiber and syringe assemblies including a protective cap for the fiber, and an extractor for the protective cap, along with other items including spare parts, protective glove, and an instruction manual, all located in an airtight container.

  7. Enhanced oil recovery by surfactant-enhanced volumetric sweep efficiency: First annual report for the period September 30, 1985-September 30, 1986. [Sandpacks

    SciTech Connect

    Harwell, J H; Scamehorn, J F

    1987-05-01

    Surfactant-enhanced volumetric sweep efficiency is a novel EOR method which utilizes precipitation/coacervation of surfactants to plug the most permeable regions of the reservoir, improving the efficiency of a waterflooding operation. This technique does not rely on reduction of interfacial tension between aqueous and oleic phases to enhance oil recovery. Therefore, even though surfactants are involved, this new technique is not a substitute or improvement on classical surfactant flooding; however, it has the potantial to compete with polymer flooding as an alternative sweep efficiency improvement method. In surfactant-enhanced volumetric sweep efficiency, a slug containing one kind of surfactant is injected into the reservoir, followed by a brine spacer. This is followed by injection of a second kind of surfactant which has lower adsorption than the first surfactant used. Anionic and cationic surfactants are one possible combination for this application. These may form either a precipitate or a coacervate upon mixing. Phase boundaries for some specific systems of this type have been determined over a wide range of conditions and a model developed to describe this behavior. Another possibility is the use of nonionic surfactants, which may form coacervate under proper conditions. The adsorption behavior of mixtures of anionic and nonionic surfactants was measured to aid in modeling the chromatographic effects with these surfactants in the reservoir. Studies with sandpacks of different permeabilities in parallel configuration using mixtures of anionic and cationic surfactants have demonstrated the capability of this method to reduce flow rates through a more permeable sandpack more than that through a less permeable sandpack. 4 refs., 23 figs., 8 tabs.

  8. Ultrasonic emulsification of food-grade nanoemulsion formulation and evaluation of its bactericidal activity.

    PubMed

    Ghosh, Vijayalakshmi; Mukherjee, Amitava; Chandrasekaran, Natarajan

    2013-01-01

    Basil oil (Ocimum basilicum) nanoemulsion was formulated using non-ionic surfactant Tween80 and water by ultrasonic emulsification method. Process of nanoemulsion development was optimized for parameters such as surfactant concentration and emulsification time to achieve minimum droplet diameter with high physical stability. Surfactant concentration was found to have a negative correlation with droplet diameter, whereas emulsification time had a positive correlation with droplet diameter and also with intrinsic stability of the emulsion. Stable basil oil nanoemulsion with droplet diameter 29.3 nm was formulated by ultrasonic emulsification for 15 min. Formulated nanoemulsion was evaluated for antibacterial activity against Escherichia coli by kinetics of killing experiment. Fluorescence microscopy and FT-IR results showed that nanoemulsion treatment resulted alteration in permeability and surface features of bacterial cell membrane. PMID:22954686

  9. Microfluidic EDGE emulsification: the importance of interface interactions on droplet formation and pressure stability

    NASA Astrophysics Data System (ADS)

    Sahin, Sami; Bliznyuk, Olesya; Rovalino Cordova, Ana; Schroën, Karin

    2016-05-01

    The fact that interactions of components with interfaces can influence processes is well-known; e.g. deposit accumulation on heat exchangers and membrane fouling lead to additional resistances against heat and mass transfer, respectively. In microfluidic emulsification, the situation is even more complex. Component accumulation at the liquid/liquid interface is necessary for emulsion stability, while undesired at the solid/liquid interface where it may change wettability. For successful emulsification both aspects need to be controlled, and that is investigated in this paper for o/w emulsification with microfluidic EDGE devices. These devices were characterised previously, and can be used to detect small wettability changes through e.g. the pressure stability of the device. We used various oil/emulsifier combinations (alkanes, vegetable oil, surfactants and proteins) and related droplet size and operational pressure stability to component interactions with the solid surface and liquid interface. Surfactants with a strong interaction with glass always favour emulsification, while surfactants that have week interactions with the surface can be replaced by vegetable oil that interacts strongly with glass, resulting in loss of emulsification. Our findings clearly show that an appropriate combination of construction material and emulsion components is needed to achieve successful emulsification in microfluidic EDGE devices.

  10. Microfluidic EDGE emulsification: the importance of interface interactions on droplet formation and pressure stability.

    PubMed

    Sahin, Sami; Bliznyuk, Olesya; Rovalino Cordova, Ana; Schroën, Karin

    2016-01-01

    The fact that interactions of components with interfaces can influence processes is well-known; e.g. deposit accumulation on heat exchangers and membrane fouling lead to additional resistances against heat and mass transfer, respectively. In microfluidic emulsification, the situation is even more complex. Component accumulation at the liquid/liquid interface is necessary for emulsion stability, while undesired at the solid/liquid interface where it may change wettability. For successful emulsification both aspects need to be controlled, and that is investigated in this paper for o/w emulsification with microfluidic EDGE devices. These devices were characterised previously, and can be used to detect small wettability changes through e.g. the pressure stability of the device. We used various oil/emulsifier combinations (alkanes, vegetable oil, surfactants and proteins) and related droplet size and operational pressure stability to component interactions with the solid surface and liquid interface. Surfactants with a strong interaction with glass always favour emulsification, while surfactants that have week interactions with the surface can be replaced by vegetable oil that interacts strongly with glass, resulting in loss of emulsification. Our findings clearly show that an appropriate combination of construction material and emulsion components is needed to achieve successful emulsification in microfluidic EDGE devices. PMID:27230981

  11. Microfluidic EDGE emulsification: the importance of interface interactions on droplet formation and pressure stability

    PubMed Central

    Sahin, Sami; Bliznyuk, Olesya; Rovalino Cordova, Ana; Schroën, Karin

    2016-01-01

    The fact that interactions of components with interfaces can influence processes is well-known; e.g. deposit accumulation on heat exchangers and membrane fouling lead to additional resistances against heat and mass transfer, respectively. In microfluidic emulsification, the situation is even more complex. Component accumulation at the liquid/liquid interface is necessary for emulsion stability, while undesired at the solid/liquid interface where it may change wettability. For successful emulsification both aspects need to be controlled, and that is investigated in this paper for o/w emulsification with microfluidic EDGE devices. These devices were characterised previously, and can be used to detect small wettability changes through e.g. the pressure stability of the device. We used various oil/emulsifier combinations (alkanes, vegetable oil, surfactants and proteins) and related droplet size and operational pressure stability to component interactions with the solid surface and liquid interface. Surfactants with a strong interaction with glass always favour emulsification, while surfactants that have week interactions with the surface can be replaced by vegetable oil that interacts strongly with glass, resulting in loss of emulsification. Our findings clearly show that an appropriate combination of construction material and emulsion components is needed to achieve successful emulsification in microfluidic EDGE devices. PMID:27230981

  12. Ultrasound-assisted temperature-controlled ionic-liquid dispersive liquid-phase microextraction method for simultaneous determination of anethole, estragole, and para-anisaldehyde in different plant extracts and human urine: a comparative study.

    PubMed

    Rajabi, Maryam; Haji-Esfandiari, Sudabeh; Barfi, Behruz; Ghanbari, Hanieh

    2014-07-01

    In this study, the performances of four ionic-liquid-based microextraction methods, ionic-liquid-based dispersive liquid-liquid microextraction (IL-DLLME), ionic-liquid-based ultrasound-assisted emulsification microextraction (IL-USA-ME), temperature-controlled ionic-liquid dispersive liquid-phase microextraction (TC-IL-DLME), and ultrasound-assisted temperature-controlled ionic-liquid dispersive liquid-phase microextraction (USA-TC-IL-DLME), were investigated for extraction of three bioactive compounds (anethole, estragole, and anisaldehyde) from different plant extracts and human urine. Anethole and estragole were chosen because they can alter cellular processes positively or negatively, and an efficient method is needed for their extraction and sensitive determination in the samples mentioned. Because there is no previous report on the separation of anethole and estragole (structural isomers), first, simultaneous gradient elution and flow programming were used. The microextraction methods were then applied and compared for analysis of these compounds in plant extracts and human urine by use of high-performance liquid chromatography (HPLC). The effect of conditions on extraction efficiency was studied and under the optimum conditions, the best enrichment factors (58-64), limits of detection (14-18 ng mL(-1)), limits of quantification (47-60 ng mL(-1)), and recovery (94.4-101.7 %) were obtained by use of USA-TC-IL-DLME. The optimized conditions were used to determine anethole, estragole, and para-anisaldehyde in fennel, anise, and tarragon extracts and in human urine. PMID:24817361

  13. Manufacture of large uniform droplets using rotating membrane emulsification.

    PubMed

    Vladisavljević, Goran T; Williams, Richard A

    2006-07-01

    A new rotating membrane emulsification system using a stainless steel membrane with 100 microm laser drilled pores was used to produce oil/water emulsions consisting of 2 wt% Tween 20 as emulsifier, paraffin wax as dispersed oil phase and 0.01-0.25 wt% Carbomer (Carbopol ETD 2050) as stabilizer. The membrane tube, 1 cm in diameter, was rotated inside a stationary glass cylinder, diameter of 3 cm, at a constant speed in the range 50-1500 rpm. The oil phase was introduced inside the membrane tube and permeated through the porous wall moving radially into the continuous phase in the form of individual droplets. Increasing the membrane rotational speed increased the wall shear stress which resulted in a smaller average droplet diameter being produced. For a constant rotational speed, the average droplet diameter increased as the stabilizer content in the continuous phase was lowered. The optimal conditions for producing uniform emulsion droplets were a Carbomer content of 0.1-0.25 wt% and a membrane rotational speed of 350 rpm, under which the average droplet diameter was 105-107 microm and very narrow coefficients of variation of 4.8-4.9%. A model describing the operation is presented and it is concluded that the methodology holds potential as a manufacturing protocol for both coarse and fine droplets and capsules. PMID:16563411

  14. Cross-Interface Emulsification for Generating Size-Tunable Droplets.

    PubMed

    Xu, Peng; Zheng, Xu; Tao, Yi; Du, Wenbin

    2016-03-15

    We report cross-interface emulsification (XiE), a simple method for the generation of monodisperse droplets of controllable volumes from picoliter to nanoliter. A device is set up in which a fused-silica capillary is vibrating across the surface of the continuous phase (mineral oil) in a reservoir, and the flow of the dispersed phase (aqueous solution) in the capillary is segmented into monodisperse droplets at the air/oil interface. We find that the volume of droplets is mainly dominated by the flow rate and vibrating frequency and not significantly influenced by other factors, such as the viscosity of the continuous phase and dispersed phase, the inner diameter of the capillary (20-100 μm), or the shape of the tip (tapered or flat). These features reflect high robustness, flexibility, and precision of XiE for on-demand volume control of droplets. The droplets automatically assemble into planar monolayer droplet arrays (PMDA) in flat-bottomed microwells of 96-well plates, offering excellent convenience for imaging of droplets. As a representative application, we carry out digital loop-mediated isothermal amplification using PMDAs with multivolume droplets for the absolute quantification of nucleic acids. Our results demonstrate that XiE is simple and controllable for the production of monodisperse size-tunable droplets, and it offers opportunities for common laboratories, even without microfabrication facilities, to perform digital quantification, single cell analysis, and other biochemical assays with high throughput. PMID:26849419

  15. Emulsification Characteristics Using a Dynamic Woven Metal Microscreen Membrane.

    PubMed

    Sabouni, Rana; Gomaa, Hassan G; Liu, Jiangshan; Zhu, Jesse

    2016-01-01

    An oscillatory emulsification system for the production of oil in water emulsions using a commercially available low-cost woven metal microscreen (WMMS) is investigated. The system allows for independent control of both the oscillation frequencies and amplitudes such that it provides two degrees of freedom for controlling the emulsion properties. The investigations included the production of both surfactant and particle-stabilized emulsions. The average droplet size was found to decrease when both the oscillation frequency and amplitude was increased. For surfactant-stabilized emulsions, using bi-surfactants in both the continuous and dispersed phases resulted in a smaller droplet size due to lower interfacial tension. For particle-stabilized emulsions, both the hydrodynamics of the system and the hydrophobic and hydrophilic nature of the stabilizing particles influenced the interfacial properties at the oil-water interface, which in turn affected the final droplet size and distribution with potential droplet breakage. In absence of the latter, a simple torque balance model can be used to reasonably predict the average emulsion droplet size. PMID:27331821

  16. Emulsification Characteristics Using a Dynamic Woven Metal Microscreen Membrane

    PubMed Central

    Sabouni, Rana; Gomaa, Hassan G.; Liu, Jiangshan; Zhu, Jesse

    2016-01-01

    An oscillatory emulsification system for the production of oil in water emulsions using a commercially available low-cost woven metal microscreen (WMMS) is investigated. The system allows for independent control of both the oscillation frequencies and amplitudes such that it provides two degrees of freedom for controlling the emulsion properties. The investigations included the production of both surfactant and particle-stabilized emulsions. The average droplet size was found to decrease when both the oscillation frequency and amplitude was increased. For surfactant-stabilized emulsions, using bi-surfactants in both the continuous and dispersed phases resulted in a smaller droplet size due to lower interfacial tension. For particle-stabilized emulsions, both the hydrodynamics of the system and the hydrophobic and hydrophilic nature of the stabilizing particles influenced the interfacial properties at the oil–water interface, which in turn affected the final droplet size and distribution with potential droplet breakage. In absence of the latter, a simple torque balance model can be used to reasonably predict the average emulsion droplet size. PMID:27331821

  17. Water fluxes and encapsulation efficiency in double emulsions: impact of emulsification and osmotic pressure unbalance.

    PubMed

    Nollet, Maxime; Mercé, Manuel; Laurichesse, Eric; Pezon, Annaïck; Soubabère, Olivier; Besse, Samantha; Schmitt, Véronique

    2016-03-30

    We study the influence of the emulsification process on encapsulation efficiency of drugs in double water-in-oil-in-water emulsions. Two drugs were used, first vitamin B12 which can be considered as a model drug and secondly a suspension of Cydia pomonella Granulovirus (CpGV), a virus used in organic agriculture to protect fruits against the Carpocapse insect. Encapsulation is measured by classical UV-Vis spectroscopy method. Additionally we show that rheology is a useful tool to determine water exchanges during emulsification. In a two-step emulsification process, using rotor-stator mixers, encapsulation reaches high levels, close to 100% whatever the flowing regime. This encapsulation decreases only if two conditions are fulfilled simultaneously: (i) during the second emulsification step the flow is turbulent and (ii) it leads to excessive fragmentation inducing formation of too small drops. We also investigate the effect of a deliberate loss of osmotic pressure balance on the encapsulation and characterize the induced water fluxes. We show that encapsulation of vitamin B12 is not affected by the osmotic pressure unbalance, while water exchanges, if they exist, are very fast and aim at restoring equilibrium. As a consequence, the emulsification efficiency is not very sensitive to osmotic stresses provided that the interfaces resist mechanically. PMID:26936127

  18. Nanoemulsions prepared by a low-energy emulsification method applied to edible films.

    PubMed

    Bilbao-Sáinz, Cristina; Avena-Bustillos, Roberto J; Wood, Delilah F; Williams, Tina G; McHugh, Tara H

    2010-11-24

    Catastrophic phase inversion (CPI) was used as a low-energy emulsification method to prepare oil-in-water (O/W) nanoemulsions in a lipid (Acetem)/water/nonionic surfactant (Tween 60) system. CPIs in which water-in-oil emulsions (W/O) are transformed into oil-in-water emulsions (O/W) were induced by changes in the phase ratio. Dynamic phase inversion emulsification was achieved by slowly increasing the water volume fraction (fw) to obtain O/W emulsions from water in oil emulsions. Composition and processing variables were optimized to minimize droplet size and polydispersity index (PdI). It was found that addition of the continuous phase to the dispersed phase following the standard CPI procedure resulted in the formation of oil droplets with diameters of 100-200 nm. Droplet size distribution during CPI and emulsification time depended on stirring speed and surfactant concentration. Droplet sizes in the inverted emulsions were compared to those obtained by direct emulsification: The process time to reach droplet sizes of around 100 nm was reduced by 12 times by using CPI emulsification. The Acetem/water nanoemulsion was also used as a carrier to incorporate oregano and cinnamon essential oils into soy protein edible films. The resulting composite films containing oregano oil showed better moisture barrier and mechanical properties compared to soy protein films. PMID:20977191

  19. Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe3O4 nanoparticles

    NASA Astrophysics Data System (ADS)

    Manafi, Mohammad Hanif; Allahyari, Mehdi; Pourghazi, Kamyar; Amoli-Diva, Mitra; Taherimaslak, Zohreh

    2015-07-01

    The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100 mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL-1 with low detection limit of 0.03 ng mL-1 were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method.

  20. Scaling-up parameters for site restoration process using surfactant-enhanced soil washing coupled with wastewater treatment by Fenton and Fenton-like processes.

    PubMed

    Bandala, Erick R; Cossio, Horacio; Sánchez-Lopez, Adriana D; Córdova, Felipe; Peralta-Herández, Juan M; Torres, Luis G

    2013-01-01

    Estimation of scaling-up parameters for a site restoration process using a surfactant-enhanced soil washing (SESW) process followed by the application of advanced oxidation processes (Fenton and photo-Fenton) was performed. For the SESW, different parameters were varied and the soil washing efficiency for pesticide (2,4-D) removal assessed. The resulting wastewater was treated using the Fenton reaction in the absence and presence of ultraviolet (UV) radiation for pesticide removal. Results showed that agitation speed of 1550 rpm was preferable for the best pesticide removal from contaminated soil. It was possible to wash contaminated soils with different soil concentrations; however the power drawn was higher as the soil concentration increased. Complete removal of the pesticide and the remaining surfactant was achieved using different reaction conditions. The best degradation conditions were for the photo-Fenton process using [Fe(II)] = 0.3 mM; [H2O2] = 4.0 mM where complete 2,4-D and sodium dodecylsulfate (SDS) removal was observed after 8 and 10 minutes of reaction, respectively. Further increase in the hydrogen peroxide or iron salt concentration did not show any improvement in the reaction rate. Kinetic parameters, i.e. reaction rate constant and scaling-up parameters, were determined. It was shown that, by coupling both processes (SESW and AOPs), it is possible the restoration of contaminated sites. PMID:23530350

  1. In situ, field-scale evaluation of surfactant-enhanced DNAPL recovery using a single-well, ``push-pull'' test

    SciTech Connect

    Istok, J.D.; Field, J.A.

    1999-10-01

    The overall goal of this project was to further develop the single-well, ``push-pull'' test method as a feasibility assessment and site-characterization tool for studying the fundamental fate and transport behavior of injected surfactants and their ability to solubilize and mobilize dense nonaqueous phase liquids (DNAPLs) in the subsurface. The specific objectives were to develop a modified push-pull test for use in identifying and quantifying the effects of sorption, precipitation, and biodegradation on the fate and transport of injected surfactants, use the developed test method to quantify the effects of these processes on the ability of injected surfactants to solubilize and mobilize residual phase trichloroethane (TCE), and demonstrate the utility of the developed test method for performing site characterization and feasibility studies for surfactant-enhanced DNAPL recovery systems in the field. The results from the intermediate-scale laboratory experiments conducted for this project indicate that the single-well, push-pull test method can provide quantitative information on the effectiveness of injected surfactants in enhancing DNAPL solubilization in natural aquifer sediments. Specifically, the results of this research demonstrate the ability of the single-well, push-pull test to characterize the behavior of multi-component surfactants in the presence of natural aquifer sediment under laboratory and in-situ field conditions.

  2. The effect of polymer-surfactant interaction on the rheological properties of surfactant enhanced alkaline flooding formulations. [Phase separation, precipitation and viscosity loss

    SciTech Connect

    French, T.R.; Josephson, C.B.

    1993-02-01

    Surfactant-enhanced, lower pH (weak) alkaline chemicals are effective for mobilizing residual oil. Polymer is used for mobility control because if mobility control is lost, then oil recovery is reduced. The ability to maintain mobility control during surfactant-alkaline flooding can be adversely affected by chemical interaction. In this work, interaction between polymers and surfactants was shown to be affected by pH, ionic strength, crude oil, and the properties of the polymers and surfactants. Polymer-surfactant interaction (phase separation, precipitation, and viscosity loss) occurred between most of the polymers and surfactants that were tested. Polymer-surfactant interaction is difficult to eliminate, and no method was found for completely eliminating interaction. Polymer-surfactant interaction occurred at optimal salinity and below optimal salinity. Polymer-surfactant interaction had an adverse effect on polymer rheology; however, the adverse effect of interaction on polymer rheology was lessened when oil was present. Increasing the pH of chemical systems further reduced the adverse effects of interaction on polymer rheology.

  3. Microextraction techniques in therapeutic drug monitoring.

    PubMed

    Farhadi, Khalil; Hatami, Mehdi; Matin, Amir Abbas

    2012-08-01

    Therapeutic drug monitoring (TDM), as part of clinical process of medical treatments, is commonly used to maintain 'therapeutic' drug concentrations. TDM is useful to identify the causes of unwanted or unexpected responses, to prevent unnecessary diagnostic testing, to improve clinical outcomes, and even to save lives. The determination of drug concentration in blood samples requires an excellent sample preparation procedure. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low or no solvent consumption. Microextraction techniques, such as liquid- and solid-phase microextraction, have these advantages over the traditional techniques. This paper reviews the recent developments in microextraction techniques used for drug monitoring in serum, plasma or blood samples. PMID:22767149

  4. Emulsification-Induced Homohelicity in Racemic Helical Polymer for Preparing Optically Active Helical Polymer Nanoparticles.

    PubMed

    Zhao, Biao; Deng, Jinrui; Deng, Jianping

    2016-04-01

    Optically active nano- and microparticles have constituted a significant category of advanced functional materials. However, constructing optically active particles derived from synthetic helical polymers still remains as a big challenge. In the present study, it is attempted to induce a racemic helical polymer (containing right- and left-handed helices in equal amount) to prefer one predominant helicity in aqueous media by using emulsifier in the presence of chiral additive (emulsification process). Excitingly, the emulsification process promotes the racemic helical polymer to unify the helicity and directly provides optically active nanoparticles constructed by chirally helical polymer. A possible mechanism is proposed to explain the emulsification-induced homohelicity effect. The present study establishes a novel strategy for preparing chirally helical polymer-derived optically active nanoparticles based on racemic helical polymers. PMID:26829250

  5. Emulsification in turbulent flow 1. Mean and maximum drop diameters in inertial and viscous regimes.

    PubMed

    Vankova, Nina; Tcholakova, Slavka; Denkov, Nikolai D; Ivanov, Ivan B; Vulchev, Vassil D; Danner, Thomas

    2007-08-15

    Systematic experimental study of the effects of several factors on the mean and maximum drop sizes during emulsification in turbulent flow is performed. These factors include: (1) rate of energy dissipation, epsilon; (2) interfacial tension, sigma; (3) viscosity of the oil phase, eta(D); (4) viscosity of the aqueous phase, eta(C); and (5) oil volume fraction, Phi. The emulsions are prepared by using the so-called "narrow-gap homogenizer" working in turbulent regime of emulsification. The experiments are performed at high surfactant concentration to avoid the effect of drop-drop coalescence. For emulsions prepared in the inertial turbulent regime, the mean and the maximum drop sizes increase with the increase of eta(D) and sigma, and with the decrease of epsilon. In contrast, Phi and eta(C) affect only slightly the mean and the maximum drop sizes in this regime of emulsification. These results are described very well by a theoretical expression proposed by Davies [Chem. Eng. Sci. 40 (1985) 839], which accounts for the effects of the drop capillary pressure and the viscous dissipation inside the breaking drops. The polydispersity of the emulsions prepared in the inertial regime of emulsification does not depend significantly on sigma and epsilon. However, the emulsion polydispersity increases significantly with the increase of oil viscosity, eta(D). The experiments showed also that the inertial turbulent regime is inappropriate for emulsification of oils with viscosity above ca. 500 mPa s, if drops of micrometer size are to be obtained. The transition from inertial to viscous turbulent regime of emulsification was accomplished by a moderate increase of the viscosity of the aqueous phase (above 5 mPa s in the studied systems) and/or by increase of the oil volume fraction, Phi>0.6. Remarkably, emulsions with drops of micrometer size are easily formed in the viscous turbulent regime of emulsification, even for oils with viscosity as high as 10,000 mPa s. In this regime

  6. Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe₃O₄ nanoparticles.

    PubMed

    Manafi, Mohammad Hanif; Allahyari, Mehdi; Pourghazi, Kamyar; Amoli-Diva, Mitra; Taherimaslak, Zohreh

    2015-07-01

    The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL(-1) with low detection limit of 0.03 ng mL(-1) were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method. PMID:25804513

  7. Ensemble of surrogates-based optimization for identifying an optimal surfactant-enhanced aquifer remediation strategy at heterogeneous DNAPL-contaminated sites

    NASA Astrophysics Data System (ADS)

    Jiang, Xue; Lu, Wenxi; Hou, Zeyu; Zhao, Haiqing; Na, Jin

    2015-11-01

    The purpose of this study was to identify an optimal surfactant-enhanced aquifer remediation (SEAR) strategy for aquifers contaminated by dense non-aqueous phase liquid (DNAPL) based on an ensemble of surrogates-based optimization technique. A saturated heterogeneous medium contaminated by nitrobenzene was selected as case study. A new kind of surrogate-based SEAR optimization employing an ensemble surrogate (ES) model together with a genetic algorithm (GA) is presented. Four methods, namely radial basis function artificial neural network (RBFANN), kriging (KRG), support vector regression (SVR), and kernel extreme learning machines (KELM), were used to create four individual surrogate models, which were then compared. The comparison enabled us to select the two most accurate models (KELM and KRG) to establish an ES model of the SEAR simulation model, and the developed ES model as well as these four stand-alone surrogate models was compared. The results showed that the average relative error of the average nitrobenzene removal rates between the ES model and the simulation model for 20 test samples was 0.8%, which is a high approximation accuracy, and which indicates that the ES model provides more accurate predictions than the stand-alone surrogate models. Then, a nonlinear optimization model was formulated for the minimum cost, and the developed ES model was embedded into this optimization model as a constrained condition. Besides, GA was used to solve the optimization model to provide the optimal SEAR strategy. The developed ensemble surrogate-optimization approach was effective in seeking a cost-effective SEAR strategy for heterogeneous DNAPL-contaminated sites. This research is expected to enrich and develop the theoretical and technical implications for the analysis of remediation strategy optimization of DNAPL-contaminated aquifers.

  8. Pilot-scale demonstration of surfactant-enhanced PCE solubilization at the Bachman Road site. 1. Site characterization and test design.

    PubMed

    Abriola, Linda M; Drummond, Chad D; Hahn, Ernest J; Hayes, Kim F; Kibbey, Tohren C G; Lemke, Lawrence D; Pennell, Kurt D; Petrovskis, Erik A; Ramsburg, C Andrew; Rathfelder, Klaus M

    2005-03-15

    A pilot-scale demonstration of surfactant-enhanced aquifer remediation (SEAR) was conducted to recover dense nonaqueous phase liquid (DNAPL) tetrachloroethene (PCE) from a sandy glacial outwash aquifer underlying a former dry cleaning facility at the Bachman Road site in Oscoda, MI. Part one of this two-part paper describes site characterization efforts and a comprehensive approach to SEAR test design, effectively integrating laboratory and modeling studies. Aquifer coring and drive point sampling suggested the presence of PCE-DNAPL in a zone beneath an occupied building. A narrow PCE plume emanating from the vicinity of this building discharges into Lake Huron. The shallow unconfined aquifer, characterized by relatively homogeneous fine-medium sand deposits, an underlying clay layer, and the absence of significant PCE transformation products, was judged suitable for the demonstration of SEAR. Tween 80 was selected for application based upon its favorable solubilization performance in batch and two-dimensional sand tank treatability studies, biodegradation potential, and regulatory acceptance. Three-dimensional flow and transport models were employed to develop a robust design for surfactant delivery and recovery. Physical and fiscal constraints led to an unusual hydraulic design, in which surfactant was flushed across the regional groundwater gradient, facilitating the delivery of concentrations of Tween 80 exceeding 1% (wt) throughout the treatment zone. The potential influence of small-scale heterogeneity on PCE-DNAPL distribution and SEAR performance was assessed through numerical simulations incorporating geostatistical permeability fields based upon available core data. For the examined conditions simulated PCE recoveries ranged from 94to 99%. The effluent treatment system design consisted of low-profile air strippers coupled with carbon adsorption to trap off-gas PCE and discharge of treated aqueous effluent to a local wastewater treatment plant. The

  9. Interfacial Properties of Raw and Roasted Peanut Oils as Related to Emulsification

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Roasted peanut oil is a unique product that can impart a desirable roasted peanut flavor in various emulsified formulations. Emulsification properties are a function of the oil physical properties, which include interfacial tension, viscosity, and density among others. These physical properties ha...

  10. Emulsification by high frequency ultrasound using piezoelectric transducer: formation and stability of emulsifier free emulsion.

    PubMed

    Kaci, Messaouda; Meziani, Smail; Arab-Tehrany, Elmira; Gillet, Guillaume; Desjardins-Lavisse, Isabelle; Desobry, Stephane

    2014-05-01

    Emulsifier free emulsion was developed with a new patented technique for food and cosmetic applications. This emulsification process dispersed oil droplets in water without any emulsifier. Emulsions were prepared with different vegetable oil ratios 5%, 10% and 15% (v/v) using high frequency ultrasounds generated by piezoelectric ceramic transducer vibrating at 1.7 MHz. The emulsion was prepared with various emulsification times between 0 and 10h. Oil droplets size was measured by laser granulometry. The pH variation was monitored; electrophoretic mobility and conductivity variation were measured using Zêtasizer equipment during emulsification process. The results revealed that oil droplets average size decreased significantly (p<0.05) during the first 6h of emulsification process and that from 160 to 1 μm for emulsions with 5%, 10% and from 400 to 29 μm for emulsion with 15% of initial oil ratio. For all tested oil ratios, pH measurement showed significant decrease and negative electrophoretic mobility showed the accumulation of OH(-) at oil/water interface leading to droplets stability in the emulsion. The conductivity of emulsions showed a decrease of the ions quantity in solution, which indicated formation of positive charge layer around OH(-) structure. They constitute a double ionic layer around oil particles providing emulsion stability. This study showed a strong correlation between turbidity measurement and proportion of emulsified oil. PMID:24315670

  11. Formation of oil-in-water emulsions from natural emulsifiers using spontaneous emulsification: sunflower phospholipids.

    PubMed

    Komaiko, Jennifer; Sastrosubroto, Ashtri; McClements, David Julian

    2015-11-18

    This study examined the possibility of producing oil-in-water emulsions using a natural surfactant (sunflower phospholipids) and a low-energy method (spontaneous emulsification). Spontaneous emulsification was carried out by titrating an organic phase (oil and phospholipid) into an aqueous phase with continuous stirring. The influence of phospholipid composition, surfactant-to-oil ratio (SOR), initial phospholipids location, storage time, phospholipid type, and preparation method was tested. The initial droplet size depended on the nature of the phospholipid used, which was attributed to differences in phospholipid composition. Droplet size decreased with increasing SOR and was smallest when the phospholipid was fully dissolved in the organic phase rather than the aqueous phase. The droplets formed using spontaneous emulsification were relatively large (d > 10 μm), and so the emulsions were unstable to gravitational separation. At low SORs (0.1 and 0.5), emulsions produced with phospholipids had a smaller particle diameter than those produced with a synthetic surfactant (Tween 80), but at a higher SOR (1.0), this trend was reversed. High-energy methods (microfluidization and sonication) formed significantly smaller droplets (d < 10 μm) than spontaneous emulsification. The results from this study show that low-energy methods could be utilized with natural surfactants for applications for which fine droplets are not essential. PMID:26528859

  12. Nanoemulsions prepared by a low-energy emulsification method applied to edible films

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Catastrophic phase inversion (CPI) was used as a low-energy emulsification method to prepare oil-in-water (O/W) nanoemulsions in a lipid (Acetem)/water/nonionic surfactant (Tween 60) system. CPIs in which water-in-oil emulsions (W/O) are transformed into oil-in-water emulsions (O/W) were induced by ...

  13. Fabrication of starch-based microparticles by an emulsification-crosslinking method

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Starch-based microparticles (MPs) fabricated by a water-in-water (w/w) emulsification-crosslinking method could be used as a controlled-release delivery vehicle for food bioactives. Due to the processing route without the use of toxic organic solvents, it is expected that these microparticles can be...

  14. New developments in microextraction techniques in bioanalysis. A review.

    PubMed

    Ocaña-González, Juan Antonio; Fernández-Torres, Rut; Bello-López, Miguel Ángel; Ramos-Payán, María

    2016-01-28

    In recent years, the interest in new extraction methods with lower sample volume requirements, simpler equipment and handling, and lower reagent consumption, has led to the development of a series of microextraction methods based on extraction phases in the microliter order. Nowadays, many references can be found for several of these methods, which imply a wide range of applications referred to both the analyte and the sample nature. In this paper, recent developments in both well-established microextraction techniques (solid phase microextraction, hollow-fiber liquid phase microextraction, dispersive liquid-liquid microextraction, etc.) and recently appeared microextraction procedures (nanoextraction systems, microchip devices, etc.) for the clinical analysis of biological samples will be reviewed and discussed. PMID:26755133

  15. Ionic-liquid-based surfactant-emulsified microextraction procedure accelerated by ultrasound radiation followed by high-performance liquid chromatography for the simultaneous determination of antidepressant and antipsychotic drugs.

    PubMed

    Zare, Fahimeh; Ghaedi, Mehrorang; Daneshfar, Ali

    2015-03-01

    In the present work, an efficient and environmental friendly method of ionic-liquid-based emulsified microextraction procedure accelerated by ultrasound radiation has been developed. Subsequently, its performance was compared with dispersive liquid-liquid microextraction and ultrasound-assisted surfactant-based emulsification microextraction methods. The optimization of experimental conditions was carried out by combination of central composite design and response surface methodology. The optimum conditions of variables were set as follows: 50 μL of 1-hexyl-3-methylimidazolium hexafluorophosphate (extracting solvent), 10 min ultrasound time, and 10 min vortex time for agitating 6 mL sample solution in pH 3 in the presence of 4 mg sodium dodecyl sulfate without addition of salt and 200 μL of methanol as diluent solvent. Under these conditions, the responses are linear for doxepin and perphenazine in the range of 0.3-1000 and 5-1000 μg/L, respectively. The limits of detection were 0.1 μg/L for doxepin and 1 μg/L for perphenazine. Relative standard deviations were lower than 3.5 for the determination of both species. Finally, the method was used for the preconcentration and determination of doxepin and perphenazine in urine sample with relative recoveries in the range of 89-98%. PMID:25545187

  16. Effects of Temperature on the Emulsification in Surfactant-Water-Oil Systems

    NASA Astrophysics Data System (ADS)

    Yuan, Yin-Quan; Zou, Xian-Wu; Xiong, Ping-Fan

    The effect of temperature on the emulsification has been investigated by discontinuous molecular dynamic simulation. When a large oil drop is put in water, on one hand the mixing entropy makes it divide into small oil drops; on the other hand the interactions among particles drives the small oil drops fowards aggregation. The evolution of the mean size of oil drops obeys the exponential delay law. There exist an active temperature, at which, the addition of surfactants has obvious effect on the emulsification. The surfactants with low HLB value (e.g. H1T3) make the dispersity of emulsion decrease, and the surfactants with high HLB value (e.g. H2T2 and H3T1) make a contribution to increase the dispersity of emulsion.

  17. Tuneable stability of nanoemulsions fabricated using spontaneous emulsification by biopolymer electrostatic deposition.

    PubMed

    Saberi, Amir Hossein; Zeeb, Benjamin; Weiss, Jochen; McClements, David Julian

    2015-10-01

    Nanoemulsions can be formed spontaneously from surfactant-oil-water systems using low energy methods. In this work, we showed that the droplets in oil-in-water nanoemulsions fabricated by spontaneous emulsification could be coated with an anionic biopolymer (beet pectin) using electrostatic deposition. Nanoemulsions were formed by titrating oil (medium chain triglycerides) and surfactant (polyoxyethylene sorbitan monostearate+lauric arginate) mixtures into an aqueous solution (10 mM citrate buffer, pH 4). Lauric arginate was used to generate a positive charge on the droplet surfaces, thereby enabling subsequent electrostatic deposition of anionic pectin. Extensive droplet aggregation occurred when intermediate pectin concentrations were used due to bridging flocculation. However, stable anionic pectin-coated lipid droplets could be formed at high pectin concentrations. These results demonstrate the possibility of tailoring the functionality of lipid nanodroplets produced by spontaneous emulsification. PMID:26070187

  18. Cross-flow membrane emulsification technique for fabrication of drug-loaded particles

    NASA Astrophysics Data System (ADS)

    Ho, Thanh Ha; Phuong Tuyen Dao, Thi; Nguyen, Tuan Anh; Dam Le, Duy; Chien Dang, Mau

    2013-12-01

    Cross-flow membrane emulsification is a new technique which was used in this study to achieve uniform and controllable emulsion systems. In this method, the droplet is individually formed at the pore on the surface of membrane in the more mild, controllable and efficient way as compared to traditional emulsification techniques. In this study, we used silicon nitride membranes of very precise parameters of pore size, shape and inter-pore distance in order to create curcumin loaded poly(d, l-lactic-co-glycolic acid) (PLGA) particles. It was demonstrated that more uniform and pore-size dependent particles was created by using different membrane pore sizes (ø200 nm, ø450 nm and ø2 μm). Other factors that could impact particle size and morphology such as membrane polarity, concentration and volume of two phases were investigated. Further tests on comparison to mechanical stirring method were also realized.

  19. A Mutant Strain of a Surfactant-Producing Bacterium with Increased Emulsification Activity

    NASA Astrophysics Data System (ADS)

    Liu, Qingmei; Yao, Jianming; Pan, Renrui; Yu, Zengliang

    2005-06-01

    As reported in this paper, a strain of oil-degrading bacterium Sp-5-3 was determined to belong to Enterobacteriaceae, which would be useful for microbial enhanced oil recovery (MEOR). The aim of our study was to generate a mutant using low energy N+ beam implantation. With 10 keV of energy and 5.2 × 1014 N+/cm2 of dose - the optimum condition, a mutant, S-34, was obtained, which had nearly a 5-fold higher surface and a 13-fold higher of emulsification activity than the wild type. The surface activity was measured by two methods, namely, a surface tension measuring instrument and a recording of the repulsive circle of the oil film; the emulsification activity was scaled through measuring the separating time of the oil-fermentation mixture. The metabolic acid was determined as methane by means of gas chromatography.

  20. Controlled microfluidic emulsification of oil in a clay nanofluid: Role of salt for Pickering stabilization

    NASA Astrophysics Data System (ADS)

    Gholamipour-Shirazi, A.; Carvalho, M. S.; Fossum, J. O.

    2016-07-01

    Research on emulsions is driven by their widespread use in different industries, such as food, cosmetic, pharmaceutical and oil recovery. Emulsions are stabilized by suitable surfactants, polymers, solid particles or a combination of them. Microfluidic emulsification is the process of droplet formation out of two or more liquids under strictly controlled conditions, without pre-emulsification step. Microfluidic technology offers a powerful tool for investigating the properties of emulsions themselves. In this work stable oil in water emulsions were formed with hydrophilic Laponite RD® nanoparticles adsorbed at the interface of the oil phase and aqueous clay nanofluid in a T junction microfluidic chip. Emulsion stability up to at least 40 days could be observed.

  1. Production of alginate microspheres by internal gelation using an emulsification method.

    PubMed

    Chan, L; Lee, H; Heng, P

    2002-08-21

    Alginate is a natural polysaccharide found in brown algae. Alginates are widely used in the food and pharmaceutical industries and have been employed as a matrix for the entrapment of drugs, macromolecules and biological cells. Alginate microspheres can be produced by the external or internal gelation method using calcium salts. The addition of calcium chloride solution in the final phase of production of microspheres by external gelation method using an emulsification technique causes the disruption of the equilibrium of the system being stirred, resulting in a significant degree of clumping of microspheres. Therefore, in this study, production of alginate microspheres by the internal gelation method using a modified emulsification technique was explored. The influence of calcium salt, added in varying amounts and at different stages, on the morphology of the microspheres was investigated. The effects of other hardening agents and different drying methods were also studied. PMID:12176259

  2. Water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction for the determination of organochlorine pesticides in aqueous samples.

    PubMed

    Li, Yee; Chen, Pai-Shan; Huang, Shang-Da

    2013-07-26

    A novel sample preparation method, "water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction (WLSEME)", coupled with gas chromatography using an electron capture detector (GC-ECD) was developed for the analysis of the organochlorine pesticides (OCPs), heptachlor, α-endosulfan, 4,4-DDE, 2,4-DDD and endrin, in aqueous samples. A microsyringe is used to withdrew and discharge 10-12μL of the extraction solvent and 60-120μL of water as the dispersed solvent (containing 1mgL(-1), Tween 80) 4 times within 10s to form a cloudy emulsified solution in the syringe. This is then injected into an 8mL aqueous sample spiked with all above OCPs. Dodecyl acetate and 2-dodecanol were both selected as extraction solvents to optimize their conditions separately. The total extraction time was about 0.5min. Under optimum conditions, using dodecyl acetate (12μL) as extraction solvent, the linear range of the method was 10-1000ngL(-1) for all OCPs, and the the limits of detection (LODs) ranged from 1 to 5ngL(-1). The absolute recoveries and relative recoveries were from 20.8 to 43.5% and 83.2 to 109.8% for lake water, and 19.9-49.2% and 85.4-115.9% for seawater respectively. In the second method, 2-dodecanol as extraction solvent, the linear range was from 5 to 5000ngL(-1) for the target compounds, and the LODs were between 0.5 and 2ngL(-1). The absolute recoveries and relative recoveries ranged from 25.7 to 42.2% and 96.3-111.2% for sea water, and 22.4-41.9% and 90.7-107.9% for stream water. This could solve several problems, which commonly occur in ultrasound-assisted emulsification micro-extraction (USAEME), dispersive liquid-liquid micro-extraction (DLLME) and other assisted emulsification methods. These problems include analyte degradation, increased solubility of the extraction solvent and analyte, and high toxicity and large volume of the organic solvent used. PMID:23566919

  3. Spontaneous Emulsification of Triolein Induced by Mixed Micellar Solutions of Sodium Polyoxyethylene Alkyl Ether Sulfate and Dodecyldimethyl Amine Oxide.

    PubMed

    Endo, Chika; Ito, Yoshiko; Akabane, Chika; Kaneko, Yukihiro; Sakai, Hideki

    2015-01-01

    A new mechanism of spontaneous emulsification without any salts or co-solvents is described, and is related to the dilatational behavior. Spontaneous emulsification can reduce the time required to remove oily soils from hard surfaces and enhance the detergency, because this type of emulsification requires no external mechanical work. In this paper, we focused on triolein, the main component of food oils and human sebum soil, and tried to induce spontaneous emulsification by using mixed micellar solutions of sodium polyoxyethylene alkyl ether sulfate and N, N-dimethyldodecylamine oxide (AES/DDAO). We characterized the dilatation of the oil/water interface using dynamic interfacial tension and elasticity measurements. This study confirmed that the degree of spontaneous emulsification can be enhanced by controlling the molar ratio of DDAO to AES. This enhancement can be attributed to an increased rate of decrease in the dynamic interfacial tension (i.e., a decreased interface dilatational elasticity), allowing for much greater suppression of the Marangoni effect. Further, we determined that one of the reasons for the decrease in the interface dilatational elasticity is the increasing number of micelles near the oil drop interface, which results from a decrease in the electrostatic repulsion between the micelles and the drop interface. Therefore, controlling the molar ratio of a mixed anionic/amphoteric surfactant solution is an effective way to induce spontaneous emulsification in the absence of salts or co-solvents. PMID:26250425

  4. Linking Findings in Microfluidics to Membrane Emulsification Process Design: The Importance of Wettability and Component Interactions with Interfaces

    PubMed Central

    Schroën, Karin; Ferrando, Montse; de Lamo-Castellví, Silvia; Sahin, Sami; Güell, Carme

    2016-01-01

    In microfluidics and other microstructured devices, wettability changes, as a result of component interactions with the solid wall, can have dramatic effects. In emulsion separation and emulsification applications, the desired behavior can even be completely lost. Wettability changes also occur in one phase systems, but the effect is much more far-reaching when using two-phase systems. For microfluidic emulsification devices, this can be elegantly demonstrated and quantified for EDGE (Edge-base Droplet GEneration) devices that have a specific behavior that allows us to distinguish between surfactant and liquid interactions with the solid surface. Based on these findings, design rules can be defined for emulsification with any micro-structured emulsification device, such as direct and premix membrane emulsification. In general, it can be concluded that mostly surface interactions increase the contact angle toward 90°, either through the surfactant, or the oil that is used. This leads to poor process stability, and very limited pressure ranges at which small droplets can be made in microfluidic systems, and cross-flow membrane emulsification. In a limited number of cases, surface interactions can also lead to lower contact angles, thereby increasing the operational stability. This paper concludes with a guideline that can be used to come to the appropriate combination of membrane construction material (or any micro-structured device), surfactants and liquids, in combination with process conditions. PMID:27187484

  5. Linking Findings in Microfluidics to Membrane Emulsification Process Design: The Importance of Wettability and Component Interactions with Interfaces.

    PubMed

    Schroën, Karin; Ferrando, Montse; de Lamo-Castellví, Silvia; Sahin, Sami; Güell, Carme

    2016-01-01

    In microfluidics and other microstructured devices, wettability changes, as a result of component interactions with the solid wall, can have dramatic effects. In emulsion separation and emulsification applications, the desired behavior can even be completely lost. Wettability changes also occur in one phase systems, but the effect is much more far-reaching when using two-phase systems. For microfluidic emulsification devices, this can be elegantly demonstrated and quantified for EDGE (Edge-base Droplet GEneration) devices that have a specific behavior that allows us to distinguish between surfactant and liquid interactions with the solid surface. Based on these findings, design rules can be defined for emulsification with any micro-structured emulsification device, such as direct and premix membrane emulsification. In general, it can be concluded that mostly surface interactions increase the contact angle toward 90°, either through the surfactant, or the oil that is used. This leads to poor process stability, and very limited pressure ranges at which small droplets can be made in microfluidic systems, and cross-flow membrane emulsification. In a limited number of cases, surface interactions can also lead to lower contact angles, thereby increasing the operational stability. This paper concludes with a guideline that can be used to come to the appropriate combination of membrane construction material (or any micro-structured device), surfactants and liquids, in combination with process conditions. PMID:27187484

  6. Drop formation using ferrofluids driven magnetically in a step emulsification device.

    PubMed

    Kahkeshani, Soroush; Di Carlo, Dino

    2016-07-01

    We present a microfluidic droplet generation technique, where instead of pumps, only magnetic field gradient strength adjusted by the position of an external magnet is used for controllable emulsification of ferrofluid containing solutions. Uniform droplet generation at frequencies O(1-100) Hz per channel for long periods of time (10s of minutes) were easily achieved. In this method, adding magnetic nanoparticles (10 nm) into aqueous solutions imparts a magnetic body force on the fluid in the presence of an external magnetic field gradient. Consequently, the aqueous fluid moves toward the position of an external magnet and towards a junction with a larger width and height oil filled reservoir. Emulsification occurs at the junction due to a rapid change in surface tension forces due to the abrupt change in channel height. Droplet generation rate could be controlled by adjusting surface tension/viscosity, number of channels, and strength of the magnetic force. The geometry of the channel, rather than flow rates or magnetic force, plays the dominant role in defining the droplet size. In addition, reagents mixed with ferrofluids could also be introduced from two or more separate inlets and mixed prior to emulsification as they move toward the step driven by magnetic force. Mixing reagents on chip and forming droplets all within a small foot-print defined by movement of an external magnet is a unique feature of this method suitable for point-of-care diagnostics and other bioengineering applications. PMID:27250530

  7. Probing insulin bioactivity in oral nanoparticles produced by ultrasonication-assisted emulsification/internal gelation

    PubMed Central

    Lopes, Marlene A; Abrahim-Vieira, Bárbara; Oliveira, Claudia; Fonte, Pedro; Souza, Alessandra M T; Lira, Tammy; Sequeira, Joana A D; Rodrigues, Carlos R; Cabral, Lúcio M; Sarmento, Bruno; Seiça, Raquel; Veiga, Francisco; Ribeiro, António J

    2015-01-01

    Alginate–dextran sulfate-based particles obtained by emulsification/internal gelation technology can be considered suitable carriers for oral insulin delivery. A rational study focused on the emulsification and particle recovery steps was developed in order to reduce particles to the nanosize range while keeping insulin bioactivity. There was a decrease in size when ultrasonication was used during emulsification, which was more pronounced when a cosurfactant was added. Ultrasonication add-on after particle recovery decreased aggregation and led to a narrower nanoscale particle-size distribution. Insulin encapsulation efficiency was 99.3%±0.5%, attributed to the strong pH-stabilizing electrostatic effect between insulin and nanoparticle matrix polymers. Interactions between these polymers and insulin were predicted using molecular modeling studies through quantum mechanics calculations that allowed for prediction of the interaction model. In vitro release studies indicated well-preserved integrity of nanoparticles in simulated gastric fluid. Circular dichroism spectroscopy proved conformational stability of insulin and Fourier transform infrared spectroscopy technique showed rearrangements of insulin structure during processing. Moreover, in vivo biological activity in diabetic rats revealed no statistical difference when compared to nonencapsulated insulin, demonstrating retention of insulin activity. Our results demonstrate that alginate–dextran sulfate-based nanoparticles efficiently stabilize the loaded protein structure, presenting good physical properties for oral delivery of insulin. PMID:26425087

  8. Water-in-oil emulsification in a non-uniform alternating electric field

    NASA Astrophysics Data System (ADS)

    Choi, Suhwan; Saveliev, Alexei

    2015-11-01

    The emulsification of a water microdroplet placed in castor oil was performed using a non-uniform alternating electric field formed in the pin-to-plate geometry. A non-uniform electric field of ~40 kV/mm alternating with a frequency of 6.7 kHz was generated near the pin electrode. The applied frequency exceeded charge relaxation frequency of castor oil (0.3 Hz) and was below charge relaxation frequency of deionized water (7.8 kHz) used in the experiments. The emulsification process was captured with a CCD camera. The emulsification process started with entrainment of the water droplet in the high electric filed region near the pin electrode under the dielectrophoretic force. Upon touching the pin, the microdroplet was disintegrated in numerous channels and secondary droplets. The process continued by entrainment of secondary droplets and continuous size reduction. Three droplet breakup mechanisms were identified: drop elongation and capillary breakup, ac electrospraying of individual droplets, chain and bridge formation and decay. The quasi-steady narrow size distribution of emulsified water droplets with diameters close to 1 μm was formed after a few minutes. The generated emulsion was confined near the needle electrode due to the dielectrophoretic force. The emulsion had a well-defined boundary with a shape resembling a pendant drop suspended on the pin electrode.

  9. Probing insulin bioactivity in oral nanoparticles produced by ultrasonication-assisted emulsification/internal gelation.

    PubMed

    Lopes, Marlene A; Abrahim-Vieira, Bárbara; Oliveira, Claudia; Fonte, Pedro; Souza, Alessandra M T; Lira, Tammy; Sequeira, Joana A D; Rodrigues, Carlos R; Cabral, Lúcio M; Sarmento, Bruno; Seiça, Raquel; Veiga, Francisco; Ribeiro, António J

    2015-01-01

    Alginate-dextran sulfate-based particles obtained by emulsification/internal gelation technology can be considered suitable carriers for oral insulin delivery. A rational study focused on the emulsification and particle recovery steps was developed in order to reduce particles to the nanosize range while keeping insulin bioactivity. There was a decrease in size when ultrasonication was used during emulsification, which was more pronounced when a cosurfactant was added. Ultrasonication add-on after particle recovery decreased aggregation and led to a narrower nanoscale particle-size distribution. Insulin encapsulation efficiency was 99.3%±0.5%, attributed to the strong pH-stabilizing electrostatic effect between insulin and nanoparticle matrix polymers. Interactions between these polymers and insulin were predicted using molecular modeling studies through quantum mechanics calculations that allowed for prediction of the interaction model. In vitro release studies indicated well-preserved integrity of nanoparticles in simulated gastric fluid. Circular dichroism spectroscopy proved conformational stability of insulin and Fourier transform infrared spectroscopy technique showed rearrangements of insulin structure during processing. Moreover, in vivo biological activity in diabetic rats revealed no statistical difference when compared to nonencapsulated insulin, demonstrating retention of insulin activity. Our results demonstrate that alginate-dextran sulfate-based nanoparticles efficiently stabilize the loaded protein structure, presenting good physical properties for oral delivery of insulin. PMID:26425087

  10. Centrifugal step emulsification applied for absolute quantification of nucleic acids by digital droplet RPA.

    PubMed

    Schuler, Friedrich; Schwemmer, Frank; Trotter, Martin; Wadle, Simon; Zengerle, Roland; von Stetten, Felix; Paust, Nils

    2015-07-01

    Aqueous microdroplets provide miniaturized reaction compartments for numerous chemical, biochemical or pharmaceutical applications. We introduce centrifugal step emulsification for the fast and easy production of monodisperse droplets. Homogenous droplets with pre-selectable diameters in a range from 120 μm to 170 μm were generated with coefficients of variation of 2-4% and zero run-in time or dead volume. The droplet diameter depends on the nozzle geometry (depth, width, and step size) and interfacial tensions only. Droplet size is demonstrated to be independent of the dispersed phase flow rate between 0.01 and 1 μl s(-1), proving the robustness of the centrifugal approach. Centrifugal step emulsification can easily be combined with existing centrifugal microfluidic unit operations, is compatible to scalable manufacturing technologies such as thermoforming or injection moulding and enables fast emulsification (>500 droplets per second and nozzle) with minimal handling effort (2-3 pipetting steps). The centrifugal microfluidic droplet generation was used to perform the first digital droplet recombinase polymerase amplification (ddRPA). It was used for absolute quantification of Listeria monocytogenes DNA concentration standards with a total analysis time below 30 min. Compared to digital droplet polymerase chain reaction (ddPCR), with processing times of about 2 hours, the overall processing time of digital analysis was reduced by more than a factor of 4. PMID:25947077

  11. Solid drop based liquid-phase microextraction.

    PubMed

    Ganjali, Mohammad Reza; Sobhi, Hamid Reza; Farahani, Hadi; Norouzi, Parviz; Dinarvand, Rassoul; Kashtiaray, Amir

    2010-04-16

    Solid drop based liquid-phase microextraction (SDLPME) is a novel sample preparation technique possessing obvious advantages of simple operation with a high pre-concentration factor, low cost and low consumption of organic solvent. SDLPME coupled with gas chromatography (GC), high-performance liquid chromatography (HPLC), and atomic absorption spectrometry (AAS) has been widely applied to the analyses of a different variety of samples. The basic principles, parameters affecting the extraction efficiency, and the latest applications of SDLPME are reviewed in this article. PMID:19962710

  12. Fluorous receptor-facilitated solid phase microextraction.

    PubMed

    Lu, Dujuan; Weber, Stephen

    2014-09-19

    Solid phase microextraction (SPME) is a widely accepted solvent-free extraction technique that usually uses a polymer sorbent as the extraction phase. In this work, we have developed receptor-doped fluorous films for solid phase microextraction. The hydrophobic and lipophobic properties of the fluorous films in principle reduce the polymer-water distribution coefficients of solutes other than those that can form noncovalent interactions with the fluorous receptor. This strategy should improve extraction selectivity. We found that the addition of a fluorous carboxylic acid (Krytox 157 FSH) to a fluorous film (Teflon AF 2400) increased the polymer-water distribution coefficients of quinoline, a nitrogen heterocycle. We studied the effects of receptor concentration and solute concentration on the distribution coefficients based on 96-well vessel SPME. We then coated this receptor doped fluorous polymer on a stainless steel fiber for SPME. Compared to a commonly used SPME fiber made of polydimethylsiloxane (PDMS), it showed a preference for the nitrogen heterocyclic compound over a non-heterocyclic control, phenol. To our knowledge, this is the first reported receptor-doped fluorous SPME. PMID:25092595

  13. Impact of the emulsification-diffusion method on the development of pharmaceutical nanoparticles.

    PubMed

    Quintanar-Guerrero, David; Zambrano-Zaragoza, María de la Luz; Gutierrez-Cortez, Elsa; Mendoza-Munoz, Nestor

    2012-12-01

    Nanotechnology is having a profound impact in many scientific fields and it has become one of the most important and exciting discipline. Like all technological advances, nanotechnology has its own scientific basis with a broad interdisciplinary effect. Perhaps, we are witnessing an exponential growth of nanotechnology, reflection of this is the important increase in the number of patents, scientific papers and specialized "nano" meetings and journals. The impact in the pharmaceutical area is related to the use of colloidal drug delivery systems as carriers for bioactive agents, in particular, the nanoparticle technology. The term nanoparticles designates solid submicronic particles formed of acceptable materials (e.g. polymers, lipids, etc.) containing an active substance. It includes both nanospheres (matricial systems) and nanocapsules (membrane systems). The knowledge of the nanoparticle preparation methods is a key issue for the formulator involved with drug-delivery research and development. In general, the methods based on preformed polymers, in particular biodegradable polymers, are preferred due to their easy implementation and lower potential toxicity. One of the most widely used methods to prepare polymeric nanoparticles is emulsification-diffusion. This method has been discussed in some reviews that compile research works but has a small number of patents. In this review, the emulsification-diffusion method is discussed from a technological point of view in order to show the operating conditions and formulation variables from data extracted of recent patents and experimental works. The main idea is to provide the reader with a general guide for formulators to make decisions about the usefulness of this method to develop specific nanoparticulate systems. The first part of this review provides an overview of the emulsification-diffusion method to prepare polymeric nanoparticles, while the second part evaluates the influence of preparative variables on the

  14. Emulsification efficiency of adsorbed chitosan for bacterial cells accumulation at the oil-water interface.

    PubMed

    Archakunakorn, Somwit; Charoenrat, Nattapat; Khamsakhon, Somruethai; Pongtharangkul, Thunyarat; Wongkongkatep, Pravit; Suphantharika, Manop; Wongkongkatep, Jirarut

    2015-04-01

    The use of bacterial cell or biocatalyst for industrial synthetic chemistry is on the way of significant growth since the biocatalyst requires low energy input compared to the chemical synthesis and can be considered as a green technology. However, majority of natural bacterial cell surface is hydrophilic which allows poor access to the hydrophobic substrate or product. In this study, Escherichia coli (E. coli) as a representative of hydrophilic bacterial cells were accumulated at the oil-water interface after association with chitosan at a concentration range of 0.75-750 mg/L. After association with negatively charged E coli having a ζ potential of -19.9 mV, a neutralization of positively charged chitosan occurred as evidenced by an increase in the ζ potential value of the mixtures with increasing chitosan concentration up to +3.5 mV at 750 mg/L chitosan. Both emulsification index and droplet size analysis revealed that chitosan-E. coli system is an excellent emulsion stabilizer to date because the threshold concentration was as low as 7.5 mg/L or 0.00075% w/v. A dramatic increase in the surface hydrophobicity of the E. coli as evidenced by an increase in contact angle from 19 to 88° with increasing chitosan concentration from 0 to 750 mg/L, respectively, resulted in an increase in the stability of oil-in-water emulsions stabilized by chitosan-E. coli system. The emulsion was highly stable even the emulsification was performed under 20% salt condition, or temperature ranged between 20 and 50 °C. Emulsification was failed when the oil volume fraction was higher than 0.5, indicating that no phase inversion occurred. The basic investigation presented in this study is a crucial platform for its application in biocatalyst industry and bioremediation of oil spill. PMID:25341365

  15. Simultaneous derivatization and extraction of chlorophenols in water samples with up-and-down shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography/mass spectrometric detection.

    PubMed

    Wang, Ke-Deng; Chen, Pai-Shan; Huang, Shang-Da

    2014-03-01

    A new up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME) for extraction and derivatization of five chlorophenols (4-chlorophenol, 4-chloro-2-methylphenol, 2,4-dichlorophenol, 2,4,6-trichloro-phenol, and pentachlorophenol) has been developed. The method requires minimal solvent usage. The relatively polar, water-soluble, and low-toxicity solvent 1-heptanol (12 μL) was selected as the extraction solvent and acetic anhydride (50 μL) as the derivatization reagent. With the use of an up-and-down shaker, the emulsification of aqueous samples was formed homogeneously and quickly. The derivatization and extraction of chlorophenols were completed simultaneously in 1 min. The common requirement of disperser solvent in DLLME could be avoided. After optimization, the linear range covered over two orders of magnitude, and the coefficient of determination (r (2)) was greater than 0.9981. The detection limit was from 0.05 to 0.2 μg L(-1), and the relative standard deviation was from 4.6 to 10.8 %. Real samples of river water and lake water had relative recoveries from 90.3 to 117.3 %. Other emulsification methods such as vortex-assisted, ultrasound-assisted, and manual shaking-enhanced ultrasound-assisted methods were also compared with the proposed UDSA-DLLME. The results revealed that UDSA-DLLME performed with higher extraction efficiency and precision compared with the other methods. PMID:23727731

  16. Optimization of folic acid nano-emulsification and encapsulation by maltodextrin-whey protein double emulsions.

    PubMed

    Assadpour, Elham; Maghsoudlou, Yahya; Jafari, Seid-Mahdi; Ghorbani, Mohammad; Aalami, Mehran

    2016-05-01

    Due to susceptibility of folic acid like many other vitamins to environmental and processing conditions, it is necessary to protect it by highly efficient methods such as micro/nano-encapsulation. Our aim was to prepare and optimize real water in oil nano-emulsions containing folic acid by a low energy (spontaneous) emulsification technique so that the final product could be encapsulated within maltodextrin-whey protein double emulsions. A non ionic surfactant (Span 80) was used for making nano-emulsions at three dispersed phase/surfactant ratios of 0.2, 0.6, and 1.0. Folic acid content was 1.0, 2.0, and 3.0mg/mL of dispersed phase by a volume fraction of 5.0, 8.5, and 12%. The final optimum nano-emulsion formulation with 12% dispersed phase, a water to surfactant ratio of 0.9 and folic acid content of 3mg/mL in dispersed phase was encapsulated within maltodextrin-whey protein double emulsions. It was found that the emulsification time for preparing nano-emulsions was between 4 to 16h based on formulation variables. Droplet size decreased at higher surfactant contents and final nano-emulsions had a droplet size<100nm. Shear viscosity was higher for those formulations containing more surfactant. Our results revealed that spontaneous method could be used successfully for preparing stable W/O nano-emulsions containing folic acid. PMID:26806649

  17. Emulsification and antioxidation of biosurfactant extracts from Chinese medicinal herbs fermentation in vitro.

    PubMed

    Chen, Chunyeh; Lin, Tachen; Shieh, Youmin

    2015-10-01

    Much attention has been paid to biosurfactants produced using microorganisms, but little direct evidence for the development of natural biosurfactants combined with Chinese medicinal herbs are available. We investigated the emulsification and antioxidation of biosurfactant extracts from Chinese medicinal herb fermentation (BECMHF) in vitro and their application in water retention capacity and the skin prick and allergy test (SPAT) index for skin cells. The results showed that the water retention capacity of BECMHF was positively associated with the emulsification index. The SPAT index of 8 Chinese medicinal herbs was 0 at a 1% or 2% concentration, suggesting no sensitivity or adverse effects on the skin cells. Eight BECMHFs produced using Alcaligenes piechaudii CC-ESB2 exhibited antioxidant capabilities, including 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical and superoxide scavenging activity, and superoxide dismutase (SOD)-like activity at a concentration of 10 mg/ml. The mechanism involved inhibitory effects on nitrite, inducible nitric oxide synthase (iNOS) expression, and reactive oxygen species (ROSs) generation. BECMHFs exhibit favorable antioxidative properties in health food and satisfactory emulsifying and moisturizing characteristics in cosmetic formulations, which have potential applications in the health food and cosmetic industries, respectively. PMID:25812919

  18. Preparation of uniform-sized agarose beads by microporous membrane emulsification technique.

    PubMed

    Zhou, Qing-Zhu; Wang, Lian-Yan; Ma, Guang-Hui; Su, Zhi-Guo

    2007-07-01

    Uniform-sized agarose beads were prepared by membrane emulsification technique in this study. Agarose was dissolved in boiling water (containing 0.9% sodium chloride) and used as water phase. A mixture of liquid paraffin and petroleum ether containing 4 wt% of hexaglycerin penta ester (PO-500) emulsifier was used as oil phase. At 55 degrees C, the water phase permeated through uniform pores of microporous membrane into the oil phase by a pressure of nitrogen gas to form uniform W/O emulsion. Then the emulsion was cooled down to room temperature under gentle agitation to form gel beads. The effect of oil phase, emulsifier, especially temperature on the uniformity of the beads were investigated and interpreted from interfacial tension between water phase and oil phase. Under optimized condition, the coefficient variation (C.V.) showing the size distribution of the beads was under 15%. This was the first report to prepare uniform agarose beads by membrane emulsification, and to investigate the effect of temperature on the size distribution of the droplets and beads. The beads with different size can be prepared by using membranes with different pore size, and the result showed that there was a linear relationship between the average diameter of beads and pore size of the membranes; beads with diameter from 15 to 60 microm were able to obtain in this study. PMID:17362974

  19. Controlled tissue emulsification produced by high intensity focused ultrasound shock waves and millisecond boiling

    PubMed Central

    Khokhlova, Tatiana D.; Canney, Michael S.; Khokhlova, Vera A.; Sapozhnikov, Oleg A.; Crum, Lawrence A.; Bailey, Michael R.

    2011-01-01

    In high intensity focused ultrasound (HIFU) applications, tissue may be thermally necrosed by heating, emulsified by cavitation, or, as was recently discovered, emulsified using repetitive millisecond boiling caused by shock wave heating. Here, this last approach was further investigated. Experiments were performed in transparent gels and ex vivo bovine heart tissue using 1, 2, and 3 MHz focused transducers and different pulsing schemes in which the pressure, duty factor, and pulse duration were varied. A previously developed derating procedure to determine in situ shock amplitudes and the time-to-boil was refined. Treatments were monitored using B-mode ultrasound. Both inertial cavitation and boiling were observed during exposures, but emulsification occurred only when shocks and boiling were present. Emulsified lesions without thermal denaturation were produced with shock amplitudes sufficient to induce boiling in less than 20 ms, duty factors of less than 0.02, and pulse lengths shorter than 30 ms. Higher duty factors or longer pulses produced varying degrees of thermal denaturation combined with mechanical emulsification. Larger lesions were obtained using lower ultrasound frequencies. The results show that shock wave heating and millisecond boiling is an effective and reliable way to emulsify tissue while monitoring the treatment with ultrasound. PMID:22088025

  20. Spontaneous Emulsification of a Metal Drop Immersed in Slag Due to Dephosphorization: Surface Area Quantification

    NASA Astrophysics Data System (ADS)

    Assis, Andre N.; Warnett, Jason; Spooner, Stephen; Fruehan, Richard J.; Williams, Mark A.; Sridhar, Seetharaman

    2015-04-01

    When a chemical reaction occurs between two immiscible liquids, mass transfer is continuously taking place at the liquid-liquid interface. Several studies have shown that if the species being exchanged between the two liquids are surface-active, a very pronounced decrease in interfacial tension can occur which can lead to a phenomenon called spontaneous emulsification. In steelmaking, this behavior has been observed for several reactions that involve the transfer of impurities from molten steel to a molten-oxide slag but little quantification has been made. This work focuses on spontaneous emulsification due to the dephosphorization of a Fe-P drop immersed in a basic oxygen furnace type slag. An Au-image furnace attached to a confocal scanning laser microscope was used to rapidly heat and cool the samples at different times, and X-ray computerized tomography was used to perform the surface area calculations of the samples where the slag/steel reaction was allowed to occur for distinct times. The results show that the surface area of the metal drop rapidly increases by over one order of magnitude during the first 60 seconds of the reaction while the chemical reaction is occurring at a fast rate. Once the reaction slows down, approximately after 60 seconds, the droplets start to coalesce back together minimizing the surface area and returning to a geometry close to its equilibrium shape.

  1. A method for estimating effective coalescence rates during emulsification from oil transfer experiments.

    PubMed

    Håkansson, Andreas; Trägårdh, Christian; Bergenståhl, Björn

    2012-05-15

    The Oil Transfer Technique (OTT) was developed by Taisne et al. [1] to measure coalescence during emulsification and has been applied since in several studies. One of the main drawbacks of this technique is that it only gives a qualitative measure of coalescence. This paper proposes a new evaluation method of OTT experimental results for estimating qualitative coalescence rates, e.g. for investigating the scaling of coalescence with emulsification parameters (such as homogenizing pressure, and emulsifier concentration). The method is based on comparison with simulated OTT experiments using bivariate Population Balance Equation models. Simulations have been performed under a wide variety of conditions in order to investigate the influence of assumptions on coalescence and fragmentation kernels. These investigations show that the scaling of coalescence rates could be determined accurately when the scaling of efficient residence time of drops in the active region of homogenization is known. The proposed evaluation method is also exemplified by analyzing OTT data from two previously published studies. PMID:22369981

  2. Controlled tissue emulsification produced by high intensity focused ultrasound shock waves and millisecond boiling.

    PubMed

    Khokhlova, Tatiana D; Canney, Michael S; Khokhlova, Vera A; Sapozhnikov, Oleg A; Crum, Lawrence A; Bailey, Michael R

    2011-11-01

    In high intensity focused ultrasound (HIFU) applications, tissue may be thermally necrosed by heating, emulsified by cavitation, or, as was recently discovered, emulsified using repetitive millisecond boiling caused by shock wave heating. Here, this last approach was further investigated. Experiments were performed in transparent gels and ex vivo bovine heart tissue using 1, 2, and 3 MHz focused transducers and different pulsing schemes in which the pressure, duty factor, and pulse duration were varied. A previously developed derating procedure to determine in situ shock amplitudes and the time-to-boil was refined. Treatments were monitored using B-mode ultrasound. Both inertial cavitation and boiling were observed during exposures, but emulsification occurred only when shocks and boiling were present. Emulsified lesions without thermal denaturation were produced with shock amplitudes sufficient to induce boiling in less than 20 ms, duty factors of less than 0.02, and pulse lengths shorter than 30 ms. Higher duty factors or longer pulses produced varying degrees of thermal denaturation combined with mechanical emulsification. Larger lesions were obtained using lower ultrasound frequencies. The results show that shock wave heating and millisecond boiling is an effective and reliable way to emulsify tissue while monitoring the treatment with ultrasound. PMID:22088025

  3. Ultrasound-assisted emulsification of cosmetic samples prior to elemental analysis by different atomic spectrometric techniques.

    PubMed

    Lavilla, I; Cabaleiro, N; Costas, M; de la Calle, I; Bendicho, C

    2009-11-15

    In this work, ultrasound-assisted emulsification with a probe system is proposed as a rapid and simple sample treatment for atomic spectrometric determinations (Electrothermal Atomic Absorption Spectrometry, Inductively Coupled Plasma Optical Emission Spectrometry, Flame Atomic Absorption Spectrometry and Cold Vapour Atomic Absorption Spectrometry) of trace elements (As, Cd, Cr, Cu, Hg, Mg, Mn, Ni, Sr and Zn) in cosmetic samples such as shampoos, gel (hair gel), crèmes (body milk, hair conditioner) and oil (body oil). The type of dispersion medium, the sample mass-to-dispersion medium volume ratio, as well as the parameters related to the ultrasound-assisted emulsification (sonication amplitude and treatment time) were exhaustively studied. Only 1 min of ultrasonic shaking and a dispersion medium containing 0.5% (w/v) of SDS+3% (v/v) of HNO(3) or HCl allows obtaining a stable emulsion at least for 3 months. Thermal programs, nebulization of emulsions, speed of pumps and concentration of reagents used in cold vapour generation were optimized. Calibration using aqueous standards was feasible in all cases. Calibration by the standard addition method and recovery studies was also applied for validation. Microwave-assisted digestion and Inductively Coupled Plasma Mass Spectrometry were used for comparison purposes. Relative standard deviations from analysis of five independent emulsions were less than 9% in all cases. PMID:19782199

  4. Preparation of lipid nanoemulsions by premix membrane emulsification with disposable materials.

    PubMed

    Gehrmann, Sandra; Bunjes, Heike

    2016-09-25

    The possibility to prepare nanoemulsions as drug carrier systems on small scale was investigated with disposable materials. For this purpose premix membrane emulsification (premix ME) as a preparation method for nanoemulsions with narrow particle size distributions on small scale was used. The basic principle of premix ME is that the droplets of a coarse pre-emulsion get disrupted by the extrusion through a porous membrane. In order to implement the common preparation setup for premix ME with disposable materials, the suitability of different syringe filters (made from polyethersulfone, cellulose acetate, cellulose ester and nylon) and different pharmaceutically relevant emulsifiers (phospholipids, polysorbate 80 and sucrose laurate) for the preparation of nanoemulsions was investigated. Already the preparation of the premix could be realized by emulsification with the help of two disposable syringes. As shown for a phospholipid-stabilized emulsion, the polyethersulfone filter was the most appropriate one and was used for the study with different emulsifiers. With this syringe filter, the median particle size of all investigated emulsions was below 500nm after 21 extrusion cycles through a 200nm filter and a subsequent extrusion cycle through a 100nm filter. Furthermore, the particle size distribution of the polysorbate 80- and sucrose laurate-stabilized emulsions prepared this way was very narrow (span value of 0.7). PMID:27477104

  5. Influence of emulsification process on the properties of Pickering emulsions stabilized by layered double hydroxide particles.

    PubMed

    Zhang, Nana; Zhang, Li; Sun, Dejun

    2015-04-28

    This paper reports the influence of emulsification process on the packing of layered double hydroxide (LDH) particles at the aqueous/oil phase interface and the properties of the resulting Pickering emulsions. Emulsions prepared by ultrasonication display superior long-term stability and gel-like characteristics at the dispersed phase volume fraction well below the random close packing limit, whereas emulsions with same compositions prepared by vortex mixing show some extent of sedimentation and liquid-like behaviors. Rheological measurements demonstrate that the zero-shear elastic modulus and yield stress of gel-like emulsions exhibit power-law dependences on particle concentration and independence on aqueous/oil phase ratio. The microstructural origin of this behavior is investigated by optical microscopy, revealing the droplets become strongly adhesive and a heterogeneous percolating network is formed among neighboring droplets. Fluorescent confocal microscopy measurements further confirm that the droplet adhesion is due to particle layers bridging opposite interfaces. In contrast, homogeneous, isolated, and densely packed droplets are present in emulsions prepared by vortex mixing, which results in these systems being dominantly viscous like the suspending fluid. This study shows that the emulsification process can be used as a trigger to modify long-term stability and rheology of solid-stabilized multiphase mixtures, which greatly expands their potential technological applications. PMID:25853297

  6. Microencapsulation by Membrane Emulsification of Biophenols Recovered from Olive Mill Wastewaters

    PubMed Central

    Piacentini, Emma; Poerio, Teresa; Bazzarelli, Fabio; Giorno, Lidietta

    2016-01-01

    Biophenols are highly prized for their free radical scavenging and antioxidant activities. Olive mill wastewaters (OMWWs) are rich in biophenols. For this reason, there is a growing interest in the recovery and valorization of these compounds. Applications for the encapsulation have increased in the food industry as well as the pharmaceutical and cosmetic fields, among others. Advancements in micro-fabrication methods are needed to design new functional particles with target properties in terms of size, size distribution, and functional activity. This paper describes the use of the membrane emulsification method for the fine-tuning of microparticle production with biofunctional activity. In particular, in this pioneering work, membrane emulsification has been used as an advanced method for biophenols encapsulation. Catechol has been used as a biophenol model, while a biophenols mixture recovered from OMWWs were used as a real matrix. Water-in-oil emulsions with droplet sizes approximately 2.3 times the membrane pore diameter, a distribution span of 0.33, and high encapsulation efficiency (98% ± 1% and 92% ± 3%, for catechol and biophenols, respectively) were produced. The release of biophenols was also investigated. PMID:27171115

  7. Solid phase microextraction device using aerogel

    DOEpatents

    Miller, Fred S.; Andresen, Brian D.

    2005-06-14

    A sample collection substrate of aerogel and/or xerogel materials bound to a support structure is used as a solid phase microextraction (SPME) device. The xerogels and aerogels may be organic or inorganic and doped with metals or other compounds to target specific chemical analytes. The support structure is typically formed of a glass fiber or a metal wire (stainless steel or kovar). The devices are made by applying gel solution to the support structures and drying the solution to form aerogel or xerogel. Aerogel particles may be attached to the wet layer before drying to increase sample collection surface area. These devices are robust, stable in fields of high radiation, and highly effective at collecting gas and liquid samples while maintaining superior mechanical and thermal stability during routine use. Aerogel SPME devices are advantageous for use in GC/MS analyses due to their lack of interfering background and tolerance of GC thermal cycling.

  8. Offline solid phase microextraction sampling system

    DOEpatents

    Harvey, Chris A.

    2008-12-16

    An offline solid phase microextraction (SPME) sampling apparatus for enabling SPME samples to be taken a number of times from a previously collected fluid sample (e.g. sample atmosphere) stored in a fused silica lined bottle which keeps volatile organics in the fluid sample stable for weeks at a time. The offline SPME sampling apparatus has a hollow body surrounding a sampling chamber, with multiple ports through which a portion of a previously collected fluid sample may be (a) released into the sampling chamber, (b) SPME sampled to collect analytes for subsequent GC analysis, and (c) flushed/purged using a fluidically connected vacuum source and purging fluid source to prepare the sampling chamber for additional SPME samplings of the same original fluid sample, such as may have been collected in situ from a headspace.

  9. Ferrofluid-based liquid-phase microextraction.

    PubMed

    Shi, Zhi-Guo; Zhang, Yufeng; Lee, Hian Kee

    2010-11-19

    A new mode of liquid-phase microextraction based on a ferrofluid has been developed. The ferrofluid was composed of silica-coated magnetic particles and 1-octanol as the extractant solvent. The 1-octanol was firmly confined within the silica-coated particles, preventing it from being lost during extraction. Sixteen polycyclic aromatic hydrocarbons (PAHs) were used as model compounds in the development and evaluation of the extraction procedure in combination with gas chromatography-mass spectrometry. Parameters affecting the extraction efficiency were investigated in detail. The optimal conditions were as follows: 20mL sample volume, 10mg of the silica-coated magnetic particles (28mg of ferrofluid), agitation at 20Hz, 20min extraction time, and 2min by sonication with 100μL acetonitrile as the final extraction solvent. Under optimal extraction conditions, enrichment factors ranging from 102- to 173-fold were obtained for the analytes. The limits of detection and the limits of quantification were in the range of 16.8 and 56.7pgmL(-1) and 0.06 and 0.19ngmL(-1), respectively. The linearities were between 0.5-100 and 1-100ngmL(-1) for different PAHs. As the ferrofluid can respond to and be attracted by a magnet, the extraction can be easily achieved by reciprocating movement of an external magnet that served to agitate the sample. No other devices were needed in this new approach of extraction. This new technique is affordable, efficient and convenient for microextraction, and offers portability for potential onsite extraction. PMID:20961552

  10. Monolithic microextraction tips by emulsion photopolymerization.

    PubMed

    Liang, Shih-Shin; Chen, Shu-Hui

    2009-03-20

    Monoliths formed by photopolymerization are excellent means for fabricating functional elements in miniaturized microdevices such as microextraction tips which are becoming important for sample preparation. Various silica-based and polymer-based materials have been used to fabricate monoliths with through pores of several nm to 4 microm. However, the back pressure created by such methods is still considered to be high for microtips that use suction forces to deliver the liquid. In this study, we demonstrated that emulsion techniques such as oil-in-water can be used to form monoliths with large through pores (>20 microm), and with rigid structures on small (10 microL) and large (200 microL) pipette tips by photopolymerization. We further showed that, with minor modifications, various functionalized particles (5-20 microm) can be added to form stable emulsions and successfully encapsulated into the monoliths for qualitative and quantitative solid-phase microextractions for a diverse application. Due to high permeability and large surface area, quick equilibration can be achieved by pipetting to yield high recovery rates. Using tryptic digests of ovalbumin as the standard, we obtained a recovery yield of 90-109% (RSD: 10-16%) with a loading capacity of 3 mug for desalting tips immobilized with C18 beads. Using tryptic digests of beta-casein and alpha-casein as standards, we showed that phosphopeptides were substantially enriched by tips immobilized with immobilized metal affinity chromatography or TiO(2) materials. Using estrogenic compounds as standards, we obtained a recovery yield of 95-108% (RSD: 10-12%) and linear calibration curves ranging from 5 to 100 ng (R(2)>0.99) for Waters Oasis HLB tips immobilized with hydrophilic beads. PMID:19203757

  11. Investigation into the Cause of Spontaneous Emulsification of a Free Steel Droplet; Validation of the Chemical Exchange Pathway

    NASA Astrophysics Data System (ADS)

    Spooner, Stephen; Assis, Andre N.; Warnett, Jason; Fruehan, Richard; Williams, Mark A.; Sridhar, Seetharaman

    2016-05-01

    Small Fe-based droplets have been heated to a molten phase suspended within a slag medium to replicate a partial environment within the basic oxygen furnace (BOF). The confocal scanning laser microscope (CSLM) has been used as a heating platform to interrogate the effect of impurities and their transfer across the metal/slag interface, on the emulsification of the droplet into the slag medium. The samples were then examined through X-ray computer tomography (XCT) giving the mapping of emulsion dispersion in 3D space, calculating the changing of interfacial area between the two materials, and changes of material volume due to material transfer between metal and slag. Null experiments to rule out thermal gradients being the cause of emulsification have been conducted as well as replication of the previously reported study by Assis et al.[1] which has given insights into the mechanism of emulsification. Finally chemical analysis was conducted to discover the transfer of oxygen to be the cause of emulsification, leading to a new study of a system with undergoing oxygen equilibration.

  12. Self-emulsification of alkaline-dissolved clove bud oil by whey protein, gum arabic, lecithin, and their combinations.

    PubMed

    Luo, Yangchao; Zhang, Yue; Pan, Kang; Critzer, Faith; Davidson, P Michael; Zhong, Qixin

    2014-05-14

    Low-cost emulsification technologies using food ingredients are critical to various applications. In the present study, a novel self-emulsification technique was studied to prepare clove bud oil (CBO) emulsions, without specialized equipment or organic solvents. CBO was first dissolved in hot alkaline solutions, added at 1% v/v into neutral solutions with 1% w/v emulsifier composed of whey protein concentrate (WPC), gum arabic, lecithin, or their equal mass mixtures, and adjusted to pH 7.0. The self-emulsification process did not affect UV-vis absorption spectrum, reversed-phase HPLC chromatogram, or antimicrobial activity of CBO against Escherichia coli O157:H7, Listeria monocytogenes Scott A, and Salmonella Enteritidis. The entrapment efficiency after extraction by petroleum ether was determined to be about 80%. Most emulsions were stable during 7 days of storage. Emulsions prepared with WPC had smaller particles, whereas emulsions prepared with emulsifier mixtures had more stable particle dimensions. The studied self-emulsification technique may find numerous applications in the preparation of low-cost food emulsions. PMID:24758517

  13. Investigation into the Cause of Spontaneous Emulsification of a Free Steel Droplet; Validation of the Chemical Exchange Pathway

    NASA Astrophysics Data System (ADS)

    Spooner, Stephen; Assis, Andre N.; Warnett, Jason; Fruehan, Richard; Williams, Mark A.; Sridhar, Seetharaman

    2016-08-01

    Small Fe-based droplets have been heated to a molten phase suspended within a slag medium to replicate a partial environment within the basic oxygen furnace (BOF). The confocal scanning laser microscope (CSLM) has been used as a heating platform to interrogate the effect of impurities and their transfer across the metal/slag interface, on the emulsification of the droplet into the slag medium. The samples were then examined through X-ray computer tomography (XCT) giving the mapping of emulsion dispersion in 3D space, calculating the changing of interfacial area between the two materials, and changes of material volume due to material transfer between metal and slag. Null experiments to rule out thermal gradients being the cause of emulsification have been conducted as well as replication of the previously reported study by Assis et al.[1] which has given insights into the mechanism of emulsification. Finally chemical analysis was conducted to discover the transfer of oxygen to be the cause of emulsification, leading to a new study of a system with undergoing oxygen equilibration.

  14. A Simple Organic Solvent-Free Liquid-Liquid Microextraction Method for the Determination of Potentially Toxic Metals as 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol Complex from Food and Biological Samples.

    PubMed

    Barfi, Behruz; Rajabi, Maryam; Asghari, Alireza

    2016-04-01

    An organic solvent-free method was developed to extract some potentially toxic metals, as complexed with 2-(5-bromo-2-pyridylazo)-5-(diethylamino)phenol, from different real samples prior to their determination by microsampling flame atomic absorption spectrometry. The method, named ionic liquid-based ultrasound-enhanced air-assisted liquid-liquid microextraction (IL-USE-AALLME), is based upon withdrawing and pushing out a mixture of an aqueous sample and an IL (as the extraction solvent) for several times into a conical test tube using a single syringe, placed in an ultrasound bath (as the enhancing mass transfer agent) during the extraction process. Different effective parameters were studied, and at the optimized conditions, limits of detection, linear dynamic ranges, and enrichment factors were ranged from 0.9 to 2.2 μg L(-1), 3.0 to 1023 μg L(-1), and 20 ± 2 to 22 ± 2, respectively. After optimization, the method was successfully applied to determine Pb(2+), Cu(2+), Co(2+), Ni(2+), and Cr(3+) in different biological (hair and nail), vegetable (coriander, parsley, and tarragon), fruit juice (apple, orange, and peach), and water (tap, mineral, and wastewater) samples. The proposed method was compared with two other IL-based and disperser solvent-free methods (i.e., IL-based air-assisted liquid-liquid microextraction and IL-based ultrasound-assisted emulsification microextraction) to demonstrate its performance. PMID:26329998

  15. Green aspects, developments and perspectives of liquid phase microextraction techniques.

    PubMed

    Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

    2014-02-01

    Determination of analytes at trace levels in complex samples (e.g. biological or contaminated water or soils) are often required for the environmental assessment and monitoring as well as for scientific research in the field of environmental pollution. A limited number of analytical techniques are sensitive enough for the direct determination of trace components in samples and, because of that, a preliminary step of the analyte isolation/enrichment prior to analysis is required in many cases. In this work the newest trends and innovations in liquid phase microextraction, like: single-drop microextraction (SDME), hollow fiber liquid-phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME) have been discussed, including their critical evaluation and possible application in analytical practice. The described modifications of extraction techniques deal with system miniaturization and/or automation, the use of ultrasound and physical agitation, and electrochemical methods. Particular attention was given to pro-ecological aspects therefore the possible use of novel, non-toxic extracting agents, inter alia, ionic liquids, coacervates, surfactant solutions and reverse micelles in the liquid phase microextraction techniques has been evaluated in depth. Also, new methodological solutions and the related instruments and devices for the efficient liquid phase micoextraction of analytes, which have found application at the stage of procedure prior to chromatographic determination, are presented. PMID:24401382

  16. Uniform titanium dioxide (TiO(2)) microcapsules prepared by glass membrane emulsification with subsequent solvent evaporation.

    PubMed

    Supsakulchai, A; Ma, G H; Nagai, M; Omi, S

    2002-01-01

    Anatase-type titanium dioxide (TiO(2)) was encapsulated using an Shirasu porous glass (SPG) membrane emulsification technique and followed by solvent evaporation. The oil phase, consisting of fine#10; powder of anatase TiO(2), Disperbyk-180, the hydrophobic oil phase additive, and polymer wall solution, was pushed through the membrane pores into the aqueous phase of poly(vinyl alcohol) and sodium dodecyl sulfate to form the solid-in-oil-in water, (S/O)/W, emulsion droplets. Three types of styrene-based copolymer poly(styrene-co-acrylic acid) (PS-AA), poly(styrene-co-2-ethyl hexyl acrylate) (PS-2EHA) and poly(styrene-co-dimethyl aminoethylmethacrylate) (PS-DMAEMA) were used as an encapsulating shell. Uniform droplets were successfully obtained by modifying the oil phase using methyl laurate or hexadecanol as the oil phase additive, together with carefully monitoring the emulsification flow rate during the emulsification. The (S/O)/W emulsion was gently stirred in a sealed reactor, and evacuation of solvent started under moderate heating with increasing a vacuum intensity. Those uniform-sized TiO(2) microcapsules revealed fine porous morphologies on their surfaces as a result of a mild phase separation induced from the addition of the oil phase additive. The encapsulation efficiency was influenced by the stability of TiO(2) in the oil phase, the polymer wall employed, and the operational control of the glass membrane emulsification process. The membrane emulsification process could prepare the TiO(2) microcapsules with about approximately 6-8.5 wt% of encapsulation loadings. PS-AA and PS-2EHA copolymers provided better encapsulation efficiency compared to PS-DMAEMA. SPG membranes with 1.42, 2.8, 5.25, 7.0, or 9.5 microm were employed and 2-20 microm microcapsules were subsequently obtained. PMID:12396381

  17. Effect of interfacial free energy on the formation of polymer microcapsules by emulsification/freeze-drying.

    PubMed

    Yin, Weisi; Yates, M Z

    2008-02-01

    Hollow polymer microparticles with a single opening on the surface were formed by freeze-drying aqueous polymer colloids swollen with solvent. The results show that the particle morphology is due to phase separation in the polymer emulsion droplets upon freezing in liquid nitrogen, and that morphological changes are driven largely by lowering interfacial free energy. The effects of added surfactant, volume fraction of solvent, type of solvent, and processing conditions on the particle morphology were examined and compared to theoretical predictions. The dried hollow particles were resuspended in a dispersing media and exposed to a second swelling solvent to close the surface opening and form microcapsules. The interfacial free energy difference between the inside and outside surfaces is the driving force for closing the hole on the surface. The emulsification/freeze-drying technique can be used to encapsulate hydrophilic additives in the core of the microcapsules, demonstrating the potential of the technique in controlled-release applications. PMID:18173290

  18. Preparation of solid lipid nanoparticles by a solvent emulsification-diffusion technique.

    PubMed

    Trotta, Michele; Debernardi, Francesca; Caputo, Otto

    2003-05-12

    A preparation method for nanoparticles based on the emulsification of a butyl lactate or benzyl alcohol solution of a solid lipid in an aqueous solution of different emulsifiers, followed by dilution of the emulsion with water, was used to prepare glyceryl monostearate nanodispersions with narrow size distribution. To increase the lipid load the process was conducted at 47+/-2 degrees C and in order to reach submicron size a high-shear homogenizer was used. Particle size of the solid lipid nanoparticles (SLN) was affected by using different emulsifiers and different lipid loads. By using lecithin and taurodeoxycholic acid sodium salt, on increasing the GMS percentage from 2.5 to 10% an increase of the mean diameter from 205 to 695 nm and from 320 to 368nm was observed for the SLN prepared using benzyl alcohol and butyl lactate, respectively. Transmission electron micrographs of SLN reveal nanospheres with a smooth surface. PMID:12711170

  19. Scale-up of nanoemulsion produced by emulsification and solvent diffusion.

    PubMed

    Mitri, Khalil; Vauthier, Christine; Huang, Nicolas; Menas, Assia; Ringard-Lefebvre, Catherine; Anselmi, Cecilia; Stambouli, Moncef; Rosilio, Veronique; Vachon, Jean-Jacques; Bouchemal, Kawthar

    2012-11-01

    The scale-up of nanoemulsions (NEs) produced by emulsification and solvent diffusion process was successfully achieved in the present work. Up to 1500 mL of NEs were produced with olive oil, castor oil, almond oil, or Arlamol™ E by using a Y-shaped mixer device. NE droplet sizes were significantly modulated from 290 to 185 nm by changing the process parameters without modification of the formulation composition. Smaller NE droplet sizes were obtained by (1) decreasing the internal diameter of the Y-mixer from 5 to 0.8 mm, (2) increasing the flow rates of the organic and the aqueous phases upon mixing, and (3) increasing the temperature of the experiment from 5°C to 40°C. All the results of NE diameters (d(sc) ) expressed as a function of the Reynolds number (Re) and the shear rate inside the Y-mixer (\\documentclass{article}\\usepackage{amssymb}\\begin{document}\\pagestyle{empty}$\\dot \\gamma$\\end{document}) showed the existence of typical power-law relationships: d(sc) = 10(2.82) Re(- 0.14) and \\documentclass{article}\\usepackage{amssymb}\\begin{document}\\pagestyle{empty}$d_{{\\rm sc}} = 10^{2.60} \\dot \\gamma ^{- 0.06}$\\end{document}, respectively. The existence of these power-laws for NE formation by emulsification and solvent diffusion process has never been reported in the literature yet and constitutes a new finding in this work. We definitely proved that the high turbulences created upon NE formation are the most important parameter allowing to decrease droplet size. PMID:22886515

  20. Conductive polymer-based microextraction methods: a review.

    PubMed

    Bagheri, Habib; Ayazi, Zahra; Naderi, Mehrnoush

    2013-03-12

    Conductive polymers (CPs) are classified as materials which exhibit highly reversible redox behavior and the unusual combined properties of metal and plastics. CPs, due to their multifunctionality, ease of synthesis and their stability, have attracted more attentions in different fields of research, including sample preparation. CPs along with several commercial hydrophilic sorbents, are alternative to the commercially available hydrophobic sorbents which despite their high specific surface areas, have poor interactions and retentions in the extraction of polar compounds. This review covers a general overview regarding the recent progress and new applications of CPs toward their synthesis and use in novel extraction and microextraction techniques including solid phase microextraction (SPME), electrochemically controlled solid-phase microextraction (EC-SPME) and other relevant techniques. Furthermore the contribution of nano-structured CPs in these methodologies is also reviewed. PMID:23452781

  1. Solvent-free microextraction techniques in gas chromatography.

    PubMed

    Laaks, Jens; Jochmann, Maik A; Schmidt, Torsten C

    2012-01-01

    Microextraction techniques represent a major part of modern sample preparation in the analysis of organic micropollutants. This article provides a short overview of recent developments in solvent-free microextraction techniques. From the first open-tubular trap techniques in the mid-1980s to recent packed-needle devices, different implementations of in-needle packings for microextraction are discussed with their characteristic benefits, shortcomings and possible sampling modes. Special emphasis is placed on methods providing full automation and solvent exclusion. In this context, in-tube extraction and the needle trap are discussed, with an overview of current research on new sorbent materials, together with the requirements for more efficient method development. PMID:22057686

  2. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-07-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal for instructional use, especially to illustrate HS analysis or as an alternative to solid-phase microextraction (SPME) to which it is very similar. The basic principles and practice of HS-GC using SDME are described, including a complete review of the literature. Some possible experiments are suggested using water and N -methylpyrrolidone (NMP) as solvents.

  3. Theory and practice of solid phase microextraction

    SciTech Connect

    Pawliszyn, J.; Zhang, Zhouyao; Gorecki, T.

    1995-12-31

    Solid Phase Microextraction (SPME) involves exposing a fused silica fibre that has been coated with a non-volatile polymeric liquid to a sample or its headspace. The absorbed analytes are thermally desorbed in the injector of a gas chromatograph (GC) or GC-mass spectrometer. The fibre is contained in a syringe-like SPME device to facilitate convenient handling. This method can be applied to liquid, gaseous or headspace samples. All three sample can be analyzed on the same instrument without modifications to the GC and the extraction and the sample injection process can be fully automated using conventional autosampler. The fibre can be used to extract target analytes directly in the field without collecting a sample. Because of its cylindrical geometry it cannot be plugged. All three sample types can be analyzed on the isothermal instrument. Advantageous of SPME will be discussed using important applications - semi-volatile and volatile compounds in air, aqueous matrices and in the headspace above dirty aqueous samples, slurries and soils.

  4. Dispersive micro-solid phase extraction using magnetic nanoparticle modified multi-walled carbon nanotubes coupled with surfactant-enhanced spectrofluorimetry for sensitive determination of lomefloxacin and ofloxacin from biological samples.

    PubMed

    Amoli-Diva, Mitra; Pourghazi, Kamyar; Hajjaran, Somayeh

    2016-03-01

    A dispersive micro-solid-phase extraction (D-μ-SPE) procedure coupled with surfactant-enhanced spectrofluorimetric detection was developed for determination of ofloxacin and lomefloxacin from biological and environmental samples. The D-μ-SPE procedure was performed using magnetic Fe3O4 nanoparticle grafted multi-walled carbon nanotube as an efficient adsorbent. The main factors affecting the signal enhancement (including surfactant concentration and pH) and extraction efficiency (including pH, extraction time, sample volume, amount of magnetic adsorbent, and desorption conditions) were investigated in detail. Under the optimized conditions, the calibration curves were linear (R(2)˃0.9995) over the concentration range of 50-450 ng mL(-1) with detection limits (LOD) of 12 and 15 ng mL(-1) for ofloxacin and lomefloxacin respectively. The relative standard deviation (RSD %) of 1.9 and 2.1% (C=100 ng mL(-1), n=5) and the enrichment factor of 192 and 188 were achieved for ofloxacin and lomefloxacin respectively. Finally, the method was successfully applied to the extraction and preconcentration of these drugs in biological (plasma and urine) samples. PMID:26706503

  5. Rapid ionic liquid-based ultrasound assisted dual magnetic microextraction to preconcentrate and separate cadmium-4-(2-thiazolylazo)-resorcinol complex from environmental and biological samples.

    PubMed

    Khan, Sumaira; Kazi, Tasneem Gul; Soylak, Mustafa

    2014-04-01

    A rapid and innovative microextraction technique named as, ionic liquid-based ultrasound-assisted dual magnetic microextraction (IL-UA-DMME) was developed for the preconcentration and extraction of trace cadmium from environmental and biological samples, prior to analyzed by flame atomic absorption spectrometry (FAAS). The proposed method has many obvious advantages, including evading the use of organic solvents and achieved high extraction yields by the combination of dispersive liquid-liquid microextraction (DLLME) and magnetic mediated-solid phase extraction (MM-SPE). In this approach ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] play an important role to extract the cadmium-4-(2-thiazolylazo)-resorcinol (Cd-TAR) complex from acid digested sample solutions and ultrasonic irradiation was applied to assist emulsification. After then, dispersed small amount of Fe3O4 magnetic nanoparticles (MNPs) in sample solutions to salvaged the IL and complete phase separation was attained. Some analytical parameters that influencing the efficiency of proposed (IL-UA-DMME) method, such as pH, volume of IL, ligand concentration, ultra-sonication time, amount of Fe3O4 MNPs, sample volume and matrix effect were optimized. Limit of detection (LOD) and enrichment factor (EF) of the method under optimal experimental conditions were found to be 0.40μgL(-1) and 100, respectively. The relative standard deviation (RSD) of 50μgL(-1) Cd was 4.29%. The validity and accuracy of proposed method, was assessed to analyzed certified reference materials of fortified lake water TMDA-54.4, SPS-WW2 waste water, spinach leaves 1570a and also checked by standard addition method. The obtained values showed good agreement with the certified values and sufficiently high recovery were found in the range of 98.1-101% for Cd. The proposed method was facile, rapid and successfully applied for the determination of Cd in environmental and different biological samples. PMID

  6. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    ERIC Educational Resources Information Center

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-01-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal…

  7. Micro-extraction techniques in analytical toxicology: short review.

    PubMed

    Flanagan, R J; Morgan, P E; Spencer, E P; Whelpton, R

    2006-01-01

    This paper discusses new developments in plasma micro-extraction techniques in the context of established micro-extraction and protein precipitation methodology. Simple liquid-liquid solvent extraction (LLE) of plasma with direct GC or HPLC analysis of the resulting extract has been used for many years. Butyl acetate and methyl t-butyl ether (MTBE) give efficient extraction of many drugs and metabolites from small volumes of plasma or whole blood at an appropriate pH, and form the upper layer, thus simplifying extract removal. Butyl acetate does not interfere with NPD, ECD or MS in GC, whilst MTBE has a relatively low UV cutoff (220 nm). Thus, HPLC eluents that use a high proportion of an organic component allow MTBE extracts to be analysed directly. 'Salting-out' and extractive derivatization using acetic anhydride or phenylboronic acid can be used with appropriate analytes. As regards protein precipitation, an important consideration is lowering the pH, although this is not feasible with acid-labile analytes. More recent developments include sold-phase micro-extraction (SPME) and liquid-phase micro-extraction (LPME). This latter technique especially may prove invaluable as analytes that cannot easily be extracted with LLE can be isolated simply at low cost with a minimum of apparatus. PMID:16779788

  8. Preparation and properties of PLGA microspheres containing hydrophilic drugs by the SPG (shirasu porous glass) membrane emulsification technique.

    PubMed

    Ito, Fuminori; Honnami, Hiroyuki; Kawakami, Hiroyoshi; Kanamura, Kiyoshi; Makino, Kimiko

    2008-11-15

    In the present paper, monodisperse poly (lactide-co-glycolide) (PLGA) microspheres containing the hydrophilic model drug, blue dextran (BLD), were manufactured by the solvent evaporation method and the shirasu porous glass (SPG) membrane emulsification technique. In order to prepare PLGA microspheres with a higher drug loading efficiency by the membrane emulsification technique, the test of stability and productivity of the primary emulsion (w(1)/o emulsion) was preliminary examined by change species or concentration of the oil-soluble surfactant and the ratio of water and organic solvent. The primary emulsion (w(1)/o) composed of the BLD aqueous solution and dichloromethane (DCM) dissolved PLGA was prepared with the micro homogenizer. The secondary emulsion (w(1)/o/w(2)) was prepared by the SPG membrane emulsification technique. BLD/PLGA microspheres of various micro level sizes of 2.0-10 microm prepared by variation of pore size of the using SPG membrane. The highly monodisperse BLD/PLGA microspheres were also manufactured by added polyethylene glycol (PEG) into the water phase, as reported in a previous paper. The initial release rate of the drug from such microspheres controlled than the sample manufactured without an additive. PMID:18774278

  9. Role of medium-chain fatty acids in the emulsification mechanistics of self-micro-emulsifying lipid formulations

    PubMed Central

    Hasan, Naser M.Y.

    2014-01-01

    Purpose The objective of the present study was to design and develop stable o/w microemulsions comprising Miglyol 812, Imwitor 988 and Tagat TO as a non ionic surfactant. This was based on particle size measurements and phase behavior studies. The empirical role of incorporating medium-chain mono/di-glycerides in the lipid matrix in the mechanistic processes of emulsification was also established in various simulating physiological conditions. Methods The efficiency of self-emulsification was evaluated under conditions of varying key compositions in the lipid mixtures; oil, cosurfactant and surfactant. Droplet diameter was measured using laser diffraction and light scattering techniques. Equilibrium phase studies were performed and phase boundaries were determined for the lipid–water systems. Results Microemulsion systems were produced from blends of Miglyol 812, Imwitor 988 and Tagat TO. An optimized formulation consisted of {Miglyol 812/Imwitor 988} and Tagat TO spontaneously self-emulsified in water producing dispersions with droplet diameters of ∼50 nm. Phase equilibrium diagrams have revealed significant enhancement in the water-solubilized region (L2) without any presence of liquid crystalline materials. Conclusions Potential SMEDDS formulations for the bioavailability enhancement of poorly water-soluble compounds were developed by mixing blends of {Miglyol 812/Imwitor 988} and Tagat TO as a non-ionic surfactant. ‘Diffusion and stranding’ appears to be the dominant mechanism of emulsification. PMID:25561872

  10. Emulsification of algal oil with soy lecithin improved DHA bioaccessibility but did not change overall in vitro digestibility.

    PubMed

    Lin, Xinjie; Wang, Qi; Li, Weili; Wright, Amanda J

    2014-11-01

    Oil emulsification facilitates digestive lipolysis and subsequent lipid bioaccessibility. This study aimed to understand the effects of emulsification on DHA-rich algal oil digestion and bioaccessibility. An oil/water emulsion (50 : 44 : 6 oil-water-soy lecithin) was subjected to an in vitro digestion model with gastric pH 1.6 or 4.0 and particle size distributions, duodenal stage lipolysis and DHA bioaccessibility were determined. The emulsion was destabilized at gastric pH 1.6, with subsequent slow duodenal lipolysis. With gastric pH 4.0, the emulsion structure remained intact, initial lipolysis proceeded rapidly and DHA bioaccessibility was higher than for bulk oil, a mixture of oil, water and soy lecithin, and the gastric pH 1.6 destabilized emulsion (p < 0.05). However, the extent of lipolysis was not affected by emulsification or gastric pH. Therefore, the presence of an intact emulsion at the start of duodenal digestion, while not impacting the extent of lipolysis, did impact the initial lipolysis and DHA bioaccessibility. PMID:25208938

  11. Influence of rheology of dispersion media in the preparation of polymeric microspheres through emulsification method.

    PubMed

    Khare, Piush; Jain, Sanjay K

    2009-01-01

    Chitosan microspheres as drug delivery system have attained importance and attracted the attention of researchers in last few years. This study was aimed toward the elucidation of the effect of viscosity of external oil phase on the properties of microspheres prepared by emulsification method. Chitosan microspheres were prepared utilizing oil phase of different viscosity viz. castor oil, heavy liquid paraffin, light liquid paraffin and mixture of light paraffin, and petroleum ether (1:1 v/v ratio). Microspheres prepared in highly viscous castor oil exhibited an average size of 11.52+/-0.57 microm with a percentage drug entrapment of 43.12+/-2.14. On the other hand, very small microspheres of 3.15+/-0.04 microm and 68.87+/-1.03% drug entrapment were obtained when mixture of liquid paraffin and petroleum ether was utilized as oil phase. Effect of viscosity on percent mucoadhesion, percent drug entrapment, zeta potential, percent process yield, etc. of microspheres has been observed. In vitro drug release in phosphate buffer pH 7.4 was determined for different batch of microspheres. The results revealed a difference in the drug release pattern of the different microspheres prepared as a function of viscosity of different oil phase. Use of low viscose oil resulted in the formulation of spherical and small size microspheres. This work was a part of our ongoing thrust and project to develop microparticulate drug delivery system. PMID:19882250

  12. Preparation of regular sized Ca-alginate microspheres using membrane emulsification method.

    PubMed

    You, J O; Park, S B; Park, H Y; Haam, S; Chung, C H; Kim, W S

    2001-01-01

    Monodisperse Ca-alginate microspheres were prepared using the membrane emulsification method. Three ionic types of drugs (anionic, cationic and non-ionic) were incorporated into the microspheres, and the effects of sodium alginate concentration and the pressure applied during the dispersing process on the properties of the microspheres were examined. Monodisperse microspheres were obtained when the concentration of alginate solution was 2 wt% and the pressure applied was 0.4 x 10(5) Pa. The mean size of microspheres was approximately 4 microm. Lidocaine x HCl (cationic), sodium salicylate (anionic) and 4-acetamidophenol (non-ionic) were selected as ionic model drugs and included in the alginate microspheres. Lidocaine x HCl (cationic drug) release was more retarded than that of the anionic drug, because of the electrostatic attraction between the negative charge of the ionized carboxyl group in the alginate chain and the positive charge of the cationic drug. In acidic release medium, a slow release was observed due to the low swelling characteristic and the increased viscosity of alginate, regardless of ionic type of drug. PMID:11428680

  13. Advances in membrane emulsification. Part B: recent developments in modelling and scale-up approaches.

    PubMed

    Spyropoulos, Fotis; Lloyd, David M; Hancocks, Robin D; Pawlik, Aleksandra K

    2014-03-15

    Membrane emulsification is a promising process for formulating emulsions and particulates. It offers many advantages over conventional 'high-shear' processes with narrower size distribution products, higher batch repeatability and lower energy consumption commonly demonstrated at a small scale. Since the process was first introduced around 25 years ago, understanding of the underlying mechanisms involved during microstructure formation has advanced significantly leading to the development of modelling approaches that predict processing output; e.g. emulsion droplet size and throughput. The accuracy and ease of application of these models is important to allow for the development of design equations which can potentially facilitate scale-up of the process and meet the manufacturer's specific requirements. Part B of this review considers the advantages and disadvantages of a variety of models developed to predict droplet size, flow behaviour and other phenomena (namely droplet-droplet interactions), with presentation of the appropriate formulae where necessary. Furthermore, the advancement of the process towards an industrial scale is also highlighted with additional recommendations by the authors for future work. PMID:24122852

  14. Preparation of stable food-grade double emulsions with a hybrid premix membrane emulsification system.

    PubMed

    Eisinaite, Viktorija; Juraite, Dovile; Schroën, Karin; Leskauskaite, Daiva

    2016-09-01

    In this study we demonstrate that food-grade double emulsions can be successfully prepared using a hybrid premix emulsification system. A coarse emulsion containing beetroot juice as inner water phase, sunflower oil as oil phase and 0.5% or 1.0% whey protein isolate solution as outer water phase was prepared using a rotor stator system. This emulsion was further refined, using a bed of glass beads (diameter 71μm), through which the emulsion was pushed at different applied pressure (200-500kPa) and number of passes (1-5). All applied pressures lead to much smaller droplets while the juice remained encapsulated (>98%). The viscosity of the emulsions increased due to swelling of the internal water phase, and this implies that it is possible to encapsulate the components efficiently at relatively low internal water phase fraction at which the emulsions can be handled easily, while allowing them to obtain their final viscosity later. PMID:27041298

  15. Spontaneous emulsification of nifedipine-loaded self-nanoemulsifying drug delivery system.

    PubMed

    Weerapol, Yotsanan; Limmatvapirat, Sontaya; Kumpugdee-Vollrath, Mont; Sriamornsak, Pornsak

    2015-04-01

    Self-nanoemulsifying drug delivery system (SNEDDS) can be used to improve dissolution of poorly water-soluble drugs. The objective of this study was to prepare SNEDDS by using ternary phase diagram and investigate their spontaneous emulsifying property, dissolution of nifedipine (NDP), as well as the pharmacokinetic profile of selected SNEDDS formulation. The results showed that the composition of the SNEDDS was a great importance for the spontaneous emulsification. Based on ternary phase diagram, the region giving the SNEDDS with emulsion droplet size of less than 300 nm after diluting in aqueous medium was selected for further formulation. The small-angle X-ray scattering curves showed no sharp peak after dilution at different percentages of water, suggesting non-ordered structure. The system was found to be robust in different dilution volumes; the droplet size was in nanometer range. In vitro dissolution study showed remarkable increase in dissolution of NDP from SNEDDS formulations compared with NDP powders. The pharmacokinetic study of selected SNEDDS formulation in male Wistar rats revealed the improved maximum concentration and area under the curve. Our results proposed that the developed SNEDDS formations could be promising to improve the dissolution and oral bioavailability of NDP. PMID:25367002

  16. Highly effective emulsification/demulsification with a CO2-switchable superamphiphile.

    PubMed

    Xu, Peipei; Wang, Zengzi; Xu, Zhenghe; Hao, Jingcheng; Sun, Dejun

    2016-10-15

    This article reports a systematic study on a highly CO2-responsive superamphiphile (D-OA) in preparation of CO2-switchable oil-in-water emulsions. The D-OA was assembled with Jeffamine D 230 and oleic acid (HOA) via electrostatic interaction, which was characterized using FT-IR, (1)HNMR, surface tension, and interfacial tension techniques. The assembled gemini-like superamphiphile D-OA was shown to have a low cmc value and adsorb quickly at the paraffin oil/water interface, decreasing the interfacial tension effectively. Highly stable O/W emulsions were obtained by mixing D-OA aqueous solution and paraffin oil. After bubbling CO2 through the stable emulsions for just 20s, quick phase separation was observed; while upon removal of CO2 by bubbling N2 at 60°C, stable emulsions were recreated. The reversible assembly and disassembly of the D-OA superamphiphile by adding or removing CO2 were considered as the cause of demulsification and re-emulsification processes. The rapid and complete demulsification of the system in response to CO2 addition and removal may have potential applications in emulsion-based fabrication/separation and enhanced oil recovery processes. PMID:27442147

  17. Improved Low pH Emulsification Properties of Glycated Peanut Protein Isolate by Ultrasound Maillard Reaction.

    PubMed

    Chen, Lin; Chen, Jianshe; Wu, Kegang; Yu, Lin

    2016-07-13

    In this work, peanut protein isolate (PPI) was grafted with maltodextrin (MD) through the ultrasound-assisted Maillard reaction. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis showed a link between PPI and MD. The substantially increased accessibility of the major subunits (conarachin, acidic subunit of arachin, and basic subunit of arachin) in PPI under high-intensity ultrasound treatment led to changes in the degree of graft (DG), zeta-potential, protein solubility, and surface hydrophobicity of conjugates. Emulsion systems (20% v/v oil, 2.0% w/v PPI equivalent, pH 3.8) formed by untreated PPI, PPI-MDC (PPI-MD conjugates obtained with wet-heating alone), and UPPI-MDC (PPI-MD conjugates obtained with ultrasound-assisted wet heating) were characterized using a light-scatter particle size analyzer and confocal laser scanning microscope. Results showed that emulsions of untreated PPI and PPI-MDC were not stable due to immediate bridging flocculation and coalescence of droplets, whereas that formed by UPPI-MDC with 32.4% DG was stable with a smaller mean droplet size. It was believed that high-intensity ultrasound promoted production of glycated PPI, which was soluble and surface active at pH 3.8 and thus improved emulsification properties for UPPI-MDC. This study shows that glycated PPI by ultrasound-assisted Maillard reaction is an effective emulsifying agent for low pH applications. PMID:27329355

  18. Crocin loaded nano-emulsions: Factors affecting emulsion properties in spontaneous emulsification.

    PubMed

    Mehrnia, Mohammad-Amin; Jafari, Seid-Mahdi; Makhmal-Zadeh, Behzad S; Maghsoudlou, Yahya

    2016-03-01

    Spontaneous emulsification may be used for encapsulating bioactive compounds in food and pharmaceutical industry. It has several advantages over high energy and other low energy methods including, protecting sensitive compounds against severe conditions of high energy method and its ability to minimize surfactant, removal of cosurfactant and thermal stability compared with other low energy methods. In this study, we examined possibility of encapsulating highly soluble crocin in W/O micro-emulsions using spontaneous method which further could be used for making double emulsions. Nonionic surfactants of Span 80 and polyglycerol polyricinoleate (PGPR) were used for making micro-emulsions that showed the high potential of PGPR for spontaneous method. Surfactant to water ratio (SWR%) was evaluated to find the highest amount of aqueous phase which can be dispersed in organic phase. Droplet size decreased by increasing SWR toward the SWR=100% which had the smallest droplet size and then increased at higher levels of surfactant. By increasing SWR, shear viscosity increased which showed the high effect of PGPR on rheological properties. This study shows in addition to W/O micro-emulsions, spontaneous method could be used for preparing stable O/W micro-emulsions. PMID:26708427

  19. Nutraceutical delivery systems: resveratrol encapsulation in grape seed oil nanoemulsions formed by spontaneous emulsification.

    PubMed

    Davidov-Pardo, Gabriel; McClements, David Julian

    2015-01-15

    The aim of this work was to fabricate nanoemulsions-based delivery systems to encapsulate resveratrol. Nanoemulsions were formed using spontaneous emulsification method: 10% oil phase (grape seed oil plus orange oil) and 10% surfactant (Tween 80) were titrated into 80% aqueous phase. An optimum orange oil-to-grape seed oil ratio of 1:1(w/w) formed small droplets (d ≈ 100 nm) with good stability to droplet growth. The maximum amount of resveratrol that could be dissolved in the oil phase was 120 ± 10 μg/ml. The effect of droplet size on the chemical stability of encapsulated resveratrol was examined by preparing systems with different mean droplet diameters of 220 ± 2; 99 ± 3; and 45 ± 0.4 nm. Encapsulation of resveratrol improved its chemical stability after exposure to UV-light: 88% retention in nanoemulsions compared to 50% in dimethylsulphoxide (DMSO). This study showed that resveratrol could be encapsulated within low-energy nanoemulsion-based delivery systems and protected against degradation. PMID:25148980

  20. Effect of emulsification and spray-drying microencapsulation on the antilisterial activity of transcinnamaldehyde.

    PubMed

    Trinh, Nga-Thi-Thanh; Lejmi, Raja; Gharsallaoui, Adem; Dumas, Emilie; Degraeve, Pascal; Thanh, Mai Le; Oulahal, Nadia

    2015-01-01

    Spray-dried redispersible transcinnamaldehyde (TC)-in-water emulsions were prepared in order to preserve its antibacterial activity; 5% (w/w) TC emulsions were first obtained with a rotor-stator homogeniser in the presence of either soybean lecithin or sodium caseinate as emulsifiers. These emulsions were mixed with a 30% (w/w) maltodextrin solution before feeding a spray-dryer. The antibacterial activity of TC alone, TC emulsions with and without maltodextrin before and after spray-drying were assayed by monitoring the growth at 30 °C of Listeria innocua in their presence and in their absence (control). Whatever the emulsifier used, antilisterial activity of TC was increased following its emulsification. However, reconstituted spray-dried emulsions stabilised by sodium caseinate had a higher antibacterial activity suggesting that they better resisted to spray-drying. This was consistent with observation that microencapsulation efficiencies were 27.6% and 78.7% for emulsions stabilised by lecithin and sodium caseinate, respectively. PMID:26398167

  1. Air sampling with solid phase microextraction

    NASA Astrophysics Data System (ADS)

    Martos, Perry Anthony

    There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

  2. Production of BCG alginate-PLL microcapsules by emulsification/internal gelation.

    PubMed

    Esquisabel, A; Hernández, R M; Igartua, M; Gascón, A R; Calvo, B; Pedraz, J L

    1997-01-01

    A biocompatible emulsification method for microencapsulation of live cells and enzymes within a calcium alginate matrix applied to Bacillus Calmette-Guérin (BCG) has been developed. Small-diameter alginate beads (microcapsules) were formed via internal gelation of an alginate solution emulsified within vegetable oil. Five different oils (sesame, sweet almond, perhydrosqualene, camomile and jojoba) were used. The rheological analysis of the oils showed a Newtonian behaviour, with viscosities = 30.0, 37.7, 51.2, 59.3 and 67.1 mPa.s for perhydrosqualene, jojoba, camomile, sesame and sweet almond oil respectively. The particle size of the microcapsules obtained ranged from 30.3 microns for the microcapsules prepared with sweet almond oil to 57.0 microns for those made with perhydrosqualene. The mean particle diameter obtained was found to be dependent on the viscosity of the oil employed, according to the equation: phi (micron) = 76.6-0.628 eta (mPa.s) (r2 = 0.943). The encapsulated BCG was identified by the Difco TB stain set K, followed by observation under optical microscopy. Freeze-drying of the microcapsules was carried out to ensure their stability during storage. Two batches of microcapsules (those prepared with sesame and jojoba oil) and four types of cryoprotectors (glucose, trehalose, mannitol and sorbitol), at three concentration levels (5, 10 and 20% w/v) were studied. The parameters evaluated were particle size, physical appearance, reconstitution of lyophilizates and microscopical evaluation. For both batches of microcapsules the best results were obtained with trehalose 5%, showing particle sizes of 42.1 microns in the case of the microcapsules prepared with sesame oil, and of 45.3 microns for those prepared with jojoba. PMID:9292438

  3. Preparation and characterization of solid lipid nanoparticles containing cyclosporine by the emulsification-diffusion method

    PubMed Central

    Urbán-Morlán, Zaida; Ganem-Rondero, Adriana; Melgoza-Contreras, Luz María; Escobar-Chávez, José Juan; Nava-Arzaluz, María Guadalupe; Quintanar-Guerrero, David

    2010-01-01

    Solid lipid nanoparticles (SLNs) have been used for carrying different therapeutic agents because they improve absorption and bioavailability. The aim of the study was to prepare lipidic nanoparticles containing cyclosporine (CyA) by the emulsification-diffusion method and to study their physicochemical stability. Glyceryl behenate (Compritol® ATO 888) and lauroyl macrogolglycerides (Gelucire® 44/14) were used as carrier materials. Nanoparticles with good stability were obtained with Gelucire®, while it was difficult to obtain stable systems with Compritol®. Systems with Gelucire® were characterized by particle size, Z-potential, differential scanning calorimetry (DSC), scanning electron microscopy (SEM), entrapment efficiency and in vitro release. Particle size and Z-potential were evaluated for at least three months. With a high CyA content (≥60 mg) in Gelucire® SLNs, variations in size were greater and particle size also increased over time in all batches; this effect may have been caused by a probable expulsion of the drug due to the lipid’s partial rearrangement. While the Z-potential decreased 10 mV after three months, this effect may be explained by the superficial properties of the drug that make the molecules to be preferably oriented at the solid-liquid interface, causing a change in the net charge of the particle. SEM confirmed size and shape of the nanoparticles. DSC studies evidenced that CyA affects the lipid structure by a mechanism still unknown. The entrapment efficiency was higher than 92%, and CyA release from SLNs was relatively fast (99.60% in 45 min). PMID:20856836

  4. SURFACTANT ENHANCED PHOTO-OXIDATION OF WASTEWATERS

    EPA Science Inventory

    Initial research projects using the nonionic surfactant Brij-35 established that this surfactant could successfully adsolublize aromatic organic pollutants such as anthracene, naphthalene, benzoic acid, chlorophenol, and benzene onto the surface of TiO2 par...

  5. Effect of ultrasound radiation duration on emulsification and demulsification of paraffin oil and surfactant solution/brine using Hele-shaw models.

    PubMed

    Hamidi, Hossein; Mohammadian, Erfan; Asadullah, Mohammad; Azdarpour, Amin; Rafati, Roozbeh

    2015-09-01

    Ultrasound technique is one of the unconventional enhanced oil recovery methods which has been of interest for more than six decades. However, the majority of the oil recovery mechanisms under ultrasound reported in the previous studies are theoretical. Emulsification is one of the mechanisms happening at the interface of oil and water in porous media under ultrasound. Oppositely, ultrasound is one of the techniques using in oil industry for demulsification of oil/water emulsion. Therefore, the conditions in which emulsification becomes dominant over demulsification under ultrasound should be more investigated. Duration of ultrasound radiation could be one of the factors affecting emulsification and demulsification processes. In this study a technique was developed to investigate the effect of long and short period of ultrasound radiation on emulsification and demulsification of paraffin oil and surfactant solution in porous media. For this purpose, the 2D glass Hele-shaw models were placed inside the ultrasonic bath under long and short period of radiation of ultrasound. A microscope was used above the model for microscopic studies on the interface of oil and water. Diffusion of phases and formation of emulsion were observed in both long and short period of application of ultrasound at the beginning of ultrasound radiation. However, by passing time, demulsification and coalescence of brine droplets inside emulsion was initiated in long period of ultrasound application. Therefore, it was concluded that emulsification could be one of the significant oil recovery mechanisms happening in porous media under short period of application of ultrasound. PMID:25616638

  6. Analysis of biosurfactants from industrially viable Pseudomonas strain isolated from crude oil suggests how rhamnolipids congeners affect emulsification property and antimicrobial activity

    PubMed Central

    Das, Palashpriya; Yang, Xin-Ping; Ma, Luyan Z.

    2014-01-01

    Rhamnolipid biosurfactants produced mainly by Pseudomonas sp. had been reported to possess a wide range of potential industrial application. These biosurfactants are produced as monorhamnolipid (MRL) and di-rhamnolipid (DRL) congeners. The present study deals with rhamnolipid biosurfactants produced by three bacterial isolates from crude oil. Biosurfactants produced by one of the strains (named as IMP67) was found to be very efficacious based on its critical micelle concentration value and hydrocarbon emulsification property. Strikingly, antimicrobial, and anti-biofilm potential of this biosurfactant were higher than biosurfactants produced by other two strains. Thin layer chromatography analysis and rhamnose quantification showed that the rhamnolipids of IMP67 had more MRL congeners than biosurfactants of the other two strains. Emulsification and antimicrobial actions were affected by manual change of MRL and DRL congener proportions. Increase of MRL proportion enhanced emulsification index and antimicrobial property to Gram negative bacteria. This result indicated that the ratio of MRL and DRL affected the emulsification potentials of rhamnolipids, and suggested that high emulsification potentials might enhance rhamnolipids to penetrate the cell wall of Gram negative bacteria. In line with this finding, rhamnolipids of IMP67 also reduced the MIC of some antibiotics against bacteria, suggesting their synergistic role with the antibiotics. PMID:25566212

  7. Solid Phase Microextraction for the Analysis of Nuclear Weapons

    SciTech Connect

    Chambers, D M

    2001-06-01

    This document is a compendium of answers to commonly asked questions about solid phase microextraction as it relates to the analysis of nuclear weapons. We have also included a glossary of terms associated with this analytical method as well as pertinent weapons engineering terminology. Microextraction is a new collection technique being developed to nonintrusively sample chemicals from weapon headspace gases for subsequent analysis. The chemicals that are being targeted outgas from the high explosives and other organic materials used in the weapon assembly. This technique is therefore a valuable tool to: (1) remotely detect and assess the aging of Lawrence Livermore National Laboratory (LLNL) and, in some cases, Sandia National Laboratory (SNL) organic materials; and (2) identify potential compatibility issues (i.e., materials interactions) that should be more carefully monitored during surveillance tear-downs. Microextraction is particularly attractive because of the practical constraints inherent to the weapon surveillance procedure. To remain transparent to other core surveillance activities and fall within nuclear safety guidelines, headspace analysis of the weapons requires a procedure that: (1) maintains ambient temperature conditions; (2) allows practical collection times of less than 20 min; (3) maintains the integrity of the weapon gas volume; (4) provides reproducible and quantitative results; and (5) can identify all possible targets.

  8. Conformational stability of a model protein (bovine serum albumin) during primary emulsification process of PLGA microspheres synthesis.

    PubMed

    Kang, Feirong; Singh, Jagdish

    2003-07-01

    The goal of this study was to investigate the conformational stability of a model protein, bovine serum albumin (BSA), during the primary emulsification process of poly(D,L-lactide-co-glycolide) (PLGA) microspheres preparation. Differential scanning calorimeter (DSC) was utilized to assess the conformational structure of BSA during primary emulsification in the presence and absence of PLGA. Three excipients [i.e. mannitol, hydroxypropyl-beta-cyclodextrin (HP-beta-CD) and sodium dodecyl sulfate (SDS)] were investigated for their stabilizing effect on BSA during emulsification process. The DSC profile of intact BSA was best fitted by a non-2-state model with two peaks, which have midpoint temperatures (T(m1), 60.9 +/- 0.4 degrees C and T(m2), 66.4 +/- 1.0 degrees C), respectively, and a total calorimetric enthalpy Delta H(tot) of 599 +/- 42 kJ/mol. After emulsifying BSA aqueous solution with methylene chloride, an additional apparent peak at a higher temperature was observed. The T(m) of this peak was 77.4 +/- 0.8 degrees C. HP-beta-CD was able to suppress the occurrence of an additional peak, whereas mannitol failed. SDS increased the thermal stability of BSA dramatically. Furthermore, HP-beta-CD increased BSA recovery from 72 +/- 8% to 89 +/- 7% after extraction from w/o in the presence of PLGA. These results provided evidence that HP-beta-CD could be a promising excipient for conformational stability of BSA during synthesis of PLGA microspheres. PMID:12818819

  9. Microchannel arrays with improved accessibility and use for cell studies and emulsification

    NASA Astrophysics Data System (ADS)

    Kikuchi, Yuji; Kikuchi, Hiroko E.; Kuboki, Yoshinori; Nakajima, Mitsutoshi

    2000-03-01

    Arrays of microgrooves (groove width; 2, 3, 4, 5, 6, 7, 8, 10, 12, and 14 micrometer, groove interval; width x3, x10, and x20, one size and interval per chip) each connecting a center well and a side edge of a silicon substrate were created by photolithography and anisotropic wet etching. A penetrating hole was made by sand blast at the substrate center for the access to the center well. By tightly covering the substrate surface with a glass plate, the microgroove arrays were converted to microchannel arrays having one ends open at the side edges of the substrate. These microchannel arrays were used for cell trapping for microinjection and also used for emulsification. Poplar (Populus alba) protoplasts were used for the test of cell trapping. Cells showed a very large variation in size and irregularity in shape, and, furthermore, the protoplast preparation contained a number of cell membrane fragments and chloroplasts. Despite the cell size and shape variations and obstruction by the admixtures, many cells could be trapped by aspiration at the channel ends because of their openness to the outside free space and also their large multiplicity in parallel. The free space outside the side of the substrate allowed a free manipulation of a glass micropipette under microscopic observation using transmitted illumination. The microscopic observation direction nearly perpendicular to the movement directions of the micropipette further allowed the movement of the pipette tip nearly always in focus. These led to an easy pointing and puncturing. In addition, the cell trapping points in a line made successive approach to adjacent cells easier. Soybean oil containing 1.5 wt% polyoxyethylene(20)sorbitan monoolete as a surfactant was forced to flow into physiological saline filling the outside of the substrate through the microchannels. Regularly sized oil particles were created by this process with a variation coefficient (S.D./mean) 16% of their diameter. This variation, which is

  10. Microchannel emulsification study on formulation and stability characterization of monodisperse oil-in-water emulsions encapsulating quercetin.

    PubMed

    Khalid, Nauman; Kobayashi, Isao; Neves, Marcos A; Uemura, Kunihiko; Nakajima, Mitsutoshi; Nabetani, Hiroshi

    2016-12-01

    The study used microchannel emulsification (MCE) to encapsulate quercetin in food grade oil-in-water (O/W) emulsions. A silicon microchannel plate (Model WMS 1-2) comprised of 10,300 discrete 10×104μm microslots was connected to a circular microhole with an inner diameter of 10μm. 1% (w/w) Tween 20 was used as optimized emulsifier in Milli-Q water, while 0.4mgml(-1) quercetin in different oils served as a dispersed phase. The MCE was carried by injecting the dispersed phase at 2mlh(-1). Successful emulsification was conducted below the critical dispersed phase flux, with a Sauter mean diameter of 29μm and relative span factor below 0.25. The O/W emulsions remained stable in terms of droplet coalescence at 4 and 25°C for 30days. The encapsulation efficiency of quercetin in the O/W emulsions was 80% at 4°C and 70% at 25°C during the evaluated storage period. PMID:27374502

  11. Preparation and characterization of paclitaxel nanosuspension using novel emulsification method by combining high speed homogenizer and high pressure homogenization.

    PubMed

    Li, Yong; Zhao, Xiuhua; Zu, Yuangang; Zhang, Yin

    2015-07-25

    The aim of this study was to develop an alternative, more bio-available, better tolerated paclitaxel nanosuspension (PTXNS) for intravenous injection in comparison with commercially available Taxol(®) formulation. In this study, PTXNS was prepared by emulsification method through combination of high speed homogenizer and high pressure homogenization, followed by lyophilization process for intravenous administration. The main production parameters including volume ratio of organic phase in water and organic phase (Vo:Vw+o), concentration of PTX, content of PTX and emulsification time (Et), homogenization pressure (HP) and passes (Ps) for high pressure homogenization were optimized and their effects on mean particle size (MPS) and particle size distribution (PSD) of PTXNS were investigated. The characteristics of PTXNS, such as, surface morphology, physical status of paclitaxel (PTX) in PTXNS, redispersibility of PTXNS in purified water, in vitro dissolution study and bioavailability in vivo were all investigated. The PTXNS obtained under optimum conditions had an MPS of 186.8 nm and a zeta potential (ZP) of -6.87 mV. The PTX content in PTXNS was approximately 3.42%. Moreover, the residual amount of chloroform was lower than the International Conference on Harmonization limit (60 ppm) for solvents. The dissolution study indicated PTXNS had merits including effect to fast at the side of raw PTX and sustained-dissolution character compared with Taxol(®) formulation. Moreover, the bioavailability of PTXNS increased 14.38 and 3.51 times respectively compared with raw PTX and Taxol(®) formulation. PMID:26027492

  12. Microextraction techniques for the determination of volatile and semivolatile organic compounds from plants: a review.

    PubMed

    Yang, Cui; Wang, Juan; Li, Donghao

    2013-10-17

    Vegetables and fruits are necessary for human health, and traditional Chinese medicine that uses plant materials can cure diseases. Thus, understanding the composition of plant matrix has gained increased attention in recent years. Since plant matrix is very complex, the extraction, separation and quantitation of these chemicals are challenging. In this review we focus on the microextraction techniques used in the determination of volatile and semivolatile organic compounds (such as esters, alcohols, aldehydes, hydrocarbons, ketones, terpenes, sesquiterpene, phenols, acids, plant secondary metabolites and pesticides) from plants (e.g., fruits, vegetables, medicinal plants, tree leaves, etc.). These microextraction techniques include: solid phase microextraction (SPME), stir-bar sorptive extraction (SBSE), single drop microextraction (SDME), hollow fiber liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME), and gas purge microsyringe extraction (GP-MSE). We have taken into consideration papers published from 2008 to the end of January 2013, and provided critical and interpretative review on these techniques, and formulated future trends in microextraction for the determination of volatile and semivolatile compounds from plants. PMID:24091369

  13. Determination of steroid hormones in biological and environmental samples using green microextraction techniques: an overview.

    PubMed

    Aufartová, Jana; Mahugo-Santana, Cristina; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan; Nováková, Lucie; Solich, Petr

    2011-10-17

    Residues of steroid hormones have become a cause for concern because they can affect the biological activity of non-target organisms. Steroid hormones are a potential risk for wildlife and humans through the consumption of contaminated food or water. Their determination requires extraction and clean-up steps, prior to detection, to reach low concentration levels. In recent years, a great effort has been made to develop new analytical methodologies, such as microextraction techniques, that reduce environmental pollution. Researchers have modified old methods to incorporate procedures that use less-hazardous chemicals or that use smaller amounts of them. They are able to do direct analysis using miniaturised equipment and reduced amounts of solvents and wastes. These accomplishments are the main objectives of green analytical chemistry. In this overview, we focus on microextraction techniques for the determination of steroid hormones in biological (e.g., human urine, human serum, fish, shrimp and prawn tissue and milk) and environmental (e.g., wastewaters, surface waters, tap waters, river waters, sewage sludges, marine sediments and river sediments) samples. We comment on the most recent applications in sorptive-microextraction modes, such as solid phase microextraction (SPME) with molecularly imprinted polymers (MIPs), in-tube solid-phase microextraction (IT-SPME), stir-bar sorptive extraction (SBSE) and microextraction in packed sorbent (MEPS). We also describe liquid-phase microextraction (LPME) approaches reported in the literature that are applied to the determination of steroid hormones. PMID:21907019

  14. Multi-residue method for determination of 58 pesticides, pharmaceuticals and personal care products in water using solvent demulsification dispersive liquid-liquid microextraction combined with liquid chromatography-tandem mass spectrometry.

    PubMed

    Caldas, Sergiane Souza; Rombaldi, Caroline; Arias, Jean Lucas de Oliveira; Marube, Liziane Cardoso; Primel, Ednei Gilberto

    2016-01-01

    A rapid and efficient sample pretreatment using solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was studied for the extraction of 58 pharmaceuticals and personal care products (PPCPs) and pesticides from water samples. Type and volume of extraction and disperser solvents, pH, salt addition, amount of salt and type of demulsification solvent were evaluated. Limits of quantification (LOQ) in the range from 0.0125 to 1.25 µg L(-1) were reached, and linearity was in the range from the LOQ of each compound to 25 μg L(-1). Recoveries ranged from 60% to 120% for 84% of the compounds, with relative standard deviations lower than 29%. The proposed method demonstrated, for the first time, that sample preparation by SD-DLLME with determination by LC-MS/MS can be successfully used for the simultaneous extraction of 32 pesticides and 26 PPCPs from water samples. The entire procedure, including the extraction of 58 organic compounds from the aqueous sample solution and the breaking up of the emulsion after extraction with water, rather than with an organic solvent, was environmentally friendly. In addition, this technique was less expensive and faster than traditional techniques. Finally, the analytical method under study was successfully applied to the analysis of all 58 pesticides and PPCPs in surface water samples. PMID:26695317

  15. Progress of solid-phase microextraction coatings and coating techniques.

    PubMed

    Jiang, Guibin; Huang, Minjia; Cai, Yaqi; Lv, Jianxia; Zhao, Zongshan

    2006-07-01

    Solid-phase microextraction (SPME) has been popular as an environmentally friendly sample pretreatment technique to extract a very wide range of analytes. This is partly owing to the development of SPME coatings. One of the key factors affecting the extraction performances, such as the sensitivity, selectivity, and reproducibility, is the properties of the coatings on SPME fibers. This paper classifies the materials used as SPME coatings and introduces some common preparation techniques of SPME coating in detail, such as sol-gel technique, electrochemical polymerization technique, particle direct pasting technique, restricted access matrix SPME technique, and molecularly imprinted SPME technique. PMID:16884587

  16. Evaluation of microextraction/capillary column gas chromatography for monitoring industrial outfalls

    SciTech Connect

    Thielen, D.R.; Olsen, G.; Davis, A.; Bajor, E.; Stefanovski, J.; Chodkowski, J.

    1987-01-01

    Microextraction and capillary-column gas chromatography techniques are applied to plant discharge streams for repetitive wastewater discharge permit analyses. This combination allows the analyst to reduce sample preparation since microextraction replaces both purge-and-trap for volatiles and microextraction for semi-volatiles. An additional advantage is the elimination of a concentration step, which is ,ften a major contributor to low method recoveries. The overall procedure is shown to be more precise than purge-and-trap but slightly less precise than conventional extraction. The results of each method are shown to be equivalent.

  17. Effect of emulsification-diffusion parameters on the formation of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) particles.

    PubMed

    Göz, Eda; Karakeçili, Ayşe

    2016-01-01

    The aim of this work was to evaluate the effect of various production parameters on the formation and particle size of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) PHBV particles prepared by the emulsification-diffusion technique. The increase in homogenization time and speed caused a decrease in particle size. No particle formation was observed below 2% (w/v) PHBV in the organic phase. Smaller particle size and narrower size distribution were observed when polyvinyl alcohol (PVA) was used as a stabilizer, when compared to didodecyldimethylammonium bromide. Submicron particles of 531 ± 150 nm size were obtained with 2% (w/v) PVA at 17 500 rpm and 15 min homogenization conditions with dichloromethane as the organic solvent. PMID:25058033

  18. [Preparation and characterization of tetrandrine-loaded PLGA nanocomposite particles by premix membrane emulsification coupled with spray-drying method].

    PubMed

    Hu, Tao; Zhu, Hua-Xu; Guo, Li-Wei; Pan, Lin-Mei; Li, Bo; Shi, Fei-Yan; Lu, Jin

    2014-11-01

    For effective inhalable dry-powder drug delivery, tetrandrine-PLGA (polylactic-co-glycolic acid) nanocomposite particles have been developed to overcome the disadvantages of nanoparticles and microparticles. The primary nanoparticles were prepared by using premix membrane emulsification method. To prepare second particles, they were spray dried. The final particles were characterized by scanning electron microscopy (SEM), dry laser particle size analysis, high performance liquid chromatography (HPLC), X-ray diffraction (XRD), differential scanning calorimetry (DSC), infrared analysis (IR) and confocal laser scanning microscope (CLSM). The average size of the primary particles was (337.5 ± 6.2) nm, while that second particles was (3.675 ± 0.16) μm which can be decomposed into primary nanoparticles in water. And the second particles were solid sphere-like with the drug dispersed as armorphous form in them. It is a reference for components delivery to lung in a new form. PMID:25757290

  19. Development of a novel environmentally friendly electropolymerization of water-insoluble monomers in aqueous electrolytes using acoustic emulsification.

    PubMed

    Asami, Ryosuke; Fuchigami, Toshio; Atobe, Mahito

    2006-11-21

    Electropolymerization of water-insoluble monomers, such as 3,4-ethylenedioxythiophene (EDOT), 3,4-dimethylthiophene (3,4-DiMeTh), 3-methylthiophene (3-MeTh), and 3-ethylthiophene (3-EtTh), proceeded successfully in aqueous electrolytes using acoustic emulsification. Ultrasonication to the water-insoluble monomer/aqueous electrolyte mixtures allowed the formation of very stable emulsions having the characteristic of giving narrow monomer droplet size distributions in the submicrometer range in aqueous electrolytes without added surfactants, and the smooth electropolymerization in the emulsions took place via direct electron transfer between the electrode and the water-insoluble monomer droplets. In this kind of electron-transfer system, the supporting electrolyte should be dissolved not only in the aqueous phase but also in the monomer droplets and contribute to the formation of an electric bilayer inside the droplets. The properties of a polymer EDOT film obtained by the present method were also investigated. PMID:17107030

  20. Preparation of Multifunctional Liposomes as a Stable Vaccine Delivery-Adjuvant System by Procedure of Emulsification-Lyophilization.

    PubMed

    Wang, Ning; Wang, Ting

    2016-01-01

    Liposomes have been proven to be useful carriers for vaccine antigens and can be modified as a versatile vaccine adjuvant-delivery system (VADS). To fulfill efficiently both functions of adjuvant and delivery, the liposomes are often modified with different functional molecules, such as lipoidal immunopotentiators, APC (antigen-presenting cell) targeting ligands, steric stabilization polymers, and charged lipids. Also, to overcome the weakness of instability, vaccines are often lyophilized as a dry product. In this chapter the procedure of emulsification-lyophilization (PEL) is introduced as an efficient method for preparing a stable anhydrous precursor to the multifunctional liposomes which bear dual modifications with APC targeting molecule of the mannosylated cholesterol and the adjuvant material of monophosphoryl lipid A. The techniques and procedures for synthesis of APC targeting molecule, i.e., the mannosylated cholesterol, and for characterization of the multifunctional liposomes are also described. PMID:27076327

  1. Preparation of uniform sized chitosan microspheres by membrane emulsification technique and application as a carrier of protein drug.

    PubMed

    Wang, Lian-Yan; Ma, Guang-Hui; Su, Zhi-Guo

    2005-08-18

    The control of size and size distribution of microspheres is necessary for obtaining repeatable controlled release behavior. The chitosan microspheres were prepared by a membrane emulsification technique in this study. Chitosan was dissolved in 1 wt.% aqueous acetic acid containing 0.9 wt.% sodium chloride, which was used as a water phase. A mixture of liquid paraffin and petroleum ether 7:5 (v/v) containing PO-500 emulsifier was used as an oil phase. The water phase was permeated through the uniform pores of a porous glass membrane into the oil phase by the pressure of nitrogen gas to form W/O emulsion. Then GST (Glutaraldehyde Saturated Toluene) as crosslinking agent was slowly dropped into the W/O emulsion to solidify the chitosan droplets. The preparation condition for obtaining uniform-sized microspheres was optimized. The microspheres with different size were prepared by using the membranes with different pore size, and there was a linear relationship between the diameter of microspheres and pore size of the membranes when the microspheres were in the range of micron size. The smallest chitosan microspheres obtained was 0.4 mum in diameter. This is the first report for preparing the uniform-sized chitosan microspheres by membrane emulsification technique. Uniform chitosan microspheres were further used as a carrier of protein drug. Bovine serum albumin (BSA) as a model drug was loaded in the microspheres and released in vitro. The effects of pH value, diameter and crosslinking degree of microspheres, and BSA concentration on loading efficiency and release behavior were discussed. PMID:15922472

  2. Preparation of insulin-loaded PLA/PLGA microcapsules by a novel membrane emulsification method and its release in vitro.

    PubMed

    Liu, Rong; Huang, Shan-Shan; Wan, Yin-Hua; Ma, Guang-Hui; Su, Zhi-Guo

    2006-08-01

    Uniform-sized biodegradable PLA/PLGA microcapsules loading recombinant human insulin (rhI) were successfully prepared by combining a Shirasu Porous Glass (SPG) membrane emulsification technique and a double emulsion-evaporation method. An aqueous phase containing rhI was used as the inner water phase (w1), and PLA/PLGA and Arlacel 83 were dissolved in a mixture solvent of dichloromethane (DCM) and toluene, which was used as the oil phase (o). These two solutions were emulsified by a homogenizer to form a w1/o primary emulsion. The primary emulsion was permeated through the uniform pores of a SPG membrane into an outer water phase by the pressure of nitrogen gas to form the uniform w1/o/w2 droplets. The solid polymer microcapsules were obtained by simply evaporating solvent from droplets. Various factors of the preparation process influencing the drug encapsulation efficiency and the drug cumulative release were investigated systemically. The results indicated that the drug encapsulation efficiency and the cumulative release were affected by the PLA/PLGA ratio, NaCl concentration in outer water phase, the inner water phase volume, rhI-loading amount, pH-value in outer water phase and the size of microcapsules. By optimizing the preparation process, the drug encapsulation efficiency was high up to 91.82%. The unique advantage of preparing drug-loaded microcapsules by membrane emulsification technique is that the size of microcapsules can be controlled accurately, and thus the drug cumulative release profile can be adjusted just by changing the size of microcapsules. Moreover, much higher encapsulation efficiency can be obtained when compared with the conventional mechanical stirring method. PMID:16814994

  3. Applications of liquid-phase microextraction techniques in natural product analysis: a review.

    PubMed

    Yan, Yunyan; Chen, Xuan; Hu, Shuang; Bai, Xiaohong

    2014-11-14

    Over the last years, liquid-phase microextraction (LPME) as a simple, rapid, practical and effective sample-preparation technique, coupled with various instrumental analytical methods, has been increasingly and widely used to research and determine trace or ultra-micro-levels of both inorganic and organic analytes from different matrix-complex samples. In this review, different kinds of LPMEs such as single drop liquid-phase microextraction, dispersive liquid-liquid microextraction, and hollow fibre liquid-phase microextraction are summarized and recent applications of LPMEs in trace compounds in vivo and in vitro from different natural product matrice analysis such as tea, vegetables, seeds, herbs, and galenical are also discussed. Finally, future developments and applications of LPMEs in complex sample analysis are prospected. PMID:25441339

  4. EVALUATION OF SOLID PHASE MICROEXTRACTION FOR THE ANALYSIS OF HYDROPHILIC COMPOUNDS

    EPA Science Inventory

    Two commercially available solid phase microextractions (SPME) fibers, polyacrylate and carboxem/polydimethylsiloxane (PDMS), were evaluated for their ability to extract hydrophilic compounds from drinking water. Conditions, such as desorption time, desorption temperature, sample...

  5. Solid Phase Microextraction (SPME) Fibers for Preconcentration of Organics in Titan's Lakes

    NASA Astrophysics Data System (ADS)

    Hodyss, R.; Beauchamp, P. M.

    2012-10-01

    Solid phase microextraction (SPME) fibers are a simple and reliable means for extracting and concentrating organic trace species from liquid hydrocarbon solutions, making them an attractive approach for chemical analysis of Titan's lakes.

  6. Emerging Environmental Contaminants and Soled Phase Microextraction: Janusz Pawliszyn's Legacy in the Environmental Arena

    EPA Science Inventory

    Solid phase microextraction (SPME) has revolutionized the way samples are extracted, enabling rapid, automated, and solventless extraction of many different sample types, including air, water, soil, and biological samples. As such, SPME is widely used for environmental, food, fo...

  7. Solid phase microextraction analysis of B83 SLTS and Core B compatibility test units

    SciTech Connect

    Chambers, D M; Ithaca, J; King, H A; Malcolm, S

    1999-03-26

    Solid phase microextraction has permitted the efficient collection and analysis of a broad range of volatile and semivolatile compounds outgassed from materials. In 1998, we implemented a microextraction protocol at Mason and Hanger, Pantex Plant, for the analysis of weapons and compatibility test units. The chemical information that was obtained from this work is interpreted by determining the source and outgas mechanism for each compound in the weapon signature, which is a task only accomplished by analysis of material standards.

  8. Microextraction by Packed Sorbent (MEPS) and Solid-Phase Microextraction (SPME) as Sample Preparation Procedures for the Metabolomic Profiling of Urine

    PubMed Central

    Silva, Catarina; Cavaco, Carina; Perestrelo, Rosa; Pereira, Jorge; Câmara, José S.

    2014-01-01

    For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS) and solid-phase microextraction (SPME), completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones. PMID:24958388

  9. Method for preparing a solid phase microextraction device using aerogel

    DOEpatents

    Miller, Fred S.; Andresen, Brian D.

    2006-10-24

    A sample collection substrate of aerogel and/or xerogel materials bound to a support structure is used as a solid phase microextraction (SPME) device. The xerogels and aerogels may be organic or inorganic and doped with metals or other compounds to target specific chemical analytes. The support structure is typically formed of a glass fiber or a metal wire (stainless steel or kovar). The devices are made by applying gel solution to the support structures and drying the solution to form aerogel or xerogel. Aerogel particles may be attached to the wet layer before drying to increase sample collection surface area. These devices are robust, stable in fields of high radiation, and highly effective at collecting gas and liquid samples while maintaining superior mechanical and thermal stability during routine use. Aerogel SPME devices are advantageous for use in GC/MS analyses due to their lack of interfering background and tolerance of GC thermal cycling.

  10. COHORT SAFETY AND EFFICACY STUDY OF SILURON2000 EMULSIFICATION-RESISTANT SILICONE OIL AND F4H5 IN THE TREATMENT OF FULL-THICKNESS MACULAR HOLE

    PubMed Central

    Pinxten, Anne-Marie; Wong, David S.

    2015-01-01

    Purpose: To evaluate safety and efficacy of using Siluron2000 silicone oil in the treatment of full-thickness macular hole by comparing its propensity to emulsify with emulsification of the “gold standard” Siluron5000, and to assess safety and efficacy of F4H5 (perfluorobutylpentane) in removing emulsified oil droplets from the eye. Methods: A single-center, randomized controlled parallel group trial in 72 patients undergoing vitrectomy for treatment of full-thickness macular hole. The study comprises four treatment groups. First, the total patient group was divided into 2 study arms of 36 patients each, receiving either Siluron2000 or Siluron5000 after vitrectomy with a 3-month follow-up after vitrectomy. Second, F4H5 was used during oil removal in half of the patients in each study arm (18 patients within each study arm) with follow-up at 6 weeks after oil removal. Oil droplets were counted within the removed oil; residual emulsification bubbles were quantified using ultrasound imaging. Results: Safety and efficacy of the oils were comparable. Injection and removal time of Siluron2000 oil was significantly less than that of Siluron5000 oil. Patients treated with F4H5 had borderline significantly less emulsification droplets than those not treated with F4H5. Conclusion: Siluron2000 silicone oil seems to be equally safe and effective as Siluron5000 oil but allows for better handling with the potential of reducing procedure time. The application of F4H5 seems to be safe and effective in reducing residual emulsification. PMID:26066703

  11. Evaluation of protein structural changes and water mobility in chicken liver paste batters prepared with plant oil substituting pork back-fat combined with pre-emulsification.

    PubMed

    Xiong, Guoyuan; Han, Minyi; Kang, Zhuangli; Zhao, Yingying; Xu, Xinglian; Zhu, Yingying

    2016-04-01

    Protein structural changes and water mobility properties in chicken liver paste batters prepared with plant oil (sunflower and canola oil combinations) substituting 0-40% pork back-fat combined with pre-emulsification were studied by Raman spectroscopy and low-field nuclear magnetic resonance (NMR). Results showed that pre-emulsifying back-fat and plant oil, including substituting higher than 20% back-fat with plant oil increased the water- and fat-binding (p<0.05) properties, formed more even and fine microstructures, and gradually decreased the NMR relaxation times (T21a, T21b and T22), which was related to the lower fluid losses in chicken liver paste batters. Raman spectroscopy revealed that compared with a control, there was a decrease (p<0.05) in α-helix content accompanied by an increase (p<0.05) in β-sheet structure when substituting 20-40% back-fat with plant oil combined with pre-emulsification. Pre-emulsification and plant oil substitution changed tryptophan and tyrosine doublet hydrophobic residues in chicken liver paste batters. PMID:26593506

  12. Preparation and evaluation of water-in-soybean oil-in-water emulsions by repeated premix membrane emulsification method using cellulose acetate membrane.

    PubMed

    Muhamad, Ida Idayu; Quin, Chang Hui; Selvakumaran, Suguna

    2016-04-01

    The purpose of this study was to investigate the preparation of formulated water- in-soybean oil-in-water emulsions by repeated premix membrane emulsification method using a cellulose acetate membrane. The effect of selective membrane emulsification process parameters (concentration of the emulsifiers, number of passes of the emulsions through the membrane and storage temperature) on the properties and stability of the developed emulsions were also investigated. 1, 3, 6, 8-pyrenetetrasulfonic acid tetrasodium salt (PTSA) was used as a hydrophilic model ingredient for the encapsulation of bioactive substances. W/O emulsions with 7 wt% (weight percentage) PGPR displays homogeneous and very fine dispersions, with the median diameter at 0.640 μm. Meanwhile, emulsions prepared by membrane emulsification (fine W/O/W) showed the highest stability at Tween 80 concentrations of 0.5 wt.% (weight percentage). It concluded that at 7 wt.% (weight percentage) PGPR concentration and 0.5 wt.% (weight percentage) Tween 80 concentrations, the most uniform particles with minimum mean size of oil drops (9.926 μm) were obtained after four passes through the membrane. Thus, cellulose acetate membrane can be used for preparing a stable W/O/W emulsions by repeated premix ME due to low cost and relatively easy to handle. PMID:27413211

  13. Determination of fluoroquinolone antibiotics via ionic-liquid-based, salt-induced, dual microextraction in swine feed.

    PubMed

    Wang, Huili; Gao, Ming; Gao, Jiajia; Yu, Nana; Huang, Hong; Yu, Qing; Wang, Xuedong

    2016-09-01

    In conventional microextraction procedures, the disperser (organic solvent or ionic liquid) is left in the aqueous phase and discarded after finishing the microextraction process. Because the disperser is water-soluble, it results in low extraction recovery for polar compounds. In this investigation, an ionic-liquid-based microextraction (ILBME) was integrated with salting-out assisted liquid-liquid microextraction (SALLME) to build an ionic-liquid-based, salt-induced, dual microextraction (ILSDME) for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P, -1.0 to 1.0). The proposed ILSDME method incorporates a dual microextraction by converting the disperser in the ILBME to the extractor in the SALLME. Optimization of key factors was conducted by integrating single-factor experiments and central composite design. The optimized experimental parameters were 80 μL [C8MIM][PF6] as extractor, 505 μL acetone as disperser, pH = 2.0, 4.1 min extraction time, and 4.2 g of Na2SO4. Under optimized conditions, high ERs (90.6-103.2 %) and low LODs (0.07-0.61 μg kg(-1)) were determined for five FQs in swine feed. Experimental precision based on RSDs was 1.4-5.2 % for intra-day and 2.4-6.9 % for inter-day analyses. The combination of ILBME with SALLME increased FQ recoveries by 15-20 % as compared with SALLME, demonstrating that the ILSDME method can enhance extraction efficiency for polar compounds compared to single-step microextraction. Therefore, the ILSDME method developed in this study has wide application for pretreatment of moderately to highly polar pollutants in complex matrices. Graphical Abstract A dual microextraction was developed by integrating ionic-liquid-based microextraction with salting-out assisted liquid-liquid microextraction for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P = -1.0 to 1.0). The principle of dual microextraction is based on converting the remaining disperser from

  14. Emulsification and size control of insulating and/or viscous liquids in liquid-liquid systems by electrostatic dispersion

    SciTech Connect

    Sato, M.; Saito, M.; Hatori, T. )

    1993-03-15

    Electrostatic atomization has been utilized in applications such as electrostatic printing, paint spraying, thin-film coating, production of ultrafine powders, and control of fuel spraying. Electrostatic emulsification of insulating and/or viscous liquids which have been impossible to disperse by ordinary methods was studied using a liquid/distilled-water system. A dc potential was applied to a capillary nozzle to produce droplets. The size of the droplets decreased with increasing potential. The mean droplet diameter (corresponding to the applied potential) could be varied over a wide range (from several mm to [mu]m). A very fine cloudy emulsion (mean diameter of c.a. 5 [mu]m) having a narrow size distribution was obtained by applying approximately -3500 V to the nozzle. In the case of liquids with low viscosity, i.e., kerosene and carbon tetrachloride, droplets were produced regularly from the cusp of the meniscus formed at the nozzle tip. On the other hand, for castor oil, a highly viscous liquid, a liquid thread was drawn out from the meniscus and then disintegrated into small droplets. The mean diameter of the caster oil droplets was larger (one order of magnitude) than that of the low viscosity kerosene at the same applied potential.

  15. Effects of aldehydes and methods of cross-linking on properties of calcium alginate microspheres prepared by emulsification.

    PubMed

    Chan, Lai Wah; Heng, Paul W S

    2002-03-01

    Calcium alginate microspheres were prepared by an emulsification method and cross-linked with various aldehydes using different methods. Methanal and pentanedial produced low aggregation of microspheres while octanal and octadecanal produced the opposite effect. The latter two aldehydes displaced very little calcium ions from the alginate microspheres, indicating that the aggregation was due to the tackiness imparted by the aldehydes to the microsphere surface. Higuchi's model was not applicable to the drug release from microspheres in this study. The microspheres treated with methanal or pentanedial showed comparable dissolution T75% values which were significantly higher than that of the control. In contrast, octanal and octadecanal produced microspheres with lower dissolution T75% values. The drug contents of the microspheres treated with aldehydes were significantly lower than that of the control. There was insignificant interaction between the aldehydes and the drug. However, the aldehydes were found to impart acidity to the aqueous solution to varying extents, resulting in varying drug loss from the microspheres. The properties of the microspheres were also markedly affected by the method of incorporating the aldehyde. Soaking the microspheres in methanal solution produced microspheres with marked aggregation and low drug content. PMID:11808537

  16. Influence of the primary emulsification procedure on the characteristics of small protein-loaded PLGA microparticles for antigen delivery.

    PubMed

    Wischke, C; Borchert, H-H

    2006-06-01

    Microparticles prepared from poly(lactic-co-glycolic acid) (PLGA) using a W1/O/W2 double emulsion solvent evaporation method are suitable vehicles for the delivery of proteins to antigen presenting cells, e.g. dendritic cells. In this study, the influence of different techniques for the preparation of the primary W1/O emulsion was investigated with respect to the protein localization within the microparticles, morphological characteristics of these particles, protein burst release and the native state of the released protein. Bovine serum albumin bearing fluorescein isothiocyanate (FITC-BSA) was used as model protein. A static micromixer was applied for the preparation of the W1/O/W2 double emulsion. Employing a rotor-stator homogenizer (Ultra-Turrax) for primary emulsification, microcapsules with a high burst release were produced, because nearly all FITC-BSA was attached to the outside of the particle wall. Using a high pressure homogenizer or an ultrasonic procedure resulted in the formation of microspheres with homogeneous protein distribution and a reduced burst release. PMID:16854818

  17. Emulsification properties of a novel hydrocolloid (Angum gum) for d-limonene droplets compared with Arabic gum.

    PubMed

    Jafari, Seid Mahdi; Beheshti, Peyman; Assadpour, Elham

    2013-10-01

    In this study, the emulsification properties of a native biopolymer namely Angum gum (Ang) for use as a food flavor encapsulant in spray drying encapsulation was investigated and the results were compared with Arabic gum (Arg) stabilized emulsions. After gum extraction, gum dispersions with maltodextrin were prepared in water (in 1-5% concentrations) and emulsified with 5 and 10% d-limonene using high pressure homogenization. Statistical analysis of emulsion droplet size data revealed a significant difference between flavor level, gum type and droplet size at α=0.05. The results showed that increasing the Arg level leads to a decrease in emulsion droplet size, while increasing Ang content results in bigger droplet sizes. However, no significant differences were observed in droplet size. Also, droplet size data revealed that Ang-emulsified droplets at 2% gum and 5% flavor level had the lowest d32, d43 and the highest specific surface area by high-pressure homogenizer which could be mentioned as the optimum level of this native gum. PMID:23817096

  18. The effect of calcium on the composition and physical properties of whey protein particles prepared using emulsification.

    PubMed

    Westerik, Nieke; Scholten, Elke; Corredig, Milena

    2015-06-15

    Protein microparticles were formed through emulsification of 25% (w/w) whey protein isolate (WPI) solutions containing various concentrations of calcium (0.0-400.0mM) in an oil phase stabilized by polyglycerol polyricinoleate (PGPR). The emulsions were heated (at 80°C) and the microparticles subsequently re-dispersed in an aqueous phase. Light microscopy and scanning electron microscopy (SEM) images revealed that control particles and those prepared with 7.4mM calcium were spherical and smooth. Particles prepared with 15.0mM calcium gained an irregular, cauliflower-like structure, and at concentrations larger than 30.0mM, shells formed and the particles were no longer spherical. These results describe, for the first time, the potential of modulating the properties of dense whey protein particles by using calcium, and may be used as structuring agents for the design of functional food matrices with increased protein and calcium content. PMID:25660860

  19. Spray dried double emulsions containing procyanidin-rich extracts produced by premix membrane emulsification: effect of interfacial composition.

    PubMed

    Berendsen, Rikkert; Güell, Carme; Ferrando, Montserrat

    2015-07-01

    Spray drying of procyanidin-loaded W1/O/W2 emulsions produced by premix membrane emulsification (ME) enabled to produce microcapsules containing procyanidins. The interface of the emulsion droplets prior to spray drying was stabilized with several hydrophilic emulsifiers (whey protein (WPI), WPI-carboxylmethyl cellulose, WPI-gum Arabic, and WPI-chitosan). Their effect on procyanidin encapsulation efficiency, water activity, moisture and oil content, and microcapsule size distribution was investigated. Furthermore, the microstructure and droplet size distribution of redispersed microcapsules were analyzed. Although premix ME produced W1/O/W2 emulsions with a narrow droplet size distribution regardless the hydrophilic emulsifier (main peak of droplet size distribution around 9 μm), microcapsules after spray drying and double emulsions after redispersion showed profound differences in sizes depending on the interfacial composition. WPI-CMC stabilized microcapsules not only showed the highest procyanidin content (5.3 g kg(-1)) but also gave the narrowest particle size distribution with the lowest particle size for both microcapsules and the corresponding emulsions after rehydration (7.7 and 9.9 μm respectively). PMID:25704709

  20. Pickering emulsions stabilized by soft microgels: influence of the emulsification process on particle interfacial organization and emulsion properties.

    PubMed

    Destribats, Mathieu; Wolfs, Mélanie; Pinaud, Florent; Lapeyre, Véronique; Sellier, Elisabeth; Schmitt, Véronique; Ravaine, Valérie

    2013-10-01

    This work reports a new evidence of the versatility of soft responsive microgels as stabilizers for Pickering emulsions. The organization of microgels at the oil-water interface is a function of the preparation pathway. The present results show that emulsification energy can be used as a trigger to modify microgel deformation at the oil-water interface and their packing density: high shear rates bring strong flattening of the microgels, whereas low shear rates lead to dense monolayers, where the microgels are laterally compressed. As a consequence, the resulting emulsions have opposite behavior in terms of flocculation, which arises from bridging between neighboring drops and is strongly dependent on their surface coverage. This strategy can be applied to any microgel which can sufficiently adsorb at low shear rates, i.e. small microgels or lightly cross-linked ones. The control of the organization of microgels at the interface does not only modify emulsion end-use properties but also constitutes a new tool for the development of Janus-type microgels, obtained by chemical modification of the adsorbed microgels. PMID:24050149

  1. Optimization of the preparation of loperamide-loaded poly (L-lactide) nanoparticles by high pressure emulsification-solvent evaporation.

    PubMed

    Ueda, M; Kreuter, J

    1997-01-01

    The entrapment of loperamide hydrochloride (LPM) in biodegradable polymeric drug carriers such as nanoparticles might enable its passage across the blood-brain barrier. The optimization of the preparation of the LPM-loaded PLA nanoparticles was performed employing high pressure emulsification-solvent evaporation. The resulting nanoparticles were characterized by particle size, distribution, thermal analysis, and drug release profiles. The partition of LPM into the organic phase increased with an increase in pH of the aqueous phase and with addition of lipophilic surfactants such as sorbitan fatty acid esters, resulting in an increase in the drug entrapment in the nanoparticles. Evaporation of the organic phase under reduced pressure and the addition of ethanol in the organic phase yielded a high drug entrapment due to the rapid polymer precipitation. The addition of the sorbitan fatty acid esters further increased the drug entrapment even at higher LPM concentrations. The results of thermal analysis suggest that LPM was homogeneously dispersed in the amorphous polymer matrix. The in vitro release of the drug from nanoparticles was biphasic, with a fast initial phase, followed by a second slower phase. Different drug release profiles from nanoparticles can be achieved by addition of sorbitan fatty acid esters, or the employment of different solvents as the organic phase. PMID:9292435

  2. Mechanistic studies for monodisperse exenatide-loaded PLGA microspheres prepared by different methods based on SPG membrane emulsification.

    PubMed

    Qi, Feng; Wu, Jie; Yang, Tingyuan; Ma, Guanghui; Su, Zhiguo

    2014-10-01

    Poly(DL-lactic-co-glycolic acid) (PLGA) microspheres have been widely prepared by many methods, including solvent evaporation, solvent extraction and the co-solvent method. However, very few studies have compared the properties of microspheres fabricated by these methods. This is partly because the broad size distribution of the resultant particles severely complicates the analysis and affects the reliability of the comparison. To this end, uniform-sized PLGA microspheres have been prepared by Shirasu porous glass premix membrane emulsification and used to encapsulate exenatide, a drug for treating Type 2 diabetes. Based on this technique, the influences on the properties of microspheres fabricated by the aforementioned three methods were intensively investigated, including in vitro release, degradation and pharmacology. We found that these microspheres presented totally different release behaviors in vitro and in vivo, but exhibited a similar trend of PLGA degradation. Moreover, the internal structural evolution visually demonstrated these release behaviors. We selected for further examination the microsphere prepared by solvent evaporation because of its constant release rate, and explored its pharmacodynamics, histology, etc., in more detail. This microsphere when injected once showed equivalent efficacy to that of twice-daily injections of exenatide with no inflammatory response. PMID:24952071

  3. Nano-liter droplet libraries from a pipette: step emulsificator that stabilizes droplet volume against variation in flow rate.

    PubMed

    Dutka, Filip; Opalski, Adam S; Garstecki, Piotr

    2016-05-24

    Many modern analytical assays, for example, droplet digital PCR, or screening of the properties of single cells or single mutated genes require splitting a liquid sample into a number of small (typically ca. nano-liter in volume) independent compartments or droplets. This calls for a method that would allow splitting small (microliter) samples of liquid into libraries of nano-liter droplets without any dead volume or waste. Step emulsification allows for facile protocols that require delivery of only the sample liquid, yet they typically exhibit dependence of the droplet size on the rate at which the sample is injected. Here, we report a novel microfluidic junction that reduces the dependence of the volume of droplets on the rate of injection. We also demonstrate generation of tightly monodisperse nanoliter droplets by introduction of solely the dispersed phase into the system from an automatic pipette. The method presented here can readily be used and can replace the sophisticated devices typically used to generate libraries of nano-liter droplets from liquid samples. PMID:27161389

  4. Continuous synthesis of drug-loaded nanoparticles using microchannel emulsification and numerical modeling: effect of passive mixing.

    PubMed

    Ortiz de Solorzano, Isabel; Uson, Laura; Larrea, Ane; Miana, Mario; Sebastian, Victor; Arruebo, Manuel

    2016-01-01

    By using interdigital microfluidic reactors, monodisperse poly(d,l lactic-co-glycolic acid) nanoparticles (NPs) can be produced in a continuous manner and at a large scale (~10 g/h). An optimized synthesis protocol was obtained by selecting the appropriated passive mixer and fluid flow conditions to produce monodisperse NPs. A reduced NP polydispersity was obtained when using the microfluidic platform compared with the one obtained with NPs produced in a conventional discontinuous batch reactor. Cyclosporin, an immunosuppressant drug, was used as a model to validate the efficiency of the microfluidic platform to produce drug-loaded monodisperse poly(d,l lactic-co-glycolic acid) NPs. The influence of the mixer geometries and temperatures were analyzed, and the experimental results were corroborated by using computational fluid dynamic three-dimensional simulations. Flow patterns, mixing times, and mixing efficiencies were calculated, and the model supported with experimental results. The progress of mixing in the interdigital mixer was quantified by using the volume fractions of the organic and aqueous phases used during the emulsification-evaporation process. The developed model and methods were applied to determine the required time for achieving a complete mixing in each microreactor at different fluid flow conditions, temperatures, and mixing rates. PMID:27524896

  5. Solvent-impregnated agarose gel liquid phase microextraction of polycyclic aromatic hydrocarbons in water.

    PubMed

    Loh, Saw Hong; Sanagi, Mohd Marsin; Wan Ibrahim, Wan Aini; Hasan, Mohamed Noor

    2013-08-01

    A new microextraction procedure termed agarose gel liquid phase microextraction (AG-LPME) combined with gas chromatography-mass spectrometry (GC-MS) was developed for the determination of selected polycyclic aromatic hydrocarbons (PAHs) in water. The technique utilized an agarose gel disc impregnated with the acceptor phase (1-octanol). The extraction procedure was performed by allowing the solvent-impregnated agarose gel disc to tumble freely in the stirred sample solution. After extraction, the agarose gel disc was removed and subjected to centrifugation to disrupt its framework and to release the impregnated solvent, which was subsequently withdrawn and injected into the GC-MS for analysis. Under optimized extraction conditions, the new method offered high enrichment factors (89-177), trace level LODs (9-14ngL(-1)) and efficient extraction with good relative recoveries in the range of 93.3-108.2% for spiked drinking water samples. AG-LPME did not exhibit any problems related to solvent dissolution, and it provided high extraction efficiencies that were comparable to those of hollow fiber liquid phase microextraction (HF-LPME) and significantly higher than those of agarose film liquid phase microextraction (AF-LPME). This technique employed a microextraction format and utilized an environmentally compatible solvent holder that supported the green chemistry concept. PMID:23809804

  6. Liquid phase microextraction for the analysis of trace elements and their speciation

    NASA Astrophysics Data System (ADS)

    Hu, Bin; He, Man; Chen, Beibei; Xia, Linbo

    2013-08-01

    Trace/ultra-trace elements and their speciation analysis in complex matrices usually require sample preparation procedures to achieve sample clean-up and analyte preconcentration. Sample preparation is often the bottleneck in trace elements and their speciation analysis which has a direct impact on accuracy, precision and limits of detection and is often the rate-determining step of the analytical process. Recent trends in sample preparation include miniaturization, automation, high-throughput performance and reduction in solvent/sample consumption and operation time. Liquid-phase microextraction (LPME) technique as a novel and promising alternative in sample preparation can meet these requirements and has become a very efficient sample preparation technique. This review updates the state of art of LPME for trace elements and their speciation analysis and discusses its promising prospects. The major thrust of the article highlights the applications of LPME including single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME) and solidified floating organic drop microextraction (SFODME) to the fields of elemental and their speciation analysis by atomic spectrometry-based methods, especially inductively coupled plasma mass spectrometry. General and specific concepts, different extraction formats and characteristics of LPME are described and compared, along with examples of recent innovations and applications presented to demonstrate its potential for trace elements and their speciation analysis in biological and environmental fields. Moreover, the application potential and an outlook on the combination of LPME and atomic spectrometry-based techniques for inorganic analysis are commentated.

  7. Directly suspended droplet microextraction in combination with microvolume UV-vis spectrophotometry for determination of phosphate.

    PubMed

    Pena-Pereira, Francisco; Cabaleiro, Noelia; de la Calle, Inmaculada; Costas, Marta; Gil, Sandra; Lavilla, Isela; Bendicho, Carlos

    2011-08-15

    A miniaturized methodology for the determination of phosphate in waters has been developed by combining directly suspended droplet microextraction (DSDME) with microvolume spectrophotometry. The method is based on the extraction of the ion pair formed between 12-molybdophosphate and malachite green onto a microdrop of methyl isobutyl ketone and subsequent spectrophotometric determination with no dilution. An enrichment factor of 325 was obtained after 7.5 min of microextraction. The detection limit was 6.1 nM phosphate and the repeatability, expressed as relative standard deviation, was 2.7% (n=6). The method was successfully applied to the determination of dissolved reactive phosphorus in different freshwater samples. PMID:21726744

  8. Evolution of dispersive liquid-liquid microextraction method.

    PubMed

    Rezaee, Mohammad; Yamini, Yadollah; Faraji, Mohammad

    2010-04-16

    Dispersive liquid-liquid microextraction (DLLME) has become a very popular environmentally benign sample-preparation technique, because it is fast, inexpensive, easy to operate with a high enrichment factor and consumes low volume of organic solvent. DLLME is a modified solvent extraction method in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In this review, in order to encourage further development of DLLME, its combination with different analytical techniques such as gas chromatography (GC), high-performance liquid chromatography (HPLC), inductively coupled plasma-optical emission spectrometry (ICP-OES) and electrothermal atomic absorption spectrometry (ET AAS) will be discussed. Also, its applications in conjunction with different extraction techniques such as solid-phase extraction (SPE), solidification of floating organic drop (SFO) and supercritical fluid extraction (SFE) are summarized. This review focuses on the extra steps in sample preparation for application of DLLME in different matrixes such as food, biological fluids and solid samples. Further, the recent developments in DLLME are presented. DLLME does have some limitations, which will also be discussed in detail. Finally, an outlook on the future of the technique will be given. PMID:20005521

  9. Solid-phase microextraction of VOCs in water

    SciTech Connect

    Pratt, K.; Shirey, R.; Mani, V.

    1996-12-31

    The measurement of very low concentrations of organic compounds in the environment has been a subject of research for many years. Recently, the sample preparation in the analysis of aqueous samples has been achieved by solid phase microextraction (SPME). This method has been shown to be fast, inexpensive, solventless, portable and automatable. SPME has several advantages over conventional liquid-liquid extraction. SPME has been shown to be quantitative technique for volatile and semivolatile compounds from gaseous and liquid samples. The quantization by SPME is also linear over four orders of magnitude. As this method can reach a detection limit of 15 ppt (parts per trillion) for several compounds and can be easily automated, the analysis of volatile organic compounds (VOCs) in the environment, in particular, water samples, is highly advantageous by this method. This study will describe the analysis of volatile organics, BTEX, and halogenated organics in water. The lowest limit of detection, linearity, and other parameters will be discussed. The analysis of a soil sample taken near an oil storage tank for VOCs by SPME will be described. A comparison between different fibers (different types of coating materials and film thickness) using different columns will be described in this work.

  10. Ultrasonic emulsification of parenteral valproic acid-loaded nanoemulsion with response surface methodology and evaluation of its stability.

    PubMed

    Tan, Suk Fei; Masoumi, Hamid Reza Fard; Karjiban, Roghayeh Abedi; Stanslas, Johnson; Kirby, Brian P; Basri, Mahiran; Basri, Hamidon Bin

    2016-03-01

    Response surface methodology (RSM) was used to optimize the formulation of a nanoemulsion for central delivery following parenteral administration. A mixture of medium-chain triglyceride (MCT) and safflower seed oil (SSO) was determined as a sole phase from the emulsification properties. Similarly, a natural surfactant (lecithin) and non-ionic surfactant (Tween 80) (ratio 1:2) were used in the formulation. A central composite design (CCD) with three-factor at five-levels was used to optimize the processing method of high energy ultrasonicator. Effects of pre-sonication ultrasonic intensity (A), sonication time (B), and temperature (C) were studied on the preparation of nanoemulsion loaded with valproic acid. Influence of the aforementioned specifically the effects of the ultrasonic processing parameters on droplet size and polydispersity index were investigated. From the analysis, it was found that the interaction between ultrasonic intensity and sonication time was the most influential factor on the droplet size of nanoemulsion formulated. Ultrasonic intensity (A) significantly affects the polydispersity index value. With this optimization method, a favorable droplet size of a nanoemulsion with reasonable polydispersity index was able to be formulated within a short sonication time. A valproic acid loaded nanoemulsion can be obtained with 60% power intensity for 15 min at 60 °C. Droplet size of 43.21±0.11 nm with polydispersity index of 0.211 were produced. The drug content was then increased to 1.5%. Stability study of nanoemulsion containing 1.5% of valproic acid had a good stability as there are no significant changes in physicochemical aspects such as droplet size and polydispersity index. With the characteristisation study of pH, viscosity, transmission electron microscope (TEM) and stability assessment study the formulated nanoemulsion has the potential to penetrate blood-brain barrier in the treatment of epilepsy. PMID:26585010

  11. Evaluation of Time-Temperature Integrators (TTIs) with Microorganism-Entrapped Microbeads Produced Using Homogenization and SPG Membrane Emulsification Techniques.

    PubMed

    Rahman, A T M Mijanur; Lee, Seung Ju; Jung, Seung Won

    2015-12-28

    A comparative study was conducted to evaluate precision and accuracy in controlling the temperature dependence of encapsulated microbial time-temperature integrators (TTIs) developed using two different emulsification techniques. Weissela cibaria CIFP 009 cells, immobilized within 2% Na-alginate gel microbeads using homogenization (5,000, 7,000, and 10,000 rpm) and Shirasu porous glass (SPG) membrane technologies (10 μm), were applied to microbial TTIs. The prepared micobeads were characterized with respect to their size, size distribution, shape and morphology, entrapment efficiency, and bead production yield. Additionally, fermentation process parameters including growth rate were investigated. The TTI responses (changes in pH and titratable acidity (TA)) were evaluated as a function of temperature (20°C, 25°C, and 30°C). In comparison with conventional methods, SPG membrane technology was able not only to produce highly uniform, small-sized beads with the narrowest size distribution, but also the bead production yield was found to be nearly 3.0 to 4.5 times higher. However, among the TTIs produced using the homogenization technique, poor linearity (R(2)) in terms of TA was observed for the 5,000 and 7,000 rpm treatments. Consequently, microbeads produced by the SPG membrane and by homogenization at 10,000 rpm were selected for adjusting the temperature dependence. The Ea values of TTIs containing 0.5, 1.0, and 1.5 g microbeads, prepared by SPG membrane and conventional methods, were estimated to be 86.0, 83.5, and 76.6 kJ/mol, and 85.5, 73.5, and 62.2 kJ/mol, respectively. Therefore, microbial TTIs developed using SPG membrane technology are much more efficient in controlling temperature dependence. PMID:26370796

  12. Studies on the formation of polymeric nano-emulsions obtained via low-energy emulsification and their use as templates for drug delivery nanoparticle dispersions.

    PubMed

    Calderó, G; Montes, R; Llinàs, M; García-Celma, M J; Porras, M; Solans, C

    2016-09-01

    Ethylcellulose nanoparticles have been obtained from O/W nano-emulsions of the water/polyoxyethylene 10 oleyl ether/[ethyl acetate+4wt% ethylcellulose] system by low energy-energy emulsification at 25°C. Nano-emulsions with droplet sizes below 200nm and high kinetic stability were chosen for solubilising dexamethasone (DXM). Phase behaviour, conductivity and optical analysis studies of the system have evidenced for the first time that both, the polymer and the drug play a role on the structure of the aggregates formed along the emulsification path. Nano-emulsion formation may take place by both, phase inversion and self-emulsification. Spherical polymeric nanoparticles containing surfactant, showing sizes below 160nm have been obtained from the nano-emulsions by organic solvent evaporation. DXM loading in the nanoparticles was high (>90%). The release kinetics of nanoparticle dispersions with similar particle size and encapsulated DXM but different polymer to surfactant ratio were studied and compared to an aqueous DXM solution. Drug release from the nanoparticle dispersions was slower than from the aqueous solution. While the DXM solution showed a Fickian release pattern, the release behaviour from the nanoparticle dispersions was faster than that expected from a pure Fickian release. A coupled diffusion/relaxation model fitted the results very well, suggesting that polymer chains undergo conformational changes enhancing drug release. The contribution of diffusion and relaxation to drug transport in the nanoparticle dispersions depended on their composition and release time. Surfactant micelles present in the nanoparticle dispersion may exert a mild reservoir effect. The small particle size and the prolonged DXM release provided by the ethylcellulose nanoparticle dispersions make them suitable vehicles for controlled drug delivery applications. PMID:27341306

  13. Preparation of uniform-sized PLA microcapsules by combining Shirasu porous glass membrane emulsification technique and multiple emulsion-solvent evaporation method.

    PubMed

    Liu, Rong; Ma, Guanghui; Meng, Fan-Tao; Su, Zhi-Guo

    2005-03-01

    Relatively Uniform-sized biodegradable poly(lactide) (PLA) microcapsules were successfully prepared by combining a Shirasu Porous Glass (SPG) membrane emulsification technique and multiple emulsion-solvent evaporation method. An aqueous phase containing lysozyme was used as the internal water phase (w1), and PLA and Arlacel 83 were dissolved in a mixture solvent of dichloromethane (DCM) and toluene which was used as the oil phase (o). These two solutions were emulsified by a homogenizer to form a w1/o primary emulsion. The primary emulsion was permeated through the uniform pores (5.25 microm) of an SPG membrane into the external water phase by the pressure of nitrogen gas to form the uniform w1/o/w2 droplets. Then, the solid polymer microcapsules were obtained by simply evaporating the solvent. It is necessary to avoid the phase separation of primary emulsion during the SPG membrane emulsification. It was found that when the density difference of the internal water phase and oil phase was reduced to nearly zero and Arlacel 83 was used as the oil emulsifier, the phase separation was not observed within 24 h. The w1/o/w2 emulsion with uniform diameter was obtained only when Arlaecl 83 concentration was limited below 2.5 wt.% based on oil phase. The drug encapsulation efficiency was found to be related to several factors including PLA molecular weight, additive type and its concentration in the internal water phase, the emulsifier type and concentration in the oil phase, the NaCl concentration and the pH value in the external water phase. Comparing with the stirring method, it was found that the size was more uniform and the drug encapsulation efficiency was much higher when the microcapsules were prepared by SPG membrane emulsification technique and the highest drug encapsulation efficiency of 92.20% was obtained. This is the first study to prepare PLA microcapsules by combining an SPG membrane emulsification technique and multiple emulsion-solvent evaporation method

  14. Vortex-assisted liquid-liquid-liquid microextraction (VALLLME) technique: A new microextraction approach for direct liquid chromatography and capillary electrophoresis analysis.

    PubMed

    Makahleh, Ahmad; Yap, Hui Fang; Saad, Bahruddin

    2015-10-01

    A new, rapid and sensitive microextraction technique named vortex-assisted liquid-liquid-liquid microextraction (VALLLME) is proposed. The complete extraction process involves two steps. First, a vortex-assisted liquid-liquid microextraction (VALLME) procedure was used to extract the analytes from a relatively large volume of sample (donor phase) to a small volume of organic solvent (intermediate phase). Next, a micro-vortex-assisted liquid-liquid extraction (µ-VALLE) was used to extract the target analytes from the intermediate phase to a smaller volume of aqueous solution (acceptor phase). The final extract (acceptor phase) can be directly injected into the high performance liquid chromatography or capillary electrophoresis units without any further treatments. The selection of the intermediate phase and the manipulation of pH are key parameters that ensure good extraction efficiency of the technique. The proposed technique has been successfully applied for the determination of carvedilol (used as model analyte) in biological fluid samples. The optimum extraction conditions were: toluene as intermediate phase (150 μL); pH of the donor phase, 9.5; vortex time of the VALLME, 45 s (maximum speed, 2500 rpm); 0.1M HCl (15 μL) as acceptor phase; vortexing time of the µ-VALLME, 75 s (maximum stirring speed, 2500 rpm) and salt concentration in the donor phase, 5% (w/v). Under these conditions, enrichment factors of 51- and 418-fold for VALLME step and VALLLME procedure, respectively, were achieved. PMID:26078176

  15. Determination of Plant Volatiles Using Solid Phase Microextraction GC-MS

    ERIC Educational Resources Information Center

    Van Bramer, Scott; Goodrich, Katherine R.

    2015-01-01

    This experiment combines analytical techniques of solid phase microextraction and gas chromatography-mass spectrometry with easily relatable and accessible plant volatile chemistry (floral and vegetative scents of local/available plants). The biosynthesis and structure of these chemicals are of interest in the areas of organic chemistry,…

  16. Solid-phase microextraction of hydrocarbons from water in a centrifuge

    NASA Astrophysics Data System (ADS)

    Ryabov, A. Yu.; Chuikin, A. V.; Velikov, A. A.

    2016-06-01

    The results of our study of solid-phase microextraction of substances using a centrifuge for determining the microquantities of hydrocarbon impurities in water are presented. The cartridge diameter, sorbent mass, and solvent volume were shown to affect the percent extraction of substances and the analytical signal intensity. The relationship between the cartridge geometry, the sorbent mass, and the solvent volume was considered.

  17. Luminescence screening of enrofloxacin and ciprofloxacin residues in swine liver after dispersive liquid - liquid microextraction cleanup

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A rapid luminescence method was developed to screen residues of enrofloxacin (ENRO) and its metabolite, ciprofloxacin (CIPRO), in swine liver. Target analytes were extracted in acetonitrile-2.5% trifluoroacetic acid-NaCl, cleaned up by dispersive liquid-liquid microextraction (DLLME), and finally de...

  18. Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

    PubMed Central

    Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma

    2014-01-01

    In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from one side, toward automatization and online coupling of sample preparation units. The primary objective of this review is to present the recent developments in microextraction sample preparation methods for analysis of drugs in biological fluids. Microextraction techniques allow for less consumption of solvent, reagents, and packing materials, and small sample volumes can be used. In this review the use of solid phase microextraction (SPME), microextraction in packed sorbent (MEPS), and stir-bar sorbtive extraction (SBSE) in drug analysis will be discussed. In addition, the use of new sorbents such as monoliths and molecularly imprinted polymers will be presented. PMID:24688797

  19. Headspace analysis of polar organic compounds in biological matrixes using solid phase microextraction (SPME)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Analysis of biological fluids and waste material is difficult and tedious given the sample matrix. A rapid automated method for the determination of volatile fatty acids and phenolic and indole compounds was developed using a multipurpose sampler (MPS) with solid phase microextraction (SPME) and GC-...

  20. SOLID PHASE MICROEXTRACTION FOR TRACE LEVEL ANALYSIS OF DISINFECTION BY-PRODUCTS

    EPA Science Inventory

    This presentation focuses on the development of a solid-phase microextraction (SPME)-gas chromatography (GC)/ion trap mass spectrometry (MS) method for the analysis of semivolatile disinfection by-products (DBPs) in drinking water in the low ug/L range. These DBPs were selected ...

  1. Downsizing vacuum-assisted headspace solid phase microextraction.

    PubMed

    Psillakis, Elefteria; Yiantzi, Evangelia; Kalogerakis, Nicolas

    2013-07-26

    Recently, we proposed a new headspace solid-phase microextraction (HSSPME) procedure, termed vacuum-assisted HSSPME (Vac-HSSPME), where headspace sampling of 10mL aqueous sample volumes took place in 500 or 1000mL sample containers under vacuum conditions. In the present study, we downsized the extraction device to a 22mL modified sample vial and concluded that changes in the final total pressure of the pre-evacuated vial following sample introduction were sufficiently low to allow efficient Vac-HSSPME sampling. The downsized extraction device was used to extract five low molecular weight polycyclic aromatic hydrocarbons and several experimental parameters were controlled and optimized. For those compounds whose mass transfer resistance in the thin gas-film adjacent to the gas/sample interface controls evaporation rates, reducing the total pressure during HSSPME sampling dramatically enhanced extraction kinetics in the 22mL modified vial. Humidity was found to affect the amount of naphthalene (intermediate KH compound) extracted by the fiber at equilibrium as well as impair extraction of all analytes at elevated sampling temperatures. All the same, the high extraction efficiency and very good sensitivity achieved at room temperature and within short sampling times comprised the most important features of Vac-HSSPME in this downsized extraction device. Analytically, the developed method was found to yield linear calibration curves with limits of detection in the low ngL(-1) level and relative standard deviations ranging between 1.3 and 5.8%. Matrix was found not to affect extraction. PMID:23473517

  2. Zirconia hollow fiber: preparation, characterization, and microextraction application.

    PubMed

    Xu, Li; Lee, Hian Kee

    2007-07-15

    A zirconia hollow fiber membrane in the macrorange was for the first time successfully synthesized via a template method coupled with a sol-gel process. A polypropylene hollow fiber was employed as the template. The preparation procedure includes repeated impregnation of the template in the proper zirconia sol precursor, and calcination to burn off the template, producing the zirconia hollow fiber. The resulting hollow fiber membrane is almost identical to its template in terms of morphology, exhibiting a hollow core structure. In addition to that, it has a bimodal porous substructure that is different from its template, narrowly distributed nanoskeleton pores, and uniform textural pores or throughpores. The wall thickness and substructures can be conveniently controlled by the synthetic conditions and postheat treatment. Moreover, the thus-prepared zirconia hollow fiber was applied for the microextraction and concentration of a nerve agent degradation product followed by liquid chromatography-mass spectrometric analysis. Since the zirconia fiber exists as an individual device and is directly usable for extracting, handling is more convenient than, for example, an adsorbent in powder form that needs to be coated on a rod for the extraction process. In addition, it is easily prepared and is superior to the monolithic material in this sense. Pinacolyl methylphosphonic acid, one degradation product of organophosphorus nerve agent (soman), was used as the model analyte. Zirconia hollow fiber was demonstrated to be a highly selective adsorbent for the phosphonic acid-containing compounds with high sensitivity. Limit of detection was as low as 0.07 ng/mL (0.39 nM). PMID:17567103

  3. Automated Agitation-Assisted Demulsification Dispersive Liquid-Liquid Microextraction.

    PubMed

    Guo, Liang; Chia, Shao Hua; Lee, Hian Kee

    2016-03-01

    Dispersive liquid-liquid microextraction (DLLME) is an extremely fast and efficient sample preparation procedure. For its capability and applicability to be fully exploited, full automation of its operations seamlessly integrated with analysis is necessary. In this work, for the first time, fully automated agitation-assisted demulsification (AAD)-DLLME integrated with gas chromatography/mass spectrometry was developed for the convenient and efficient determination of polycyclic aromatic hydrocarbons in environmental water samples. The use of a commercially available multipurpose autosampler equipped with two microsyringes of different capacities allowed elimination or significant reduction of manpower, labor, and time with the large-volume microsyringe used for liquid transfers and the small-volume microsyringe for extract collection and injection for analysis. Apart from enhancing accessibility of DLLME, the procedure was characterized by the application of agitation after extraction to break up the emulsion (that otherwise would need centrifugation or a demulsification solvent), further improving overall operational efficiency and flexibility. Additionally, the application of low-density solvent as extractant facilitated the easy collection of extract as the upper layer over water. Some parameters affecting the automated AAD-DDLME procedure were investigated. Under the optimized conditions, the procedure provided good linearity (ranging from a minimum of 0.1-0.5 μg/L to a maximum of 50 μg/L), low limits of detection (0.010-0.058 μg/L), and good repeatability of the extractions (relative standard deviations, below 5.3%, n = 6). The proposed method was applied to analyze PAHs in real river water samples. PMID:26818217

  4. Micro and nano polycaprolactone particles preparation by pulsed back-and-forward cross-flow batch membrane emulsification for parenteral administration.

    PubMed

    Imbrogno, A; Piacentini, E; Drioli, E; Giorno, L

    2014-12-30

    In the pharmaceutical field, manufacturing processes which are able to make products with tailored size at suitable shear stress conditions and high productivity are important requirements for their industrial application. Cross-flow and premix membrane emulsification are the membrane-based processes generally used for particles preparation at large scale, however some disadvantages still limit their applicability for the production of fragile products. In this work, we investigated, for the first time, the preparation of micro and nano polymeric particles in a size range between 2.35 (±0.14)μm and 210 (±10)nm by using pulsed back-and-forward membrane emulsification for the application in pharmaceutical field. The suitability of the method to produce tailored particles by applying mild shear conditions has been demonstrated. The optimized fluid-dynamic conditions studied allowed the production of particles with target size by selecting the appropriate pore size of the membrane (1 μm and 0.1 μm). The uniformity of the particles could be obtained with an axial velocity of 0.5 ms(-1) (corresponding to a shear stress of 4.1 Pa) that is 9 times lower than the maximum cross flow velocity reported in literature (4.5 ms(-1)). PMID:25445520

  5. Quantification of Spontaneous W/O Emulsification and its Impact on the Swelling Kinetics of Multiple W/O/W Emulsions.

    PubMed

    Bahtz, Jana; Gunes, Deniz Z; Syrbe, Axel; Mosca, Nicola; Fischer, Peter; Windhab, Erich J

    2016-06-14

    An osmotic imbalance between the two water phases of multiple water-in-oil-in-water (W1/O/W2) emulsions results in either emulsion swelling or shrinking due to water migration across the oil layer. Controlled mass transport is not only of importance for emulsion stability but also allows transient emulsion thickening or the controlled release of encapsulated substances, such as nutriments or simply salt. Our prior work has shown that mass transport follows two sequential stages. In the first stage, the oil-phase structure is changed in a way that allows rapid, osmotically driven water transport in the second, osmotically dominated stage. These structural changes in the oil layer are strongly facilitated by the spontaneous formation of tiny water droplets in the oil phase, induced by the oil-soluble surfactant, i.e., polyglycerol polyricinoleate (PGPR). This study provides a simple method based on microscopy image analysis, allowing a detailed investigation of spontaneous W/O emulsification. It quantitatively describes the volume of droplets generated and the rate of droplet creation. Moreover, it describes the effect of spontaneous W/O emulsification on the swelling kinetics of microfluidic processed W1/O/W2 emulsions. Two different concentration regimes of the oil-soluble surfactant are identified: below a critical concentration the overall water transport rate increases, and above a critical concentration water transport stagnates because of maximized structure formation. PMID:27195479

  6. Porous, High Capacity Coatings for Solid Phase Microextraction by Sputtering.

    PubMed

    Diwan, Anubhav; Singh, Bhupinder; Roychowdhury, Tuhin; Yan, DanDan; Tedone, Laura; Nesterenko, Pavel N; Paull, Brett; Sevy, Eric T; Shellie, Robert A; Kaykhaii, Massoud; Linford, Matthew R

    2016-02-01

    We describe a new process for preparing porous solid phase microextraction (SPME) coatings by the sputtering of silicon onto silica fibers. The microstructure of these coatings is a function of the substrate geometry and mean free path of the silicon atoms, and the coating thickness is controlled by the sputtering time. Sputtered silicon structures on silica fibers were treated with piranha solution (a mixture of concd H2SO4 and 30% H2O2) to increase the concentration of silanol groups on their surfaces, and the nanostructures were silanized with octadecyldimethylmethoxysilane in the gas phase. The attachment of this hydrophobic ligand was confirmed by X-ray photoelectron spectroscopy and contact angle goniometry on model, planar silicon substrates. Sputtered silicon coatings adhered strongly to their surfaces, as they were able to pass the Scotch tape adhesion test. The extraction time and temperature for headspace extraction of mixtures of alkanes and alcohols on the sputtered fibers were optimized (5 min and 40 °C), and the extraction performances of SPME fibers with 1.0 or 2.0 μm of sputtered silicon were compared to those from a commercial 7 μm poly(dimethylsiloxane) (PDMS) fiber. For mixtures of alcohols, aldehydes, amines, and esters, the 2.0 μm sputtered silicon fiber yielded signals that were 3-9, 3-5, 2.5-4.5, and 1.5-2 times higher, respectively, than those of the commercial fiber. For the heavier alkanes (undecane-hexadecane), the 2.0 μm sputtered fiber yielded signals that were approximately 1.0-1.5 times higher than the commercial fiber. The sputtered fibers extracted low molecular weight analytes that were not detectable with the commercial fiber. The selectivity of the sputtered fibers appears to favor analytes that have both a hydrophobic component and hydrogen-bonding capabilities. No detectable carryover between runs was noted for the sputtered fibers. The repeatability (RSD%) for a fiber (n = 3) was less than 10% for all analytes tested

  7. Sol-gel-based molecularly imprinted xerogel for capillary microextraction.

    PubMed

    Bagheri, Habib; Piri-Moghadam, Hamed

    2012-09-01

    A novel molecularly imprinted xerogel (MIX) based on organically modified silica (ORMOSIL) was successfully prepared for on-line capillary microextraction (CME) coupled with high-performance liquid chromatography (HPLC). The sol-gel-based xerogel was prepared using only one precursor and exhibited extensive selectivity towards triazines along with significant thermal and chemical stability. Atrazine was selected as a model template molecule and 3-(trimethoxysilyl)propylmethacrylate (TMSPMA) as a precursor in which the propylmethacrylate moiety was responsible for van der Waals, dipole-dipole, and hydrogen-bond interactions with the template. This moiety plays a key role in creation of selective sites while methoxysilyl groups in TMSPMA acted as crosslinkers between the template and the propylmethacrylate moiety. Moreover, a non-imprinted xerogel (NIX) was also prepared in the absence of the template for evaluating the extraction efficiency of the prepared MIX. Then, the prepared imprinted and non-imprinted xerogels were used for extraction of three selected analytes of triazines class including atrazine, ametryn, and terbutryn, which have rather similar structures. The extraction efficiency of the prepared xerogel for atrazine, the template molecule, was found to be ten times greater than the efficiency achieved by the non-imprinted one. In the meantime, the extraction efficiency ratio of MIX to NIX for ametryn and terbutryn was also rather significant (eight times). Moreover, other compounds from different classes including dicamba, mecoprop, and estriol were also analyzed to evaluate the selectivity of the prepared MIX towards triazines. The ratio of enrichment factors (EF) of MIX to NIX for atrazine, ametryn, terbutryn, dicamba, mecoprop, and estriol were about 10, 8, 8, 2, 2, and 3, respectively. The linearity for the analytes was in the range of 5-700 μg L(-1). Limit of detection was in the range of 1-5 μg L(-1) and the RSD% values (n = 5) were all below 6

  8. Effect of blending and emulsification on thermal behavior, solid fat content, and microstructure properties of palm oil-based margarine fats.

    PubMed

    Saadi, S; Ariffin, A A; Ghazali, H M; Miskandar, M S; Abdulkarim, S M; Boo, H C

    2011-01-01

    The ability of palm oil (PO) to crystallize as beta prime polymorph has made it an attractive option for the production of margarine fat (MF). Palm stearin (PS) expresses similar crystallization behavior and is considered one of the best substitutes of hydrogenated oils due to its capability to impart the required level of plasticity and body to the finished product. Normally, PS is blended with PO to reduce the melting point at body temperature (37 °C). Lipid phase, formulated by PO and PS in different ratios were subjected to an emulsification process and the following analyses were done: triacylglycerols, solid fat content (SFC), and thermal behavior. In addition, the microstructure properties, including size and number of crystals, were determined for experimental MFs (EMFs) and commercial MFs (CMFs). Results showed that blending and emulsification at PS levels over 40 wt% significantly changed the physicochemical and microstructure properties of EMF as compared to CMF, resulting in a desirable dipalmitoyl-oleoyl-glycerol content of less than 36.1%. SFC at 37 °C, crystal size, crystal number, crystallization, and melting enthalpies (ΔH) were 15%, 5.37 μm, 1425 crystal/μm(2), 17.25 J/g, and 57.69J/g, respectively. All data reported indicate that the formation of granular crystals in MFs was dominated by high-melting triacylglycerol namely dipalmitoyl-oleoyl-glycerol, while the small dose of monoacylglycerol that is used as emulsifier slowed crystallization rate. Practical Application: Most of the past studies were focused on thermal behavior of edible oils and some blends of oils and fats. The crystallization of oils and fats are well documented but there is scarce information concerning some mechanism related to crystallization and emulsification. Therefore, this study will help to gather information on the behavior of emulsifier on crystallization regime; also the dominating TAG responsible for primary granular crystal formations, as well as to determine

  9. Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

    PubMed

    de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2016-09-14

    An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. PMID:27566338

  10. Headspace single drop microextraction coupled with microwave extraction of essential oil from plant materials.

    PubMed

    Zhai, Yujuan; Sun, Shuo; Wang, Ziming; Zhang, Yupu; Liu, He; Sun, Ye; Zhang, Hanqi; Yu, Aimin

    2011-05-01

    Headspace single drop microextraction (HS-SDME) coupled with microwave extraction (ME) was developed and applied to the extraction of the essential oil from dried Syzygium aromaticum (L.) Merr. et Perry and Cuminum cyminum L. The operational parameters, such as microdrop volume, microwave absorption medium (MAM), extraction time, and microwave power were optimized. Ten microliters of decane was used as the microextraction solvent. Ionic liquid and carbonyl iron powder were used as MAM. The extraction time was less than 7 min at the microwave power of 440 W. The proposed method was compared with hydrodistillation (HD). There were no obvious differences in the constituents of essential oils obtained by the two methods. PMID:21416601

  11. Field recovery of explosive residues using solid-phase microextraction followed by chromatographic analysis

    NASA Astrophysics Data System (ADS)

    Almirall, Jose R.; Wu, Lianming; Bi, Grace; Shannon, Michael W.; Furton, Kenneth G.

    1999-02-01

    An inexpensive, rapid and sensitive method for the field pre-concentration and subsequent analysis of high explosive residues from solid debris samples and from aqueous samples has been evaluated using solid-phase microextraction. Explosives studied included nitrobenzene, 2-nitrotoluene, 3- nitrotoluene, 4-nitrotoluene, 2,6-dinitrotoluene, 1,3- dinitrobenzene, 2,4-dinitrotoluene, trinitrotoluene, 1,3,5- trinitrobenzene, 4-amino-2,6-dinitrotoluene, 2-amino-4,6- dinitrotolene and tetryl.

  12. Generation, Characterization, and Application of Hierarchically Structured Self-Assembly Induced by the Combined Effect of Self-Emulsification and Phase Separation.

    PubMed

    Wang, Xiuyu; Hou, Yi; Yao, Li; Gao, Mingyuan; Ge, Maofa

    2016-02-24

    Hierarchically structured magnetic single-hole hollow spheres (MSHS) have been successfully obtained via a facile self-assembly strategy. This methodology allows the double emulsions generated via the combined effect of self-emulsification and phase separation to provide confinement for directing the self-assembly of magnetic nanoparticles (MNPs). The resulting MSHS fully capitalize on both the multifunctional properties of MNPs and container features of single-hole hollow spheres. Moreover, the magnetic properties showed obvious improvement and can be tuned by modulating the assembled structure. Thus, MSHS can be used as a smart platform with multiple functionalities including image contrast enhancement, selective encapsulation for biomacromolecules, on-demand release, and magnetically guided transport. This strategy is very promising in the design of hierarchically structured assemblies for desired applications in biomedicine and other fields. PMID:26835545

  13. Investigation of a microextraction procedure for the analysis of priority pollutants

    SciTech Connect

    Olszewski, L.T.

    1985-01-01

    The goal of this project was to develop a sample preparation procedure for the gas chromatographic analysis of priority pollutants in water using the technique known as microextraction. A microextraction procedure is one in which an aqueous sample is extracted with a much smaller volume of an immiscible organic solvent, thereby concentrating the analytes in the process of extracting them. Three groups of priority pollutants, the phenols, the phthalate esters and the nitroaromatics were used as model compounds. The procedure currently recommended by the US Environmental Protection Agency (EPA) for the analysis of these compounds involves a large scale extraction followed by evaporation of the extraction solvent. It was felt that microextraction would eliminate some of the difficulties of the EPA procedure such as lengthy sample preparation time, potential loss of volatile analytes and interference from impurities in the solvent which are concentrated during evaporation. The primary criteria used to evaluate the procedure were the recovery of analytes and the precision. A number of factors were investigated to determine their effect on these criteria. These factors included the choice of extraction solvent, the ratio of sample to solvent volume, the extraction time and technique, the effect of inorganic salts and the effect of sample concentration.

  14. Spectroscopic analysis of bosentan in biological samples after a liquid-liquid microextraction

    PubMed Central

    Sajedi-Amin, Sanaz; Assadpour-Zeynali, Karim; Panahi-Azar, Vahid; Kebriaeezadeh, Abbas; Khoubnasabjafari, Maryam; Ansarin, Khalil; Jouyban-Gharamaleki, Vahid; Jouyban, Abolghasem

    2015-01-01

    Introduction:Microextraction processes with UV-Vis measurement have been developed and validated for analysis of bosentan in biological samples. Methods:In this work, liquid–liquid microextraction procedures (DLLME & USAEME) were employed for cleanup, pre-concentration, and determination of bosentan in biological samples by UV-Vis spectroscopy at 270 nm. The method was validated and applied to the determination of bosentan in spiked serum, exhaled breath condensate and urine samples. Results:Various experimental factors including type of extraction and dispersive solvents and their volumes, pH, sonication time and centrifuging time were investigated. Under the optimum conditions, the method was linear in the range of 1.0–5.0 μg.mL-1, with coefficient of determination (R2) of > 0.998. The limit of detection (LOD) was 0.07 mg.L-1. Recovery of the target analyte in biological samples was 106.2%. The method could be easily applied for higher concentration of bosentan and needs more improvement for application in the pharmacokinetic investigations where more sensitive methods are required. Conclusion:A simple, low cost, precise and accurate spectrophotometric analysis of bosentan in biological samples after liquid-liquid microextraction were developed and validated for routine analyses. PMID:26929923

  15. Nanoformulation of poly(ethylene glycol) polymerized organic insect repellent by PIT emulsification method and its application for Japanese encephalitis vector control.

    PubMed

    Balaji, A P B; Mishra, Prabhakar; Suresh Kumar, R S; Mukherjee, Amitava; Chandrasekaran, Natarajan

    2015-04-01

    The utilization of increased dosage of insect repellents to overcome mosquito resistance has raised environmental concerns globally. In accord to this, we have formulated an efficacious, water-dispersive, nanometric formulation of a poor water-soluble insect repellent, diethylphenylacetamide (DEPA) by poly(ethylene glycol) (PEG) polymerization followed by PIT emulsification method. The critical micelle concentration of PEG in the spontaneously emulsified conventional DEPA droplets was determined, based on the droplets physical stability. Subjecting them to PIT emulsification yielded monodispersed polymeric nanomicelles of DEPA (Nano DEPA) with hydrodynamic mean diameter of 153.74 nm. The high-resolution scanning and transmission electron microscopic studies revealed the characteristic core-shell structure of micelle. The comparative efficacy of Bulk DEPA and Nano DEPA was evaluated by larvicidal and WHO cone bioassay against the Japanese encephalitis vector Culex tritaeniorhynchus. The median lethal concentrations (48 h) for 3rd instars C. tritaeniorhynchus larvae were found to be 0.416 mg/L for Bulk DEPA and 0.052 mg/L for Nano DEPA, respectively. The median knockdown concentrations (60 min) for the two to three-day-old, sucrose-fed, female adult mosquitoes were 5.372% (v/v) and 3.471% (v/v) for Bulk and Nano DEPA, respectively. Further investigation by histopathological and biochemical studies propound that Nano DEPA exerted better bioefficacy as comparative to its bulk form even at minimal exposure concentrations. Hence, Nano DEPA will serve as an effective alternate in controlling the vector expansion with reduced dosage. PMID:25766922

  16. Effects of sugars on the formation of nanometer-sized droplets of vegetable oil by an isothermal low-energy emulsification method.

    PubMed

    Ikeda, Shinya; Miyanoshita, Michitaka; Gohtani, Shoichi

    2013-07-01

    Effects of sugars on the formation of nanometer-sized oil droplets induced by the addition of vegetable oil to aqueous dispersions of polyoxyethylene sorbitan monooleate (MOPS, Tween 80) at 25 °C without the application of intensive mechanical energy were investigated. Phase diagrams were constructed using polarized light microscopy and small angle X-ray scattering (SAXS) to elucidate the relationship between the type of phases involved in the process of emulsification and the droplet size in the resulting emulsions. Nanometer-sized oil droplets as small as 220 nm in diameter were obtained when the sponge phase (L3 ) was formed at first, followed by the phase transition to coexisting multiple phases including the micellar cubic phase (I1 ) with increasing vegetable oil content. Sugars expanded the area of the sponge phase toward lower MOPS contents, enabling the formation of nano-emulsions from a wider range of the initial composition. The area of the sponge phase increased in the order of d-fructose ≈ d-glucose < sucrose < d-maltose, consistent with the order of the literature value of the mean number of equatorial hydroxyl groups per sugar molecule and that of the hydration number of sugar that represents the average number of water molecules forming a complex with a single molecule of sugar in aqueous solution. The present results confirm that sugars facilitate the formation of nano-emulsions using the isothermal low-energy emulsification method, presumably due to their abilities to shift the effective hydrophile-lipophile balance (HLB) of the surfactant toward the hydrophobic side. PMID:23701718

  17. Influence of process parameters on the size distribution of PLA microcapsules prepared by combining membrane emulsification technique and double emulsion-solvent evaporation method.

    PubMed

    Liu, Rong; Ma, Guang-Hui; Wan, Yin-Hua; Su, Zhi-Guo

    2005-11-10

    Relatively uniform-sized biodegradable poly(lactide) (PLA) microcapsules with various sizes were successfully prepared by combining a glass membrane emulsification technique and water-in-oil-in-water (w1/o/w2) double emulsion-solvent evaporation method. A water phase was used as the internal water phase, a mixture solvent of dichloromethane (DCM) and toluene dissolving PLA and Arlacel 83 was used as the oil phase (o). These two solutions were emulsified by a homogenizer to form a w1/o primary emulsion. The primary emulsion was permeated through the uniform pores of a glass membrane into the external water phase by the pressure of nitrogen gas to form the uniform w1/o/w2 double emulsion droplets. Then, the solid polymer microcapsules were obtained by simply evaporating solvent. The influence of process parameters on the size distribution of PLA microcapsules was investigated, with an emphasis on the effect of oil-soluble emulsifier. A unique phenomenon was found that a large part of emulsifier could adsorb on the interface of internal water phase and oil phase, which suppressed its adsorption on the surface of glass membrane, and led to the successful preparation of uniform-sized double emulsion. Finally, by optimizing the process parameters, PLA microcapsules with various sizes having coefficient of variation (CV) value under 14.0% were obtained. Recombinant human insulin (rhI), as a model protein, was encapsulated into the microcapsules with difference sizes, and its encapsulation efficiency and cumulative release were investigated. The result suggested that the release behavior could be simply adjusted just by changing precisely the diameters of microcapsule, benefited from the membrane emulsification technique. PMID:16198091

  18. O/W nano-emulsion formation using an isothermal low-energy emulsification method in a mixture of polyglycerol polyricinoleate and hexaglycerol monolaurate with glycerol system.

    PubMed

    Wakisaka, Satoshi; Nishimura, Takahisa; Gohtani, Shoichi

    2015-01-01

    We investigated how phase behavior changes by replacing water with glycerol in water/mixture of polyglycerol polyricinoleate (PGPR) and hexaglycerol monolaurate (HGML) /vegetable oil system, and studied the effect of glycerol on o/w nano-emulsion formation using an isothermal low-energy method. In the phase behavior study, the liquid crystalline phase (Lc) + the sponge phase (L3) expanded toward lower surfactant concentration when water was replaced with glycerol in a system containing surfactant HLP (a mixture of PGPR and HGML). O/W nano-emulsions were formed by emulsification of samples in a region of Lc + L3. In the glycerol/surfactant HLP/vegetable oil system, replacing water with glycerol was responsible for the expansion of a region containing Lc + L3 toward lower surfactant concentration, and as a result, in the glycerol/surfactant HLP/vegetable oil system, the region where o/w nano-emulsions or o/w emulsions could be prepared using an isothermal low-energy emulsification method was wide, and the droplet diameter of the prepared o/w emulsions was also smaller than that in the water/surfactant HLP/vegetable oil system. Therefore, glycerol was confirmed to facilitate the preparation of nano-emulsions from a system of surfactant HLP. Moreover, in this study, we could prepare o/w nano-emulsions with a simple one-step addition of water at room temperature without using a stirrer. Thus, the present technique is highly valuable for applications in several industries. PMID:25766932

  19. Fabrication, characterization and pharmacokinetic evaluation of doxorubicin-loaded water-in-oil-in-water microemulsions using a membrane emulsification technique.

    PubMed

    Pradhan, Roshan; Kim, Yong-Il; Jeong, Jee-Heon; Choi, Han-Gon; Yong, Chul Soon; Kim, Jong Oh

    2014-01-01

    Doxorubicin (DOX)-loaded water-in-oil-in-water (W/O/W) microemulsions were produced using a shirasu-porous-glass (SPG) membrane emulsification technique. Soybean oil was used as the oil phase; polyglycerol polyricinoleate (PGPR) or tetraglycerol polyricinoleate (TGPR) was used as the surfactant to stabilize the feed W/O emulsions, while Tween 20 was used in the external water phase to stabilize oil droplets containing water droplets. Increasing the feed pressure from 50 to 90 kPa increased the particle size of W/O/W emulsions, whereas it was decreased by increasing the agitator speed. The smallest particle sizes of multiple emulsions were obtained at the feed pressure of 50 kPa and agitator speed of 350 rpm. Under this set of conditions, the increase in the concentration of PGPR or TGPR showed a decrease in the particle size of DOX-loaded W/O/W emulsions. The optimized formulation comprising of 5% w/v PGPR and 3% w/v Tween 20 in the oil phase and external water phase, respectively, with 0.5% w/v of DOX had a particle size of 0.440±0.007 µm and polydispersity index of 0.220±0.087, which was supported by the transmission electron microscopy image. The formulations showed a sustained release profile in phosphate buffer solution (pH 7.4). The plasma concentrations of DOX after intravenous administration to rats were prolonged and gave approximately 17-fold higher area under the drug concentration-time curve (AUC) compared to free DOX solution. Thus, these results demonstrated that the SPG membrane emulsification technique could be used as a promising technique to prepare W/O/W microemulsions for delivering DOX with sustained release characteristics and better bioavailability. PMID:25177016

  20. Analysis of Whiskey by Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography/Mass Spectrometry: An Upper Division Analytical Chemistry Experiment Guided by Green Chemistry

    ERIC Educational Resources Information Center

    Owens, Janel E.; Zimmerman, Laura B.; Gardner, Michael A.; Lowe, Luis E.

    2016-01-01

    Analysis of whiskey samples prepared by a green microextraction technique, dispersive liquid-liquid microextraction (DLLME), before analysis by a qualitative gas chromatography-mass spectrometry (GC/MS) method, is described as a laboratory experiment for an upper division instrumental methods of analysis laboratory course. Here, aroma compounds in…

  1. Preparation of a graphene-based magnetic nanocomposite for the extraction of carbamate pesticides from environmental water samples.

    PubMed

    Wu, Qiuhua; Zhao, Guangying; Feng, Cheng; Wang, Chun; Wang, Zhi

    2011-11-01

    A graphene-based magnetic nanocomposite was synthesized and used for the first time as an effective adsorbent for the preconcentration of the five carbamate pesticides (metolcarb, carbofuran, pirimicarb, isoprocarb and diethofencarb) in environmental water samples prior to high performance liquid chromatography-diode array detection. The properties of the magnetic nanocomposite were characterized by scanning electron microscopy and X-ray diffraction. This novel graphene-based magnetic nanocomposite showed great adsorptive ability towards the analytes. The method, which takes the advantages of both nanoparticle adsorption and magnetic phase separation from the sample solution, could avoid some of the time-consuming experimental procedures related to the traditional solid phase extraction. Various experimental parameters that could affect the extraction efficiencies have been investigated. Under the optimum conditions, the enrichment factors of the method for the analytes were in the range from 474 to 868. A linear response was achieved in the concentration range of 0.1-50 ng mL(-1). The limits of detection of the method at a signal to noise ratio of 3 for the pesticides were 0.02-0.04 ng mL(-1). Compared with the dispersive liquid-liquid microextraction and the ultrasound-assisted surfactant-enhanced emulsification microextraction, much higher enrichment factors and sensitivities were achieved with the developed method. The method has been successfully applied for the determination of the carbamate pesticides in environmental water samples. PMID:21962496

  2. Comparison between solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HFLPME) for determination of extractables from post-consumer recycled PET into food simulants.

    PubMed

    Oliveira, Éder Costa; Echegoyen, Yolanda; Cruz, Sandra Andrea; Nerin, Cristina

    2014-09-01

    Hollow fiber liquid phase microextraction (HFLPME) and solid phase microextraction (SPME) methods for pre-concentration of contaminants (toluene, benzophenone, tetracosane and chloroform) in food simulants were investigated. For HFLPME 1-heptanol, 2-octanone and dibutyl-ether were studied as extracting solvents. Analysis by gas chromatography coupled to mass spectrometry (GC-MS), flame ionization (GC-FID) and electron capture detectors (GC-ECD) were carried out. In addition, the methods were employed to evaluate the safety in use of a PET material after the recycling process (comprising washing, extrusion and solid state polymerization (SSP)) through extractability studies of the contaminants using 10% (v/v) ethanol in deionized water and 3% (w/v) acetic acid in deionized water as food simulants in different conditions: 10 days at 40°C and 2h at 70°C. The HFLPME preconcentration method provided increased sensitivity when compared to the SPME method and allowed to analyze concentration levels below 10 µg surrogate per kg food simulant. The results of the extractability studies showed considerable reductions after the extrusion and SSP processes and indicated the compliance with regulations for using recycled PET in contact with food. PMID:24913857

  3. SURFACTANT ENHANCED REMEDIATION OF SOIL COLUMNS CONTAMINATED BY RESIDUAL TETRACHLOROETHYLENE

    EPA Science Inventory

    The ability of aqueous surfactant solutions to recover tetrachloroethylene (PCE) entrapped in Ottawa sand was evaluated in four column experiments. Residual PCE was emplaced by injecting 14C-labeled PCE into water-saturated soil columns and displacing the free product ...

  4. SURFACTANT ENHANCEMENT OF LIQUID CO2 FOR SURFACE CLEANING

    EPA Science Inventory

    The goal of this research activity is to develop the technical basis for a liquid CO2 (LCO2) based surface cleaning technology for metals and fabrics utilizing CO2 compatible surfactants. The use of CO2 is considered attractive for surface cleaning since it is abundant, cheap t...

  5. Surfactants Enhance Primisulfuron Activity in Common Lambsquarters (Chenopodium album L.)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Common lambsquarters (Chenopodium album L.) is one of the most widely distributed weed species in the world and is competitive with 40 crops. Greenhouse and laboratory studies were conducted to determine the effect of non-ionic (Induce®) and organosilicone (Silwet L-77®) surfactants on primisulfuron...

  6. Surfactant-enhanced alkaline flooding field project. Annual report

    SciTech Connect

    French, T.R.; Josephson, C.B.

    1993-12-01

    The Tucker sand from Hepler field, Crawford County, Kansas, was characterized using routine and advanced analytical methods. The characterization is part of a chemical flooding pilot test to be conducted in the field, which is classified as a DOE Class I (fluvial-dominated delta) reservoir. Routine and advanced methods of characterization were compared. Traditional wireline logs indicate that the reservoir is vertically compartmentalized on the foot scale. Routine core analysis, X-ray computed tomography (CT), minipermeameter measurement, and petrographic analysis indicate that compartmentalization and lamination extend to the microscale. An idealized model of how the reservoir is probably structured (complex layering with small compartments) is presented. There was good agreement among the several methods used for characterization, and advanced characterization methods adequately explained the coreflood and tracer tests conducted with short core plugs. Tracer and chemical flooding tests were conducted in short core plugs while monitoring with CT to establish flow patterns and to monitor oil saturations in different zones of the core plugs. Channeling of injected fluids occurred in laboratory experiments because, on core plug scale, permeability streaks extended the full length of the core plugs. A graphic example of how channeling in field core plugs can affect oil recovery during chemical injection is presented. The small scale of compartmentalization indicated by plugs of the Tucker sand may actually help improve sweep between wells. The success of field-scale waterflooding and the fluid flow patterns observed in highly heterogeneous outcrop samples are reasons to expect that reservoir flow patterns are different from those observed with short core plugs, and better sweep efficiency may be obtained in the field than has been observed in laboratory floods conducted with short core plugs.

  7. Surfactant-Enhanced Benard Convection on an Evaporating Drop

    NASA Astrophysics Data System (ADS)

    Nguyen, Van X.; Stebe, Kathleen J.

    2001-11-01

    Surfactant effects on an evaporating drop are studied experimentally. Using a fluorescent probe, the distribution and surface phase of the surfactant is directly imaged throughout the evaporation process. From these experiments, we identify conditions in which surfactants promote surface tension-driven Benard instabilities in aqueous systems. The drops under study contain finely divided particles, which act as tracers in the flow, and form well-defined patterns after the drop evaporates. Two flow fields have been reported in this system. The first occurs because the contact line becomes pinned by solid particles at the contact line region. In order for the contact line to remain fixed, an outward flow toward the ring results, driving further accumulation at the contact ring. A ‘coffee ring’ of particles is left as residue after the drop evaporates[1]. The second flow is Benard convection, driven by surface tension gradients on the drop[2,3]. In our experiments, an insoluble monolayer of pentadecanoic acid is spread at the interface of a pendant drop. The surface tension is recorded, and the drop is deposited on a well-defined solid substrate. Fluorescent images of the surface phase of the surfactant are recorded as the drop evaporates. The surfactant monolayer assumes a variety of surface states as a function of the area per molecule at the interface: surface gaseous, surface liquid expanded, and surface liquid condensed phases[4]. Depending upon the surface state of the surfactant as the drop evaporates, transitions of residue patterns left by the particles occur, from the coffee ring pattern to Benard cells to irregular patterns, suggesting a strong resistance to outward flow are observed. The occurrence of Benard cells on a surfactant-rich interface occurs when the interface is in LE-LC coexistence. Prior research concerning surfactant effects on this instability predict that surfactants are strongly stabilizing[5]. The mechanisms for this change in behavior are discussed. References: [1]R. D. Deegan,, PRE 61,475 (2000). [2]M. Maillard et al., J. Phys. Chem. B 104, 11871 (2000). [3]H. Wang et al. Langmuir 15, 957 (2001). [4]B. G. Moore et al., J. Phys. Chem. 94, 4588 (1990). [5]J. C. Berg & A. Acrivos, Chem. Eng. Sci. 20,737 (1965).

  8. Nonionic surfactants enhancing bactericidal activity at their critical micelle concentrations.

    PubMed

    Tobe, Seiichi; Majima, Toshiaki; Tadenuma, Hirohiko; Suekuni, Tomonari; Sakai, Kenichi; Sakai, Hideki; Abe, Masahiko

    2015-01-01

    Bactericidal activities of benzalkonium chloride [also known as alkyldimethylbenzylammonium chloride (ADBAC)] containing nonionic surfactants such as methyl ester ethoxylates (MEE) with the alkyl group C8-C14 and oxyethylene (EO) group of average adduct number 3-15 were measured against Escherichia coli and Staphylococcus aureus. Sample solutions containing MEE in the vicinity of the critical micelle concentration exhibited a dramatic decrease in viable bacterial counts. MEE with an alkyl group of C12 and an oxyethylene group of lower adduct number exhibited little viable bacterial counts than those having higher EO adduct numbers. MEE with reduced EO adduct numbers increased fluorescence intensity in E. coli using the viability stain SYTO 9. Our results show that MEE molecules with low EO adduct numbers exhibited bactericidal activity by increasing the permeability of the E. coli cell membrane. Sample solution containing ADBAC and MEE molecules with lower EO adduct numbers also displayed higher zeta potentials. Moreover, ADBAC molecules incorporated into micelles of MEE with lower EO adduct numbers were adsorbed onto the surface of E. coli, which augmented bactericidal activity. PMID:25492231

  9. Microbial surfactant-enhanced mineral oil recovery under laboratory conditions.

    PubMed

    Bordoloi, N K; Konwar, B K

    2008-05-01

    Microbial enhanced oil recovery (MEOR) is potentially useful to recover incremental oil from a reservoir being beyond primary and secondary recovery operations. Effort has been made to isolate and characterize natural biosurfactant produced by bacterial isolates collected from various oil fields of ONGC in Assam. Production of biosurfactant has been considered to be an effective major index for the purpose of enhanced oil recovery. On the basis of the index, four promising bacterial isolates: Pseudomonas aeruginosa (MTCC7815), P. aeruginosa (MTCC7814), P. aeruginosa (MTCC7812) and P. aeruginosa (MTCC8165) were selected for subsequent testing. Biosurfactant produced by the promising bacterial isolates have been found to be effective in the recovery of crude oil from saturated column under laboratory conditions. Two bacterial strains: P. aeruginosa (MTCC7815) and P. aeruginosa (MTCC7812) have been found to be the highest producer of biosurfactant. Tensiometer studies revealed that biosurfactants produced by these bacterial strains could reduce the surface tension (sigma) of the growth medium from 68 to 30 mN m(-1) after 96 h of growth. The bacterial biosurfactants were found to be functionally stable at varying pH (2.5-11) conditions and temperature of 100 degrees C. The treatment of biosurfactant containing, cell free culture broth in crude oil saturated sand pack column could release about 15% more crude oil at 90 degrees C than at room temperature and 10% more than at 70 degrees C under laboratory condition. PMID:18164187

  10. Surfactant mixing rules applied to surfactant enhanced alkaline flooding

    SciTech Connect

    Taylor, K.C. )

    1992-01-01

    This paper discusses surfactant mixing rules which have been used to describe crude oil/alkali/surfactant phase behavior, using David Lloydminster crude oil and the surfactant Neodol 25-3S. It was found that at a fixed salinity and alkali concentration, a specific mole fraction of synthetic surfactant to petroleum soap was required to produce optimal phase behavior as the water-to-oil ratio varied. This methodology is useful in understanding the relationship between the variables of water-to-oil ratio and synthetic surfactant concentration in phase behavior systems that produce a petroleum soap.

  11. Competitive substrate biodegradation during surfactant-enhanced remediation

    SciTech Connect

    Goudar, C.; Strevett, K.; Grego, J.

    1999-12-01

    The impact of synthetic surfactants on the aqueous phase biodegradation of benzene, toluene, and p-xylene (BTpX) was studied using two anionic surfactants, sodium dodecyl sulfate (SDS) and sodium dodecyl benzene sulfonate (SDBS), and two nonionic surfactants, POE(20) sorbitan monooleate (T-maz-80) and octyl-phenolpoly(ethyleneoxy) ethanol (CA-620). Batch biodegradation experiments were performed to evaluate surfactant biodegradability using two different microbial cultures. Of the four surfactants used in this study, SDS and T-maz-80 were readily degraded by a microbial consortium obtained from an activated sludge treatment system, whereas only SDS was degraded by a microbial culture that was acclimated to BTpX. Biodegradation kinetic parameters associated with SDS and T-maz-80 degradation by the activated sludge consortium were estimated using respirometric data in conjunction with a nonlinear parameter estimation technique as {mu}{sub max} = 0.93 h{sup {minus}1}, K{sub s}= 96.18 mg/L and {mu}{sub max} = 0.41 h{sup {minus}1}, K{sub s} = 31.92 mg/L, respectively. When both BTpX and surfactant were present in the reactor along with BTpX-acclimated microorganisms, two distinct biodegradation patterns were seen. SDS was preferentially utilized inhibiting hydrocarbon biodegradation, whereas, the other three surfactants had no impact on BTpX biodegradation. None of the four surfactants were toxic to the microbial cultures used in this study. Readily biodegradable surfactants are not very effective for subsurface remediation applications as they are rapidly consumed, and also because of their potential inhibitory effects on intrinsic hydrocarbon biodegradation. This greatly increases treatment costs as surfactant recovery and reuse are adversely affected.

  12. Surfactant enhanced electrokinetic remediation of DDT from soils.

    PubMed

    Karagunduz, Ahmet; Gezer, Aras; Karasuloglu, Gulden

    2007-10-15

    Electrokinetic remediation has been investigated extensively as one of the noble technologies in remediation of metal contaminated soils. However, its applications in remediation of organic contaminants have been limited due to low solubilities of organics in water. In addition, most organic contaminants are non-ionic and therefore, they are not mobile under electrical field. The use of surfactants may increase the remediation efficiency by increasing the solubility of organics. Significant fraction of organics associated with soil, can be transferred to micellar phase, which then can be transported toward either cathode or anode, depending on the ionic group of surfactants. In this study, the removal of hydrophobic organic contaminants from a soil using electrokinetic method was investigated in the presence of surfactants. A nonionic surfactant, Tween 80, and an anionic surfactant, SDBS, were used in the experiments. DDT was chosen as the model organic contaminant. Phase distribution studies and column experiments were conducted. It was found that both Tween 80 and SDBS had similar solubilization potentials for DDT. It was also shown that the aqueous DDT mass could reach from 0.01 to 13% of the total mass in the presence of 7500 mg/L of SDBS. No significant movement of DDT was observed when Tween 80 was used in the column experiments. This was attributed to low rates of electroosmotic flows and strong interaction of Tween 80 with the soil. The amount of surfactant was not enough to mobilize DDT significantly in the column studies. On the other hand, electrokinetic transport with SDBS yielded much better results. DDT transport toward the anode within the negatively charged micelles overcame the opposite electrosmotic flow. This was attributed to the lower degree of interaction between the soil and SDBS, and the electrokinetic transport of negatively charged micelles. PMID:17706747

  13. Development of dispersive liquid-liquid microextraction based on solidification of floating organic drop for the determination of trace nickel.

    PubMed

    Wang, Yukun; Zhang, Jingwen; Zhao, Bin; Du, Xin; Ma, Jingjun; Li, Jingci

    2011-12-01

    A liquid-phase microextraction technique was developed using dispersive liquid-liquid microextraction based on solidification of floating organic drop combined with flame atomic absorption spectrometry, for the extraction and determination of trace amounts of nickel in water samples. Microextraction efficiency factors, such as the type and volume of extraction and dispersive solvents, pH, extraction time, the chelating agent amount, and ionic strength, were investigated and optimized. Under optimum conditions, the calibration graph was linear in the range of 4.23-250 μg L(-1) with a detection limit of 1.27 μg L(-1). The relative standard deviation for ten replicate measurements of 10 and 100 μg L(-1) of nickel were 3.21% and 2.55%, respectively. The proposed method was assessed through the analysis of certified reference water or recovery experiments. PMID:21598026

  14. Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

    PubMed

    Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

    2016-03-01

    An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. PMID:26833965

  15. Application of solid phase microextraction to the analysis of chlorinated contaminants in environmental matrices

    SciTech Connect

    Webster, G.R.B.; Sarna, L.P.; Anderson, K.L.; Graham, K.N.

    1994-12-31

    Contamination of aquatic and terrestrial systems with organic contaminants is an increasing toxicological problem. In both the monitoring of such contamination and the determination of the success of remediation methods, straightforward and inexpensive analytical methodology increases the ease of environmental assessment and facilitates regulatory enforcement. Solid phase microextraction (SPME) technology is a recently developed solvent less extraction system with the potential for application to the analysis of a wide range of compounds. Application of SPME, in combination with gas chromatography and GC-MS, will be described for the analysis of chlorinated environmental contaminants such as pesticides and selected PCBs, dioxins, and furans in soils, sediments, and water.

  16. Selective Stationary Phase for Solid-Phase Microextraction Analysis of Sarin (GB)

    SciTech Connect

    Harvey, Scott D.; Nelson, David A.; Wright, Bob W.; Grate, Jay W.

    2002-04-19

    A number of critical field applications require monitoring air samples for trace levels of chemical warfare agents. Solid-phase microextraction (SPME) is a convenient format to conduct these analyses. Measurements could be significantly improved if a SPME phase selective for nerve agents were substituted for nonselective polymers typically used (e.g.,polydimethylsiloxane). This paper evaluates a novel stationary phase, previously developed for methylphosphonate sensor applications, for use with SPME sampling. The phenol-based polymer, BSP3, was found to offer far higher selectivity toward sarin (GB) than polydimethylsiloxane due to a pronounced affinity toward the target analyte and a lower affinity toward hydrocarbons.

  17. Selective Stationary Phase for Solid-Phase Microextraction Analysis of Sarin (GB)

    SciTech Connect

    Harvey, Scott; Nelson, D. A.; Wright, Bob W.; Gates, J. W.

    2002-03-02

    A number of critical field applications require monitoring air samples for trace levels of chemical warfare agents. Solid-phase microextraction (SPME) is a convenient format to conduct these analyses. Measurements could be significantly improved if a SPME phase selective for nerve agents were substituted for nonselective polymers typically used (e.g., polydimethylsiloxane). This paper evaluates a novel stationary phase, previously developed for methylphosphonate sensor applications, for use with SPME sampling. The phenol-based polymer, BSP3, was found to offer far higher selectivity toward sarin (GB) than polydimethylsiloxane due to a pronounced affinity toward the target analyte and a lower affinity toward hydrocarbons.

  18. Direct Mass Spectrometry Analysis of Biofluid Samples Using Slug Flow Microextraction NanoESI**

    PubMed Central

    Ren, Yue; McLuckey, Morgan N.; Liu, Jiangjiang; Ouyang, Zheng

    2015-01-01

    Direct mass spectrometry (MS) analysis of biofluids with simple procedures represents a key step in translation of MS technologies to the clinical and point-of-care applications. The current study reports the development of a single-step method using slug flow microextraction and nanoESI (electrospray ionization) for MS analysis of organic compounds in blood and urine. High sensitivity and quantitation precision have been achieved for analysis of therapeutic and illicit drugs in 5 μL samples. Real-time chemical derivatization has been incorporated for analyzing anabolic steroids. The monitoring of enzymatic functions has also been demonstrated with the cholinesterase in wet blood. PMID:25284028

  19. Capillary microextraction (CME) and its application to trace elements analysis and their speciation.

    PubMed

    Hu, Bin; Zheng, Fei; He, Man; Zhang, Nan

    2009-09-14

    As a solvent-free miniaturized sample preparation technique, capillary microextraction (CME) has been hyphenated with different analytical instruments for trace elements analysis of environmental, biological, food and pharmaceutical samples. This review discusses the fundamentals and recent development of CME, including the theoretical basis, extraction modes (packed, open-tubular and monolithic CME) and capillary materials for CME. The emphasis is placed on the application of CME to trace/ultra-trace elements analysis and their speciation. Existing coating/monolithic materials used for CME are summarized together with a detailed overview of their preparation methods. PMID:19720168

  20. Ultrasound-assisted magnetic dispersive solid-phase microextraction: A novel approach for the rapid and efficient microextraction of naproxen and ibuprofen employing experimental design with high-performance liquid chromatography.

    PubMed

    Ghorbani, Mahdi; Chamsaz, Mahmoud; Rounaghi, Gholam Hossein

    2016-03-01

    A simple, rapid, and sensitive method for the determination of naproxen and ibuprofen in complex biological and water matrices (cow milk, human urine, river, and well water samples) has been developed using ultrasound-assisted magnetic dispersive solid-phase microextraction. Magnetic ethylendiamine-functionalized graphene oxide nanocomposite was synthesized and used as a novel adsorbent for the microextraction process and showed great adsorptive ability toward these analytes. Different parameters affecting the microextraction were optimized with the aid of the experimental design approach. A Plackett-Burman screening design was used to study the main variables affecting the microextraction process, and the Box-Behnken optimization design was used to optimize the previously selected variables for extraction of naproxen and ibuprofen. The optimized technique provides good repeatability (relative standard deviations of the intraday precision 3.1 and 3.3, interday precision of 5.6 and 6.1%), linearity (0.1-500 and 0.3-650 ng/mL), low limits of detection (0.03 and 0.1 ng/mL), and a high enrichment factor (168 and 146) for naproxen and ibuprofen, respectively. The proposed method can be successfully applied in routine analysis for determination of naproxen and ibuprofen in cow milk, human urine, and real water samples. PMID:27027588

  1. [Studies on preparation by SPG membrane emulsification method and in vitro characterization of tetradrine-tashionone II(A)-PLGA composite microspheres].

    PubMed

    Lu, Jin; Zhang, Meng; Zhu, Hua-xu; Guo, Li-wei; Pan, Lin-mei; Fu, Ting-ming

    2015-03-01

    Tetradrine-tashionone II(A)-PLGA composite microspheres were prepared by the SPG membrane emulsification method, and the characterization of tetradrine-tashionone II(A) -PLGA composite microspheres were studied in this experiment. The results of IR, DSC and XRD showed that teradrine and tashionone II(A) in composite microspheres were highly dispersed in the PLGA with amorphous form. The results of tetradrine-tashionone II(A) -PLGA composite microspheres in vitro release experiment showed that the cumulative release amounts of tetradrine and tashionone II(A) were 6.44% and 3.60% in 24 h, and the cumulative release amounts of tetradrine and tashionone II(A) were 89.02% and 21.24% in 17 d. The process of drug in vitro release accorded with the model of Riger-Peppas. Tetradrine-tashionone II(A) -PLGA composite microspheres had slow-release effect, and it could significantly reduce the burst release, prolong the therapeutic time, decrease the dosage of drugs and provide a new idea and method to prepare traditional Chinese medicine compound. PMID:26226751

  2. A modified spontaneous emulsification solvent diffusion method for the preparation of curcumin-loaded PLGA nanoparticles with enhanced in vitro anti-tumor activity

    NASA Astrophysics Data System (ADS)

    Chen, Cen; Yang, Wei; Wang, Dan-Tong; Chen, Chao-Long; Zhuang, Qing-Ye; Kong, Xiang-Dong

    2014-12-01

    To improve the anti-tumor activity of hydrophobic drug curcumin, we prepared curcumin-loaded PLGA nanoparticles (PLGA-Cur NPs) through a modified spontaneous emulsification solvent diffusion (modified-SESD) method. The influence of main preparation parameters was investigated, such as the volume ratio of binary organic solvents and the concentration of surfactant. Results indicated that the synthesized regular spherical PLGA NPs with the average diameter of 189.7 nm exhibited relatively higher yield (58.9%), drug loading (11.0% (w/w)) and encapsulation efficiency (33.5%), and also a controllable drug release profile. In order to evaluate the in vitro cytotoxicity of the prepared NPs, MTT assay was conducted, and results showed that the NPs could effectively inhibit HL60 and HepG2 cells with lower IC50 values compared with free curcumin. Furthermore, confocal microscopy together with flow cytometry analysis proved the enhanced apoptosis-inducing ability of PLGA-Cur NPs. Polymeric NP formulations are potential to be used for hydrophobic drug delivery systems in cancer therapy.

  3. Studies on the formation of O/W nano-emulsions, by low-energy emulsification method, suitable for cosmeceutical applications.

    PubMed

    Jaworska, Małgorzata; Sikora, Elżbieta; Zielina, Michał; Ogonowski, Jan

    2013-01-01

    The formation of oil/water (O/W) nano-emulsions suitable for cosmeceutical application was studied. Nano-emulsions were prepared by using phase inversion composition (PIC) method, one of the low-energy emulsification methods. The process consist of stepwise water addition to oil/surfactant mixture, at T = 25°C. Caprylic/capric triglycerides (GTCC), propylene glycol dicaprylate/dicaprate (PC) and oleic acid (OA) were applied as an oil phase. Polysorbate 80 was used as the surfactant. Kinetic stability of the nano-emulsions was analyzed by measuring droplet size as a function of time for different oil/surfactant ratio. The particles size distribution was analyzed by means DLS measurement technique (Dynamic Light Scattering), using Zetasizer Nano ZS (Malvern Instruments, UK). One of triterpenoic acid, practically non-water soluble substance was selected as an active and incorporated into the stable formulation. The obtained results proved that the nanoemulsion NE-T80-GTCC-20:80 based on caprylic/capric triglycerides with the oil/surfactant ratio O/S = 2 0:80 and the droplet size r = 25 nm was the most stable one and additionally showed the highest solubilisation capacity for the triterpene. PMID:24432331

  4. In vitro biomineralization and bulk characterization of chitosan/hydroxyapatite composite microparticles prepared by emulsification cross-linking method: orthopedic use.

    PubMed

    Maachou, Hamida; Bal, Kheireddine; Bal, Youcef; Chagnes, Alexandre; Cote, Gerard; Aliouche, Djamel

    2012-11-01

    Chitosan/hydroxyapatite composite microparticles were prepared by a solid-in-water-in-oil emulsification cross-linking method. The characteristics and activity in presence of simulated body fluid for 14 and 21 days were investigated. The size distribution, surface morphology, and microstructure of these biomaterials were evaluated. The scanning electron microscopy revealed an aggregate of microparticles with a particle size, ranged from 4 to 10 μm. The deposited calcium phosphate was studied using X-ray diffraction analysis, Fourier transform infrared spectroscopy, and inductively coupled plasma/atomic emission spectroscopy analysis of phosphorus. These results show that the mineral, formed on microparticles, was a mixture of carbonated hydroxyapatite and calcite. Scanning electron microscopy revealed that calcium phosphate crystals growth was in form of rods organized as concentric triangular packets interconnected to each other by junctions. Interaction between chitosan and growing carbonated hydroxyapatite and calcite crystals are responsible for a composite growth into triangular and spherical shapes. The results demonstrated that these microparticles were potential materials for bone repair. PMID:23015190

  5. Dynamic microwave-assisted extraction combined with continuous-flow microextraction for determination of pesticides in vegetables.

    PubMed

    Wu, Lijie; Hu, Mingzhu; Li, Zhanchao; Song, Ying; Yu, Cui; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2016-02-01

    A simple, rapid, solventless and cost-effective dynamic microwave-assisted extraction (DMAE) combined with continuous-flow microextraction (CFME) system was firstly assembled and validated for extraction of eight organophosphorus pesticides in vegetables. The method combines the advantages of DMAE and CFME, and extends the application of the single drop microextraction to complex solid samples. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, analytes were first extracted from the vegetables using 3% NaCl solution as extraction solvent, then concentrated into microextraction solvent. After extraction, the microextraction solvent containing the enriched analyte was directly analyzed by GC-MS without any filtration or clean-up process. Several parameters affecting the extraction efficiency were investigated and optimized. Real vegetable samples were analyzed, satisfactory recoveries were obtained in the range of 80.7-106.7%, and relative standard deviations were lower than 8.7%. PMID:26304388

  6. PARTITION INFRARED METHOD FOR TOTAL GASOLINE RANGE ORGANICS IN WATER BASED ON SOLID PHASE MICROEXTRACTION. (R825343)

    EPA Science Inventory

    A new method is described for determining total gasoline-range organics
    (TGRO) in water that combines solid-phase microextraction (SPME) and infrared
    (IR) spectroscopy. In this method, the organic compounds are extracted from
    250-mL of water into a small square (3....

  7. Sensitive Determination of Terazosin in Pharmaceutical Formulations and Biological Samples by Ionic-Liquid Microextraction Prior to Spectrofluorimetry

    PubMed Central

    Zeeb, Mohsen; Sadeghi, Mahdi

    2012-01-01

    An efficient and environmentally friendly sample preparation method based on the application of hydrophobic 1-Hexylpyridinium hexafluorophosphate [Hpy][PF6] ionic liquid (IL) as a microextraction solvent was proposed to preconcentrate terazosin. The performance of the microextraction method was improved by introducing a common ion of pyridinium IL into the sample solution. Due to the presence of the common ion, the solubility of IL significantly decreased. As a result, the phase separation successfully occurred even at high ionic strength, and the volume of the settled IL-phase was not influenced by variations in the ionic strength (up to 30% w/v). After preconcentration step, the enriched phase was introduced to the spectrofluorimeter for the determination of terazosin. The obtained results revealed that this system did not suffer from the limitations of that in conventional ionic-liquid microextraction. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.027 μg L−1 and a relative standard deviation (R.S.D.) of 2.4%. The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples. Considering the large variety of ionic liquids, the proposed microextraction method earns many merits, and will present a wide application in the future. PMID:22505920

  8. Rapid screening of oxytetracycline residue in catfish muscle by dispersive liquid-liquid microextraction and europium-sensitized luminescence

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Oxytetracycline (OTC) residue in catfish muscle was screened by dispersive liquid-liquid microextraction (DLLME) and europium-sensitized luminescence (ESL). After extraction in EDTA, HCl, and acetonitrile, cleanup was carried out by DLLME, and ESL was measured at microgram = 385 nm and wavelength = ...

  9. Application of graphene nanoplatelets silica composite, prepared by sol-gel technology, as a novel sorbent in two microextraction techniques.

    PubMed

    Heidari, Mahmoud; Bahrami, Abdolrahman; Ghiasvand, Ali Reza; Shahna, Farshid Ghorbani; Soltanian, Ali Reza; Rafieiemam, Maryam

    2015-12-01

    In this study, the application of a novel nanomaterial composite was investigated in two microextraction techniques of solid-phase microextraction and a needle trap device in a variety of sampling conditions. The optimum sampling temperature and relative humidity were 10°C and 20%, respectively, for both techniques with two sorbents of graphene/silica composite and polydimethyl siloxane. The two microextraction techniques with the proposed sorbent showed recoveries of 95.2 and 94.6% after 7 days. For the needle trap device the optimums desorption time and temperature were 3 min at 290°C and for SPME these measures were 1 and 1.5 min at 240-250°C for the graphene/silica composite and polydimethyl siloxane, respectively. The relative standard division obtained in inter- and intra-day comparative studies were 3.3-14.3 and 5.1-25.4, respectively. For four sample the limit of detection was 0.021-0.25 ng/mL, and the limit of quantitation was 0.08-0.75 ng/mL. The results show that the graphene/silica composite is an appropriate extraction media for both techniques. Combining an appropriate sorbent with microextraction techniques, and using these in conjunction with a sensitive analytical instrument can introduce a strong method for sampling and analysis of occupational and environmental pollutants in air. PMID:26459611

  10. Sensitive determination of terazosin in pharmaceutical formulations and biological samples by ionic-liquid microextraction prior to spectrofluorimetry.

    PubMed

    Zeeb, Mohsen; Sadeghi, Mahdi

    2012-01-01

    An efficient and environmentally friendly sample preparation method based on the application of hydrophobic 1-Hexylpyridinium hexafluorophosphate [Hpy][PF(6)] ionic liquid (IL) as a microextraction solvent was proposed to preconcentrate terazosin. The performance of the microextraction method was improved by introducing a common ion of pyridinium IL into the sample solution. Due to the presence of the common ion, the solubility of IL significantly decreased. As a result, the phase separation successfully occurred even at high ionic strength, and the volume of the settled IL-phase was not influenced by variations in the ionic strength (up to 30% w/v). After preconcentration step, the enriched phase was introduced to the spectrofluorimeter for the determination of terazosin. The obtained results revealed that this system did not suffer from the limitations of that in conventional ionic-liquid microextraction. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.027 μg L(-1) and a relative standard deviation (R.S.D.) of 2.4%. The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples. Considering the large variety of ionic liquids, the proposed microextraction method earns many merits, and will present a wide application in the future. PMID:22505920

  11. SCREENING METHOD FOR NITROAROMATIC COMPOUNDS IN WATER BASED ON SOLID-PHASE MICROEXTRACTION AND INFRARED SPECTROSCOPY. (R825343)

    EPA Science Inventory

    A new method is described for determining nitroaromatic compounds in water
    that combines solid-phase microextraction (SPME) and infrared (IR) spectroscopy. In this method, the compounds are extracted from a 250-mL volume of water into a small square (3.2 cm ? 3.2 cm ? 61.2...

  12. Headspace in-tube microextraction coupled with micellar electrokinetic chromatography of neutral aromatic compounds.

    PubMed

    Cho, Sung Min; Park, Bum Su; Jung, Woo Sung; Lee, Sang Won; Jung, Yunhwan; Chung, Doo Soo

    2016-02-01

    Headspace (HS) extraction can be carried out easily and aptly via single drop microextraction coupled with capillary electrophoresis (CE). However, one drawback is the difficulty of keeping the single drop stably at the capillary tip. To solve this problem, we have recently demonstrated HS in-tube microextraction (ITME) of acidic compounds such as chlrophenols in an acidic sample using a basic run buffer plug in the separation capillary for CE as an acceptor phase. In this report, an organic acceptor plug in a capillary was used to extract neutral organic volatile pollutants such as BTEX (benzene, toluene, ethylbenzene, and m-xylene). After extraction, the analytes enriched in the organic acceptor plug were analyzed with micellar electrokinetic chromatography (MEKC). The enrichment factors for BTEX in a standard solution were up to 350 under an optimal condition of 25°C for 20 min. As an application, BTEX spiked into bottled water were analyzed with HS-ITME-MEKC, and the enrichment factors for BTEX were up to 320. The limits of detections were 1-4 ppb, which are at least 200 times lower than the US Environmental Protection Agency guidelines for drinking water, except benzene. The entire procedure of HS-ITME-MEKC was carried out automatically using a commercial CE instrument. PMID:26653509

  13. Matrix compatible solid phase microextraction coating, a greener approach to sample preparation in vegetable matrices.

    PubMed

    Naccarato, Attilio; Pawliszyn, Janusz

    2016-09-01

    This work proposes the novel PDMS/DVB/PDMS fiber as a greener strategy for analysis by direct immersion solid phase microextraction (SPME) in vegetables. SPME is an established sample preparation approach that has not yet been adequately explored for food analysis in direct immersion mode due to the limitations of the available commercial coatings. The robustness and endurance of this new coating were investigated by direct immersion extractions in raw blended vegetables without any further sample preparation steps. The PDMS/DVB/PDMS coating exhibited superior features related to the capability of the external PDMS layer to protect the commercial coating, and showed improvements in terms of extraction capability and in the cleanability of the coating surface. In addition to having contributed to the recognition of the superior features of this new fiber concept before commercialization, the outcomes of this work serve to confirm advancements in the matrix compatibility of the PDMS-modified fiber, and open new prospects for the development of greener high-throughput analytical methods in food analysis using solid phase microextraction in the near future. PMID:27041299

  14. Supported liquid membrane-protected molecularly imprinted fibre for solid-phase microextraction of thiabendazole.

    PubMed

    Barahona, Francisco; Turiel, Esther; Martín-Esteban, Antonio

    2011-05-23

    In this work, molecularly imprinted polymer fibres (MIP-fibre) have been prepared and evaluated for solid-phase microextraction (SPME), using thiabendazole (TBZ) as template. Inherent limitations of molecular imprinted polymers, such as target recognition in aqueous media, have been solved with the use of organic supported liquid membrane (SLM) protecting the MI-SPME process. MIP-fibres were located inside a polypropylene hollow capillary and protected by an organic solvent immobilized as a thin SLM in the pores of the capillary wall. The extraction procedure involved two simultaneous processes: liquid phase microextraction using polypropylene hollow fibres (HF-LPME) of the analytes from the sample to an organic acceptor solution through a SLM; and SPME of the analytes from the organic acceptor solution to a MIP-fibre inside the polypropylene capillary. The developed methodology was optimized and applied to the extraction of TBZ form spiked orange juices. Calibration curves showed good linearity in the concentration range under study (0.01-5.00 mg L(-1)) and a regression coefficient better than 0.995 was obtained. The detection limit was 4 μg L(-1), low enough to permit the satisfactory analysis of TBZ in real samples, according to European regulation. Relative standard deviations ranged below 10%, indicating good repeatability. By this manner, the advantages of inherent selectivity of MIP SPME fibres and the enrichment and sample cleanup capability of the HF-LPME have been successfully combined into a single device. PMID:21565306

  15. Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

    PubMed

    Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

    2013-12-20

    Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. PMID:24238710

  16. Palladium-coated stainless-steel wire as a solid-phase microextraction fiber.

    PubMed

    Sun, Min; Feng, Juanjuan; Bu, Yanan; Wang, Xiaojiao; Duan, Huimi; Luo, Chuannan

    2015-05-01

    A novel palladium solid-phase microextraction coating was fabricated on a stainless-steel wire by a simple in situ oxidation-reduction process. The palladium coating exhibited a rough microscaled surface and its thickness was about 2 μm. Preparation conditions (reaction time and concentration of palladium chloride and hydrochloric acid) were optimized in detail to achieve sufficient extraction efficiency. Extraction properties of the fiber were investigated by direct immersion solid-phase microextraction of several polycyclic aromatic hydrocarbons and phthalate esters in aqueous samples. The extracted analytes were transferred into a gas chromatography system by thermal desorption. The effect of extraction and desorption conditions on extraction efficiency were investigated. Under the optimum conditions, good linearity was obtained and correlation coefficients between 0.9908 and 0.9990 were obtained. Limits of detection were 0.05-0.10 μg/L for polycyclic aromatic hydrocarbons and 0.3 μg/L for phthalate esters. Their recoveries for real aqueous samples were in the range from 97.1 to 121% and from 89.1 to 108%, respectively. The intra- and interday tests were also investigated with three different addition levels, and satisfactory results were also obtained. PMID:25726925

  17. Capturing Plant Metabolome with Direct-Immersion in Vivo Solid Phase Microextraction of Plant Tissues.

    PubMed

    Risticevic, Sanja; Souza-Silva, Erica A; DeEll, Jennifer R; Cochran, Jack; Pawliszyn, Janusz

    2016-01-19

    For the first time, an in vivo sampling mode of direct immersion-solid phase microextraction (DI-SPME) was employed to capture the metabolome of living plant specimens, using apple (Malus × domestica Borkh.) as a model system. Metabolites were extracted from apple tissues and introduced by thermal desorption into a comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry instrument. The feasibility of this sampling approach, based on exploitation of microextraction principles, including negligible depletion of free analyte concentrations, solventless sampling and sample preparation, and on-site compatibility, was determined in global metabolite analysis. Rather than adopting an approach of traditional sample preparation, requiring metabolism quenching and laborious sample preparation, the objective of the study was to capture the metabolome in vivo, evaluate the feasibility of the approach to provide unbiased extraction coverage, and compare analytical precision when different SPME sampling modes are employed. The potential of in vivo DI-SPME in quantitative plant metabolomics was assessed by evaluating changes in metabolic fingerprints in response to fruit maturation. The in vivo SPME sampling approach has been demonstrated as capable of sampling living systems with high reproducibility, considering that nearly 50% of hundreds of evaluated compounds included in the determination of analytical performance met the 15% RSD FDA criterion. Esters were extracted with high repeatability (% RSD for hexyl butanoate and butyl butanoate of 16.5 and 5.9, respectively, from 9 determinations in 3 apples) and found to be upregulated in response to apple fruit maturation. PMID:26666307

  18. Microextraction techniques coupled to liquid chromatography with mass spectrometry for the determination of organic micropollutants in environmental water samples.

    PubMed

    Padrón, Ma Esther Torres; Afonso-Olivares, Cristina; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2014-01-01

    Until recently, sample preparation was carried out using traditional techniques, such as liquid-liquid extraction (LLE), that use large volumes of organic solvents. Solid-phase extraction (SPE) uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS) and time-of-flight mass spectrometric (TOF/MS) techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME), stir bar sorptive extraction (SBSE) and liquid-phase microextraction (LPME). Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These compounds must be

  19. Emulsification mechanism and storage instabilities of hydrocarbon-in-water sub-micron emulsions stabilised with Tweens (20 and 80), Brij 96v and sucrose monoesters.

    PubMed

    Henry, John V L; Fryer, Peter J; Frith, William J; Norton, Ian T

    2009-10-01

    The influence of both the nature of the surfactant and surfactant concentration on the processes of droplet break-up and coalescence in the formation of decane-in-water nano-emulsions in a high-pressure homogenizer was investigated. Emulsions were produced using a Christison Scientific M110-S microfluidiser with an impinging jet high-shear chamber. For all six surfactants studied (Tween 20, Tween 80, Brij 96v, sucrose monolaurate, sucrose monomyristate and sucrose monopalmate), the droplet size decreased with increasing surfactant concentration reaching a limiting droplet size at a surfactant concentration of 15 mM. The limiting droplet size for the different surfactants used were; Tween 20 (approximately 250+/-30 nm), Tween 80 (approximately 320+/-40 nm), Brij 96v (approximately 200+/-20 nm) and the three sucrose monoesters had very similar sizes of approximately 250+/-20 nm. A hydrophobic fluorescent dye (1-undecylpyrene) was used to establish the extent of competition between droplet break-up and coalescence in the emulsification process. For all the emulsifiers studied, droplet coalescence in the process reduced as the amount of emulsifier increased, becoming zero at concentrations of about 15 mM, i.e. the same concentration as that required to produce the limiting minimum droplet size. This shows that in the emulsification process droplet size is determined by both break-up and re-coalescence events, and at lower surfactant concentrations (<15 mM) that the final droplet size is probably a consequence of multiple break-up events. Emulsion stability over 200 h was investigated by measuring changes in the droplet size using dynamic light scattering. The increase in droplet volume was shown to be linear with respect to time, indicating an Ostwald ripening process. The observed ripening rate for the three sucrose monoesters (monopalmitate, monomyristate and monolaurate) was approximately 20 nm(3) s(-1), which is the ripening rate calculated using the Lifshitz

  20. Preparation and characterization of uniform-sized chitosan microspheres containing insulin by membrane emulsification and a two-step solidification process.

    PubMed

    Wang, Lian-Yan; Gu, Yong-Hong; Zhou, Qing-Zhu; Ma, Guang-Hui; Wan, Yin-Hua; Su, Zhi-Guo

    2006-07-01

    Chitosan microsphere has important application in controlled release of protein and peptide drug, because it shows excellent mucoadhesive and permeation enhancing effect across the biological surfaces. In the conventional preparation methods of chitosan microsphere, the W/O emulsion was usually prepared by mechanical stirring method, and then the droplets were solidified by glutaraldehyde. There existed limitation and shortage such as broad size distribution, de-activity of bio-drug and difficulty in drug release because protein and peptide drug have the same amino group as chitosan. In this study, we established a method to prepare uniform-sized microsphere, and solve above problems by combining a special membrane emulsification technique and a step-wise crosslinking method. That is, the chitosan/acetic acid aqueous solution was pressed through the uniform pores of a porous glass membrane into a paraffin/petroleum ether mixture containing PO-500 emulsifier, to form a W/O emulsion with uniform droplet size. Then, the uniform droplets were solidified by a two-step crosslinking method. At the first step, tripolyphosphate (TPP) solution was dropped gradually in the emulsion, TPP diffused into the droplet to crosslink chitosan by an ionic linkage, generating a microgel. At the second step, an adequate amount of glutaraldehyde was added. The solidification conditions of the two-step process were optimized by investigating the effects of solidification conditions on morphology of microspheres, encapsulation efficiency (EE), drug activity and release profile in vitro. The suitable preparative conditions were determined as follows: pH value of aqueous phase and TPP solution was 3.5-4.0, the molar ratio of amino group of chitosan to aldehyde group of glutaraldehyde was 1:1 and the crosslinking time of glutaraldehyde was 60 min. PMID:16787743

  1. Ultrasound-assisted emulsification-extraction of orange peel metabolites prior to tentative identification by LC-QTOF MS/MS.

    PubMed

    Molina-Calle, María; Priego-Capote, Feliciano; Luque de Castro, María D

    2015-08-15

    An optimized method for extraction and characterization of compounds present in orange peel has been developed. The extraction method allows the simultaneous extraction of polar and non-polar compounds by using two immiscible extractants (a polar extractant-an 80:20 (v/v) methanol-water mixture, and a non-polar extractant-n-hexane). The method is ultrasound-assisted, thus facilitating both formation of a stable emulsion between the two immiscible extractants and favoring mass-transfer from the solid sample to the liquid phases by a wide contact surface. Optimization of the ultrasound-assisted emulsification-extraction (USAEE) led to the following values as desirability conditions for both extracts: 32% amplitude, 0.75s/s duty cycle and 7.5min of extraction time. The extracts obtained under these conditions were analyzed by LC-QTOF MS/MS in positive and negative ionization modes. Tentative identification of the most significant compounds present in each extract allowed their characterization by using high resolution tandem mass spectrometry. The optimum extracts provided by USAEE were compared by using Principal Component Analysis to those obtained by conventional extraction based on maceration. Thus, the composition of the polar extracts obtained after 7.5min ultrasonication was similar to that of conventional maceration for 4h in both the ionization modes. On the contrary, the analysis of non-polar extracts led to different results depending on the ionization mode: the ultrasound-assisted extract was similar to those of conventional maceration for 10h in negative and positive ionization. This behavior could be explained by the contribution of different groups of compounds to each ionization mode. PMID:25966395

  2. Single-drop microextraction as a powerful pretreatment tool for capillary electrophoresis: A review.

    PubMed

    AlOthman, Zeid A; Dawod, Mohamed; Kim, Jihye; Chung, Doo Soo

    2012-08-20

    Single drop microextraction (SDME) is a convenient and powerful preconcentration and sample cleanup method for capillary electrophoresis (CE). In SDME, analytes are typically extracted from a sample donor solution into an acceptor drop hanging at the inlet tip of a capillary. The enriched drop is then introduced to the capillary for CE analysis. Since the volume of the acceptor drop can be as small as a few nanoliters, the consumption of solvents can be minimized and the preconcentration effect is enhanced. In addition, by covering the acceptor phase with an organic layer or by using an organic acceptor phase, inorganic ions such as salts in the sample solution can be blocked from entering the acceptor phase, providing desalting effects. Here, we describe the basic principles and instrumentation for SDME and its coupling with CE. We also review recent developments and applications of SDME-CE. PMID:22819045

  3. Headspace solid-phase microextraction analysis of volatile components in Phalaenopsis Nobby's Pacific Sunset.

    PubMed

    Yeh, Chih-Hsin; Tsai, Wan-Yu; Chiang, Hsiu-Mei; Wu, Chin-Sheng; Lee, Yung-I; Lin, Li-Yun; Chen, Hsin-Chun

    2014-01-01

    Phalaenopsis is the most important economic crop in the Orchidaceae family. There are currently numerous beautiful and colorful Phalaenopsis flowers, but only a few species of Phalaenopsis have an aroma. This study reports the analysis volatile components present in P. Nobby's Pacific Sunset by solid-phase microextraction (SPME) coupled with gas chromatography (GC) and gas chromatography/mass spectrometry (GC-MS). The results show that the optimal extraction conditions were obtained by using a DVB/CAR/PDMS fiber. A total of 31 compounds were identified, with the major compounds being geraniol, linalool and α-farnesene. P. Nobby's Pacific Sunset had the highest odor concentration from 09:00 to 13:00 on the eighth day of storage. It was also found that in P. Nobby's Pacific Sunset orchids the dorsal sepals and petals had the highest odor concentrations, whereas the column had the lowest. PMID:25207714

  4. Improvements in the vapor-time profile analysis of explosive odorants using solid-phase microextraction.

    PubMed

    Young, Mimy; Schantz, Michele; MacCrehan, William

    2016-07-15

    A modified approach for characterization of the vapor-time profile of the headspace odors of explosives was developed using solid-phase microextraction (SPME) incorporating introduction of an externally-sampled internal standard (ESIS) followed by gas chromatography/mass spectrometry (GC/MS) analysis. With this new method, reproducibility of the measurements of 2-ethyl-1-hexanol and cyclohexanone were improved compared to previous work (Hoffman et al., 2009; Arthur and Pawliszyn, 1990) through the use of stable-isotope-labeled internal standards. Exposing the SPME fiber to the ESIS after sampling the target analyte proved to be advantageous, while still correcting for fiber variability and detector drift. For the analysis of high volatility compounds, incorporation of the ESIS using the SPME fiber in the retracted position minimized the subsequent competitive loss of the target analyte, allowing for much longer sampling times. PMID:27286650

  5. A novel hybrid metal-organic framework-polymeric monolith for solid-phase microextraction.

    PubMed

    Lin, Chen-Lan; Lirio, Stephen; Chen, Ya-Ting; Lin, Chia-Her; Huang, Hsi-Ya

    2014-03-17

    This study describes the fabrication of a novel hybrid metal-organic framework- organic polymer (MOF-polymer) for use as a stationary phase in fritless solid-phase microextraction (SPME) for validating analytical methods. The MOF-polymer was prepared by using ethylene dimethacrylate (EDMA), butyl methacrylate (BMA), and an imidazolium-based ionic liquid as porogenic solvent followed by microwave-assisted polymerization with the addition of 25 % MOF. This novel hybrid MOF-polymer was used to extract penicillin (penicillin G, penicillin V, oxacillin, cloxacillin, nafcillin, dicloxacillin) under different conditions. Quantitative analysis of the extracted penicillin samples using the MOF-organic polymer for SPME was conducted by using capillary electrochromatography (CEC) coupled with UV analysis. The penicillin recovery was 63-96.2 % with high reproducibility, sensitivity, and reusability. The extraction time with the proposed fabricated SPME was only 34 min. PMID:24615770

  6. Silica-fiber microextraction for laser desorption ion trap mass spectrometry

    SciTech Connect

    Cisper, M.E.; Earl, W.L.; Nogar, N.S.; Hemberger, P.H. )

    1994-06-01

    We have coupled sample collection by solid-phase microextraction on disposable fused silica optical fibers with analysis by laser desorption ion trap mass spectrometry for rapid screening of organic contaminants in complex matrices. Because the silica-fiber probe serves as both the sampling medium and the sample support for laser desorption, traditional methods of sample preparation are eliminated with the expected gains in speed and simplicity. Pyrene was the benchmark compound in these experiments but we show that the technique is also applicable to other polycyclic aromatic hydrocarbons (PAHs) and semivolatile compounds, laser dyes, pesticides, and peptides. Derivatizing the silica fiber improves the analyte collection efficiency, and firing the laser during a ring electrode rf ramp promotes dependable trapping of laser-desorbed ions. 32 refs., 5 figs.

  7. A novel silver-coated solid-phase microextraction metal fiber based on electroless plating technique.

    PubMed

    Feng, Juanjuan; Sun, Min; Li, Jubai; Liu, Xia; Jiang, Shengxiang

    2011-09-01

    A novel silver-coated solid-phase microextraction fiber was prepared based on electroless plating technique. Good extraction performance of the fiber for model compounds including phthalate esters (dibutyl phthalate, dioctyl phthalate, dicyclohexyl phthalate and diallyl phthalate) and polycyclic aromatic hydrocarbons (naphthalene, fluorene, phenanthrene, fluoranthene) in aqueous solution was obtained. Under the optimized conditions (extraction temperature, extraction time, ionic strength and desorption temperature), the proposed SPME-GC method showed wide linear ranges with correlation coefficients (R(2)) ranging from 0.9745 to 0.9984. The limits of detection were at the range of 0.02 to 0.1 μg L(-1). Single fiber repeatability and fiber-to-fiber reproducibility as well as stability to acid, alkali and high temperature were studied and the results were all satisfactory. The method was applied successfully to the aqueous extracts of disposable paper cup and instant noodle barrel. Several kinds of analytes were detected and quantified. PMID:21801885

  8. A digital microfluidic interface between solid-phase microextraction and liquid chromatography-mass spectrometry.

    PubMed

    Choi, Kihwan; Boyacı, Ezel; Kim, Jihye; Seale, Brendon; Barrera-Arbelaez, Luis; Pawliszyn, Janusz; Wheeler, Aaron R

    2016-04-29

    We introduce a method to couple solid-phase microextraction (SPME) with HPLC-MS using digital microfluidics (DMF). In the new system, SPME fibers are used to extract analytes from complex sample solutions, after which the analytes are desorbed into solvent droplets in a DMF device. The open geometry of DMF allows straightforward insertion of SPME fibers without requiring a complicated interface, and automated droplet manipulation enables multiplexed processing of the fibers. In contrast to other multiplexed SPME elution interfaces, the low volumes inherent to DMF allow for pre-concentration of analytes prior to analysis. The new SPME-DMF-HPLC-MS method was applied to the quantification of pg/mL-level free steroid hormones in urine. We propose that this new method will be useful for a wide range of applications requiring cleanup and pre-concentration with convenient coupling to high-performance analytical techniques. PMID:27048987

  9. Molecularly imprinted calixarene fiber for solid-phase microextraction of four organophosphorous pesticides in fruits.

    PubMed

    Li, Jing-Wen; Wang, Yu-Long; Yan, Shan; Li, Xiu-Juan; Pan, Si-Yi

    2016-02-01

    Calixarene was used as a functional monomer to fabricate a molecularly imprinted polymer (MIP) by sol-gel technique for solid-phase microextraction (SPME) of parathion-methyl and its structural analogs. The MIP-coated fiber possessed excellent thermal and chemical stability as well as high extraction capacity. Its selectivity and possible recognition mechanism were investigated. The similarities in molecular shape and functional group play a key role in the selective recognition of the imprinted material. Any changes to the structure of the template would decrease the imprinting factor. A comparison of MIP-SPME was made with liquid-liquid extraction coupled with gas chromatography for the determination of organophosphorus pesticides (OPPs) in fruits. Much lower limits of detection and better recoveries were achieved by SPME in spiked apple and pineapple samples. The experiment demonstrates that the proposed method using the calixarene MIP fiber was more suitable for selective determination of trace OPPs in those fruit samples. PMID:26304345

  10. Headspace-single drop microextraction with a commercial capillary electrophoresis instrument.

    PubMed

    Park, Sung Tai; Kim, Jihye; Choi, Kihwan; Lee, Hye Ryeo; Chung, Doo Soo

    2012-10-01

    Automated coupling of headspace-single drop microextraction (HS-SDME) and CE has been demonstrated using a commercial CE instrument. When a drop hanging at the inlet tip of a capillary for CE is used as the acceptor phase, HS-SDME becomes a simple but powerful sample pretreatment technique for CE before injection to facilitate sample cleanup and enrichment. By combining HS-SDME with an on-line sample preconcentration technique, large volume sample stacking using an electroosmotic flow pump, the sensitivity can be improved further. The overall enrichment factors for phenolic compounds were from 1900 to 3400. HS-SDME large volume sample stacking using an electroosmotic flow pump was successfully applied to a red wine sample to obtain an LOD of 4 nM (0.8 ppb) for 2,4,6-trichlorophenol which is a precursor for 2,4,6-trichloroanisole causing the foul odor in wine called cork taint. PMID:23015463

  11. Quantitative determination of geosmin in red beets (Beta vulgaris L.) using headspace solid-phase microextraction.

    PubMed

    Lu, Guiping; Fellman, John K; Edwards, Charles G; Mattinson, D Scott; Navazio, John

    2003-02-12

    An improved analytical method for the determination of geosmin in red beets was developed using headspace solid-phase microextraction (HSPME). Volatiles of beet juice were extracted in headspace for 2 h using a polydimethylsiloxane/divinylbenzene fiber, thermally desorbed from the fiber, and analyzed by gas chromatography. The HSPME method was determined to be suitable for geosmin analysis as evidenced by high relative recovery (99.2%), low relative standard deviation (7.48%), and reasonable detection limit (1 microg/kg of beet root tissue). The concentrations of geosmin in four beet cultivars ranged from 9.69 +/- 0.22 to 26.7 +/- 0.27 microg/kg, depending on cultivar. PMID:12568566

  12. Nanoporous Conducting Polymer-Based Coatings in Microextraction Techniques for Environmental and Biomedical Applications.

    PubMed

    Szultka-Mlynska, Malgorzata; Olszowy, Pawel; Buszewski, Bogusław

    2016-05-01

    Biologically active compounds constitute a wide group of chemicals, therefore it is a big challenge to create sorbents that are sensitive as well as selective. Development of nanoporous sorbents based on conducting polymers has expanded the boundaries of detection and quantification. Additionally, electrochemical synthesis used to deposit polymeric coatings directly on solid supports makes it possible to control physico-chemical properties of such sorbents. Besides the development of new polymeric nanoporous materials, the question of selectivity needs to be addressed. One possibility, successfully adapted to solid-phase microextraction, is molecular imprinting. Coatings created with this technology allow obtaining higher selectivity, with sensitivity at a constantly high level. The main aim of this review is to present comprehensively the concept of nanoporous sorbents based on conducting polymers, possible coating methods with their characteristics, and their various applications. This article focuses on applications in environmental and biomedical analyses. PMID:26322903

  13. A highly efficient three-phase single drop microextraction technique for sample preconcentration.

    PubMed

    Jahan, Sharmin; Xie, Haiyang; Zhong, Ran; Yan, Jian; Xiao, Hua; Fan, Liuyin; Cao, Chengxi

    2015-05-01

    A highly efficient three-phase single drop microextraction (SDME) method is presented by using an organic-aqueous compound droplet. A coupling microdevice is designed to produce compound droplets in different sizes conveniently. In this way, the volume ratio of organic phase to aqueous phase in a compound droplet can be significantly reduced. Good operability and droplet stability were observed during extraction under vigorous stirring conditions. Five statins were used as model compounds and spiked in river water and human serum samples to evaluate the analytical performance of the proposed method. By using a 1.2 μL toluene-aqueous compound droplet (volume ratio 0.2 : 1), a 350 to 1712 fold enrichment of statins was obtained within 4 minutes. The results indicate that the proposed method is a very rapid and efficient sample pretreatment method, and is promising for automated and high-throughput applications. PMID:25756087

  14. Characterization and semiquantitative analysis of volatiles in seedless watermelon varieties using solid-phase microextraction.

    PubMed

    Beaulieu, John C; Lea, Jeanne M

    2006-10-01

    Seedless triploid watermelons have increased in popularity since the early 1990s, and the demand for seedless fruit is on the rise. Sweetness and sugars are crucial breeding focuses for fruit quality. Volatiles also play an important role; yet, we found no literature for seedless varieties and no reports using solid-phase microextraction (SPME) in watermelon. The objective of this experiment was to identify volatile and semivolatile compounds in five seedless watermelon varieties using carboxen divinylbenzene polydimethylsiloxane solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS). Fully ripe watermelon was squeezed through miracloth to produce rapid juice extracts for immediate headspace SPME GC-MS. Aldehydes, alcohols, ketones, and one furan (2-pentyl furan, a lipid oxidation product) were recovered. On the basis of total ion count peak area, the most abundant compounds in five varieties were 3-nonen-1-ol/(E,Z)-2,6-nonadienal (16.5-28.2%), (E)-2-nonenal (10.6-22.5%), and (Z)-6-nonenal (2.0-11.3%). Hexanal was most abundant (37.7%) in one variety (Petite Perfection) [corrected] The most abundant ketone was 6-methyl-5-hepten-2-one (2.7-7.7%). Some sensory attributes reported for these compounds are melon, citrus, cucumber, orange, rose, floral, guava, violet, vegetable, green, grassy, herbaceous, pungent, fatty, sweet, and waxy. Identifying and relating these compounds to sensory attributes will allow for future monitoring of the critical flavor compounds in seedless watermelon after processing and throughout fresh-cut storage. PMID:17002453

  15. Cold fiber solid-phase microextraction device based on thermoelectric cooling of metal fiber.

    PubMed

    Haddadi, Shokouh Hosseinzadeh; Pawliszyn, Janusz

    2009-04-01

    A new cold fiber solid-phase microextraction device was designed and constructed based on thermoelectric cooling. A three-stage thermoelectric cooler (TEC) was used for cooling a copper rod coated with a poly(dimethylsiloxane) (PDMS) hollow fiber, which served as the solid-phase microextraction (SPME) fiber. The copper rod was mounted on a commercial SPME plunger and exposed to the cold surface of the TEC, which was enclosed in a small aluminum box. A heat sink and a fan were used to dissipate the generated heat at the hot side of the TEC. By applying an appropriate dc voltage to the TEC, the upper part of the copper rod, which was in contact to the cold side of the TEC, was cooled and the hollow fiber reached a lower temperature through heat transfer. A thermocouple was embedded in the cold side of the TEC for indirect measurement of the fiber temperature. The device was applied in quantitative analysis of off-flavors in a rice sample. Hexanal, nonanal, and undecanal were chosen as three off-flavors in rice. They were identified according to their retention times and analyzed by GC-flame ionization detection instrument. Headspace extraction conditions (i.e., temperature and time) were optimized. Standard addition calibration graphs were obtained at the optimized conditions and the concentrations of the three analytes were calculated. The concentration of hexanal was also measured using a conventional solvent extraction method (697+/-143ng/g) which was comparable to that obtained from the cold fiber SPME method (644+/-8). Moreover, the cold fiber SPME resulted in better reproducibility and shorter analysis time. Cold fiber SPME with TEC device can also be used as a portable device for field sampling. PMID:18814881

  16. A highly thermal stable solid phase microextraction fiber prepared by an inorganic binder.

    PubMed

    Liu, Hongmei; Ran, Fanpeng; Tao, Caihong; Zhao, Mengmeng; Jia, Yulong; Guo, Yong

    2016-04-28

    An easy method to prepare solid phase microextraction fibers by introducing an inorganic binder was demonstrated in this study, where MoS2 was selected as the extraction phase material because of its graphite-like layered structure with large specific adsorption area and good stability, and was then adhered to a stainless steel wire by acid aluminum phosphate binder with the spraying method. The as-prepared solid phase microextraction fiber coupled with gas chromatography was then used to extract some polycyclic aromatic hydrocarbons target analytes including the low-volatile benzo(a)pyrene etc. from a standard sample. Comparing with the MoS2-epoxy resin and commercial polyacrylate fibers, the MoS2-acid aluminum phosphate fiber has a higher thermal stability because of highly thermal stable acid aluminum phosphate, which is durable for a long service life at a high temperature (320 °C), and has the advantage in the extraction of low-volatility analytes. After the optimization of adsorption and desorption factors (ionic strength, adsorption time and temperature, and desorption temperature), method detection limits of <0.1 μg L(-1) were achieved, and the calibration curves were all linear (R(2) ≥ 0.9981) within the range of 0.1-100 μg L(-1). The satisfying repeatability was also achieved, the RSD values of single-fiber were 3.49-5.81%, and the ones of fiber-to-fiber were 5.32-7.22%. As a result, the present fiber with good thermal stability can work at high temperature for a long service life, which is useful for the detection of low-volatility target analytes in practical applications. PMID:27046208

  17. Determination of selected pharmaceutical residues in wastewater using an automated open bed solid phase microextraction system.

    PubMed

    Togunde, Oluranti P; Cudjoe, Erasmus; Oakes, Ken D; Mirnaghi, Fatemah S; Servos, Mark R; Pawliszyn, Janusz

    2012-11-01

    The detection of trace levels of pharmaceuticals in environmental matrices requires an analyte pre-concentration procedure to obtain the required sensitivity for quantitative determination. This research aims to develop a simple automated analytical method based on C(18) thin film solid phase microextraction (TF-SPME) for the simultaneous extraction of pharmaceutical compounds detected in surface waters. As a sample preparation method, solid phase microextraction, is a rapid, environmentally friendly, and a sensitive analytical technique which isolates and pre-concentrates trace organic pollutants from environmental water samples in a single step. High throughput analysis was achieved with the use of a robotic auto sampler which enabled parallel analyte extraction in a 96-well plate format. Application of the method was demonstrated using wastewater from pilot-scale municipal treatment plants and environmental water samples from wastewater-dominated reaches of the Grand River (adjacent Waterloo, ON) which were analysed using a liquid chromatography-mass spectrometry (LC-ESI-MS/MS) technique. The proposed method successfully determined concentrations of carbamazepine, fluoxetine, sertraline, and paroxetine in treated effluent at concentrations ranging from 240 to 3820 ng/L with a method detection limit of 2-13 ng/L with a relative standard deviation of less than 16%. Matrix effect was not observed with this method; therefore internal standards are not necessary for quantification of target compounds. The results suggest that this method is capable of detecting and quantifying many compounds present in both wastewater and wastewater-influenced surface water from multiple municipal sources. In this study, automated TF-SPME system is demonstrated as a simple and fast alternative method for high throughput analysis of pharmaceutical contaminants in environmental matrices. PMID:22999422

  18. A metal organic framework-polyaniline nanocomposite as a fiber coating for solid phase microextraction.

    PubMed

    Bagheri, Habib; Javanmardi, Hasan; Abbasi, Alireza; Banihashemi, Solmaz

    2016-01-29

    A metal organic framework-polyaniline (MOF/PANI) nanocomposite was electrodeposited on a stainless steel wire and used as a solid phase microextraction (SPME) fiber coating. The electropolymerization process was carried out under a constant deposition potential and applied to the corresponding aqueous electrolyte containing aniline and MOF particles. The employment of MOFs with their large and small cages and 3-D structures in synthesizing a nanocomposite was assumed to be efficient constitutes to induce more non-smooth and porous structures, approved by scanning electron microscopy (SEM) images. Three different MOFs were incorporated to synthesize the desired nanocomposites and the preliminary experiments showed that all of them, particularly the one containing MOF2, have higher extraction performances in compared with PANI. The applicability of the new fiber coating was examined by headspace-solid phase microextraction (HS-SPME) of some chlorobenzenes (CBs) from aqueous samples. Influencing parameters on the synthesize and extraction processes including the electrodeposition voltage and its duration time, the weight ratio of PANI and MOF, the ionic strength, desorption temperature and time, and extraction time and temperature were optimized. The developed method was validated by analyzing the spiked distilled water and gas chromatography-mass spectrometry (GC-MS). Under optimum condition, the relative standard deviation (RSD%) values for a double distilled water spiked with the selected CBs at 20ngL(-1) were 5-8% (n=3) and the detection limits were below 0.2ngL(-1). The linear dynamic range (LDR) of the method was in the concentration range of 0.5-1000ngL(-1) (R(2)>0.9994). The fiber-to-fiber reproducibility was found to be in the range of 4-7%. Eventually, various real-water samples were analyzed by the MOF/PANI-based HS-SPME and GC-MS and the relative recovery values were found to be in the range of 92-98%. PMID:26792446

  19. Aniline-silica nanocomposite as a novel solid phase microextraction fiber coating.

    PubMed

    Bagheri, Habib; Roostaie, Ali

    2012-05-18

    A new unbreakable solid phase microextraction (SPME) fiber coating based on aniline-silica nanocomposite was electrodeposited on a stainless steel wire. The electropolymerization process was carried out at a constant deposition potential, applied to the corresponding aqueous electrolyte containing aniline and silica nanoparticles. The scanning electron microscopy (SEM) images showed the non-smooth and the porous surface structure of the prepared nanocomposite. The applicability of the new fiber coating was examined by headspace-solid phase microextraction (HS-SPME) of some environmentally important polycyclic aromatic hydrocarbons (PAHs), as model compounds, from aqueous samples. Subsequently, the extracted analytes were transferred into a gas chromatography (GC) by thermal desorption. Parameters affecting the synthesizing and extraction processes including the voltage of power supply, the weight ratio of components, the time of electrodeposition, extraction time and temperature, the ionic strength, and desorption temperature and time were optimized. Eventually, the developed method was validated by gas chromatography-mass spectrometry (GC-MS). At the optimum conditions, the relative standard deviation (%RSD) values for a double distilled water spiked with the selected PAHs at 40 ng L(-1) were 6-13% (n=3) while the limit of detection (LOD) results were between 1 and 3 ng L(-1). The calibration graphs were linear in the concentration range from 20 to 4000 ng L(-1) (R(2)>0.995). Finally the developed method was applied to the analysis of Kalan dam, rain and tap water samples and the relative recovery values were found to be in the range of 76-109%, under optimized conditions. In addition, the synthesis of the nanocomposite coating was carried out conveniently while it is rather inexpensive, easy, simple, rapid and highly durable and can be used frequently. PMID:22498354

  20. Automated hollow-fiber liquid-phase microextraction followed by liquid chromatography with mass spectrometry for the determination of benzodiazepine drugs in biological samples.

    PubMed

    Nazaripour, Ali; Yamini, Yadollah; Ebrahimpour, Behnam; Fasihi, Javad

    2016-07-01

    In this study, two-phase hollow-fiber liquid-phase microextraction and three-phase hollow-fiber liquid-phase microextraction based on two immiscible organic solvents were compared for extraction of oxazepam and Lorazepam. Separations were performed on a liquid chromatography with mass spectrometry instrument. Under optimal conditions, three-phase hollow-fiber liquid-phase microextraction based on two immiscible organic solvents has a better extraction efficiency. In a urine sample, for three-phase hollow fiber liquid-phase microextraction based on two immiscible organic solvents, the calibration curves were found to be linear in the range of 0.6-200 and 0.9-200 μg L(-1) and the limits of detection were 0.2 and 0.3 μg L(-1) for oxazepam and lorazepam, respectively. For two-phase hollow fiber liquid-phase microextraction, the calibration curves were found to be linear in the range of 1-200 and 1.5-200 μg L(-1) and the limits of detection were 0.3 and 0.5 μg L(-1) for oxazepam and lorazepam, respectively. In a urine sample, for three-phase hollow-fiber-based liquid-phase microextraction based on two immiscible organic solvents, relative standard deviations in the range of 4.2-4.5% and preconcentration factors in the range of 70-180 were obtained for oxazepam and lorazepam, respectively. Also for the two-phase hollow-fiber liquid-phase microextraction, preconcentration factors in the range of 101-257 were obtained for oxazepam and lorazepam, respectively. PMID:27144369

  1. Tandem air-agitated liquid-liquid microextraction as an efficient method for determination of acidic drugs in complicated matrices.

    PubMed

    Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Asghari, Alireza; Hemmati, Maryam

    2016-04-21

    A rapid and simple microextraction method with a high sample clean-up, termed as tandem air-agitated liquid-liquid microextraction (TAALLME), is described. This method is based upon the tandem implementation of the air-agitated liquid-liquid microextraction (AALLME), and this approach improves the applicability of the dispersive liquid-liquid microextraction (DLLME) methods in complicated matrices. With very simple tools, the three non-steroidal anti-inflammatory drugs diclofenac, ibuprofen, and mefenamic acid were efficiently extracted, with an overall extraction time of 7 min. By performing the first AALLME, these acidic analytes, contained in an aqueous sample solution (donor phase, 8.0 mL), were extracted into the organic solvent (1,2-dichloroethane, 37 μL), and their simple back-extraction into the aqueous acceptor solution (pH, 10.01, 51 μL) was obtained in 2 min by a second implementation of AALLME. Response surface methodology (RSM) was used for optimization of the experimental parameters. The pH values 2.94 and 10.01 were obtained for the donor and acceptor phases, respectively, and the volumes 99.5 and 51 μL were obtained for the organic solvent and the acceptor phase, respectively, as the optimal extraction conditions. Under the optimized conditions, tandem AALLME-HPLC-UV provided a good linearity in the range of 0.5-4000 ng mL(-1), limits of detection (0.1-0.3 ng mL(-1)), extraction repeatabilities (relative standard deviations (RSDs) below 7.7%, n = 5), and the enrichment factors (EFs) of 80-104. Finally, the applicability of the proposed method was evaluated by the extraction and determination of the drugs under study in the wastewater and human plasma samples. PMID:27026599

  2. Ionic-liquid-based dispersive liquid-liquid microextraction for high-throughput multiple food contaminant screening.

    PubMed

    Ho, Yee-Man; Tsoi, Yeuk-Ki; Leung, Kelvin Sze-Yin

    2013-12-01

    This paper describes an innovation of dispersive liquid-liquid microextraction enabling multiple-component analysis of eight high-priority food contaminants in two chemically distinctive families: Sudan dyes and phthalate plasticizers. To provide convenient sample handling for solid and solid-containing matrices, a modified dispersive liquid-liquid microextraction procedure used an extractant precoated frit to perform simultaneous filtration, solvent mixing, and phase dispersion in one simple step. A binary ionic liquid extractant system was carefully tuned to deliver high quality analysis based only on affordable LC with diode array detector instrumentation. The method is comprehensively validated for robust quantification with good precision (6.9-9.8% RSD) in a linear 2-1000 μg/L range. Having accomplished enrichment factors up to 451, the treatment enables sensitive detection at 0.09-1.01 μg/L levels. Analysis of six high-risk solid condiments and sauces further verified its practical applicability within a 70-120% recovery range. Compared to other approaches, the current dispersive liquid-liquid microextraction treatment offers major advantages in terms of minimal solvent (1.5 mL) and sample (0.1 g) consumption, ultra-high analytical throughput (6 min), and the ability to handle complex solid matrices. The idea of performing simultaneous analysis for multiple contaminants presented here fosters a more effective mode of operation in food control routines. PMID:24039178

  3. Using dispersive liquid-liquid microextraction and liquid chromatography for determination of guaifenesin enantiomers in human urine.

    PubMed

    Hatami, Mehdi; Farhadi, Khalil; Abdollahpour, Assem

    2011-11-01

    A simple, rapid, and efficient method, dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography-fluorescence detector, has been developed for the determination of guaifenesin (GUA) enantiomers in human urine samples after an oral dose administration of its syrup formulation. Urine samples were collected during the time intervals 0-2, 2-4, and 4-6 h and concentration and ratio of two enantiomers was determined. The ratio of R-(-) to S-(+) enantiomer concentrations in urine showed an increase with time, with R/S ratios of 0.66 at 2 h and 2.23 at 6 h. For microextraction process, a mixture of extraction solvent (dichloromethane, 100 μL) and dispersive solvent (THF, 1 mL) was rapidly injected into 5.0 mL diluted urine sample for the formation of cloudy solution and extraction of enantiomers into the fine droplets of CH(2)Cl(2). After optimization of HPLC enantioselective conditions, some important parameters, such as the kind and volume of extraction and dispersive solvents, extraction time, temperature, pH, and salt effect were optimized for dispersive liquid-liquid microextraction process. Under the optimum extraction condition, the method yields a linear calibration curve in the concentration range from 10 to 2000 ng/mL for target analytes. LOD was 3.00 ng/mL for both of the enantiomers. PMID:21972192

  4. Comparison of three different solid-phase microextraction fibres for analysis of essential oils in yacon (Smallanthus sonchifolius) leaves.

    PubMed

    Adam, M; Juklová, M; Bajer, T; Eisner, A; Ventura, K

    2005-08-19

    A headspace solid-phase microextraction (HS-SPME) procedure based on three commercialised fibers (100 microm polydimethylsiloxane, 65 microm polydimethylsiloxane-divinylbenzene and 50/30 microm divinylbenzene-Carboxen-polydimethylsiloxane) is presented for the determination of a selected essential oils in dried leaves of yacon (Smallanthus sonchifolius). The extraction performances of these compounds were compared using fibers with one, two and three coatings. The optimal experimental procedures for the adsorption and desorption of target compounds were determined. Significant parameters affecting sorption process such as sample weight, sorption and desorption time and temperature were optimised and discussed. Finally, the optimised procedures were applied successfully for the determination of these compounds in various yacon species. The relative concentration factors of three characteristic components of yacon were measured for relative evaluation of the fiber efficiency. Main essential oils were isolated from dried yacon leaves by appropriate solid-phase microextraction fiber and semi-quantitative analysis of the target volatiles was conducted by gas chromatography-flame ionisation detection (GC-FID) using a capillary column. Three compounds--beta-pinene, caryophylene and y-cadinene were found as the predominant essential oils. Its relative content was important for specification of yacon varieties. Solid-phase microextraction in combination with gas chromatography enabled a rapid and simple determination of relative content of essential oils in yacon. PMID:16114228

  5. Study of enrichment factors for six β-blockers in aliphatic alcohols by hollow-fiber liquid-phase microextraction.

    PubMed

    Li, Qing-Lian; Jing, Shao-Jun; Zhang, Jin-Feng; Zhang, Lin; Ran, Cong-Cong; Du, Chao-Hui; Jiang, Ye

    2015-10-01

    The selectivity of a suitable organic solvent is key for extraction in liquid-phase microextraction experiments. Nevertheless, the screening process remains a daunting task. Our research aimed to study the relationship between extraction efficiency and extraction solvents, analytes, and finally select the appropriate extraction solvent. In the present article, β-blockers and six extraction solvents were chosen as the models and hollow-fiber liquid-phase microextraction was conducted. The relationship was built by statistical analysis on the data. Factors affecting extraction efficiency including the logarithms of the octanol/water partition coefficient (logPo/w ) of analytes, acid dissociation constants, the logarithms of the octanol/water partition coefficient of solvents and pH of the sample solution were investigated. The results showed that a low water solubility of extraction solvent is the foundation to ensure higher extraction efficiency. Moreover, when ΔlogPo/w > 0, a higher extraction efficiency is observed at lower ΔlogPo/w , on the contrary, when ΔlogPo/w < 0, extraction efficiency is higher as the absolute value of ΔlogPo/w becomes greater. Finally, the relationship between enrichment factor and extraction solvents, analytes was established and a helpful guidance was provided for the selection of an optimal solvent to obtain the best extraction efficiency by liquid-phase microextraction. PMID:26224511

  6. Optimization of a derivatization-solid-phase microextraction method for the analysis of thirty phenolic pollutants in water samples.

    PubMed

    Llompart, Maria; Lourido, Mercedes; Landin, Pedro; García-Jares, Carmen; Cela, Rafael

    2002-07-19

    Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry has been applied to the extraction of 30 phenol derivatives from water samples. Analytes were in situ acetylated and headspace solid-phase microextraction was performed. Different parameters affecting extraction efficiency were studied. Optimization of temperature, type of microextraction fiber and volume of sample has been done by means of a mixed-level categorical experimental design, which allows to study main effects and second order interactions. Five different fiber coatings were employed in this study; also, extraction temperature was studied at three levels. Both factors, fiber coating and extraction temperature, were important to achieve high sensitivity. Moreover, these parameters showed a significant interaction, which indicates the different kinetic behavior of the SPME process when different coatings are used. It was found that 75 microm carboxen-polydimethylsiloxane and 100 microm polydimethylsiloxane, yield the highest responses. The first one is specially appropriated for phenol, methylphenols and low chlorinated chlorophenols and the second one for highly chlorinated phenols. The two methods proposed in this study shown good linearity and precision. Practical applicability was demonstrated through the analysis of a real sewage water sample, contaminated with phenols. PMID:12187964

  7. Microextraction techniques for the non-chromatographic speciation of ultratraces of elements in waters: some significant cases

    NASA Astrophysics Data System (ADS)

    Lopez-Garcia, Ignacio; Vicente-Martinez, Yesica; Hernandez-Cordoba, Manuel; Martínez-Sanchez, Maria Jose; Perez-Sirvent, Carmen

    2015-04-01

    The speciation of very low concentrations of some elements in waters is of interest due to the different behaviour and toxicity the species can have. This task can be carried out by using liquid chromatographic techniques (LC) for separation together with inductively coupled plasma mass spectrometry (ICP-MS) for detection. However, this combination is not easily available in all laboratories mainly due to the relative high cost of acquisition and maintenance of the ICP-MS spectrometer, and so other alternatives are of practical interest. Present knowledge of microextraction techniques involving minimal (or none) amounts of organic solvents allows, in some cases, speciation to be carried out without the need of such an expensive instrument, and even avoiding the use of a chromatographic stage. The selectivity of the separation (fractionation or speciation) can be achieved by modifying the experimental conditions used for microextraction, and a sensitive final measurement be obtained by means of electrothermal atomic absorption spectrometry (ETAAS). In this way, since an ETAAS instrument is common (and sometimes underused) in all laboratories, the speciation procedures are made available to most laboratories worldwide. The high preconcentration factor achieved by means of the microextraction stage together with the high sensitivity inherent in ETAAS measurements result in extremely sensitive methods that permit the speciation at ultratrace levels. The advantages of this methodology are presented by discussing speciation of chromium and arsenic as representative examples.

  8. Determination of arsenic and selenium by hydride generation and headspace solid phase microextraction coupled with optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Tyburska, Anna; Jankowski, Krzysztof; Rodzik, Agnieszka

    2011-07-01

    A hydride generation headspace solid phase microextraction technique has been developed in combination with optical emission spectrometry for determination of total arsenic and selenium. Hydrides were generated in a 10 mL volume septum-sealed vial and subsequently collected onto a polydimethylsiloxane/Carboxen solid phase microextraction fiber from the headspace of sample solution. After completion of the sorption, the fiber was transferred into a thermal desorption unit and the analytes were vaporized and directly introduced into argon inductively coupled plasma or helium microwave induced plasma radiation source. Experimental conditions of hydride formation reaction as well as sorption and desorption of analytes have been optimized showing the significant effect of the type of the solid phase microextraction fiber coating, the sorption time and hydrochloric acid concentration of the sample solution on analytical characteristics of the method developed. The limits of detection of arsenic and selenium were 0.1 and 0.8 ng mL - 1 , respectively. The limit of detection of selenium could be improved further using biosorption with baker's yeast Saccharomyces cerevisiae for analyte preconcentration. The technique was applied for the determination of total As and Se in real samples.

  9. Nanoparticles decorated with a Schiff's base for the microextraction of Cd, Pb, Ni, and Co in environmental samples.

    PubMed

    Shah, Faheem; Naeemullah; Shah, Muhammad Raza; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Kiramat

    2016-05-01

    In this paper, we report a new liquid-liquid microextraction procedure called "nanoparticles decorated with a Schiff's base for the microextraction of Cd, Pb, Ni, and Co in environmental samples". The developed procedure was utilized for the extraction of Cd, Pb, Ni, and Co in environmental samples. The Schiff's base was formed by reacting salicylaldehyde with 3-aminopropyltriethoxysilane-functionalized iron oxide nanoparticles. Analyte extraction was conducted in a capillary column system loaded with modified nanoparticles and triton X-114 as dispersion medium. 1-Butyl-3-methylimidazolium hexafluorophosphate was employed as an extraction solvent. Acidified methanol in ultrasonic bath was used as desorption solvent, and elemental determination was carried out with flame atomic absorption spectrometer. Characterization of modified nanoparticles was performed with FTIR spectroscopy and transmission electron microscopy. Solution pH, nanoparticles amount, dispersant concentration, ionic liquid, and temperature were optimized for the extraction. Detection limits obtained for Cd, Pb, Ni, and Co were 0.183, 0.201, 0.241, and 0.192 μg L(-1), respectively, and enhancement factors were 79.1, 86.4, 95.7, and 82.0, respectively. The reproducibility of the developed procedure was in the range of 3.98-5.10%. Validation was checked by applying the developed procedure on certified reference water samples. The microextraction based on nanoparticles decorated with Schiff's base was successfully applied for the extraction of Cd, Pb, Ni, and Co in real environmental water samples. PMID:27187842

  10. Multivariate optimization of "In capillary-Schiff's base functionalized magnetic nanoparticle based microextraction" of Pb(+2): A novel synergistic approach.

    PubMed

    Shah, Faheem; Muhammad, Haji; Naeemullah; Ullah, Azeem

    2016-07-01

    A novel microextraction procedure based on Schiff's base functionalized magnetic nanoparticles (SBMNPs) has been developed for Pb(+2) extraction. Compared to conventional microextraction systems, the main advantage of proposed procedure is that no volatile/flammable reagents have used and experimental time is also reduced. Schiff's base has been derived from salicylaldehyde and 3-aminopropyltriethoxysilane modified nanoparticles. Extraction of Pb(+2) was carried out in a capillary column containing analyte followed by the addition of SBMNPs and triton X-114 where ionic-liquid "1-Butyl-3-methylimidazolium hexafluorophosphate" was used as an extractant. After extraction; analyte concentration was determined with flame atomic absorption spectrometer through a self made micro-injection system. The SBMNPs were characterized by FTIR and TEM, respectively, demonstrating their distinct core-shell structures. Different experimental parameters were optimized through multivariate strategy. Detection limit, enhancement factor and relative standard deviation obtained with developed procedure were 0.193μgL(-1), 26.3 and 4.01%, respectively. Validity was checked through the recovery experiments and satisfactory results were obtained. In brief the synergistic combination of SBMNPs in column with ionic-liquid resulted in an efficient microextraction procedure for Pb(+2) in real samples. PMID:27154669

  11. Fast analysis of volatile components of Achillea tenuifolia Lam with microwave distillation followed by headspace single-drop microextraction coupled to gas chromatography-mass spectrometry (GC-MS).

    PubMed

    Piryaei, Marzieh; Nazemiyeh, Hossein

    2016-04-01

    This article investigates the effect of microwaves on the amount of volatile compounds Achillea tenuifolia Lam with two methods, headspace single-drop microextraction and microwave-assisted headspace single-drop microextraction (MA-SDME), for the analysis of essential oil. Solvent selection, solvent volume, microwave power, irradiation time and sample mass were optimised by the simplex method. PMID:26329700

  12. Combination of counter current salting-out homogenous liquid-liquid extraction and dispersive liquid-liquid microextraction as a novel microextraction of drugs in urine samples.

    PubMed

    Akramipour, Reza; Fattahi, Nazir; Pirsaheb, Meghdad; Gheini, Simin

    2016-02-15

    The counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) joined with the dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) has been developed as a high preconcentration technique for the determination of different drugs in urine samples. Amphetamines were employed as model compounds to assess the extraction procedure and were determined by high performance liquid chromatography-ultraviolet detection (HPLC-UV). In this method, initially, NaCl as a separation reagent is filled into a small column and a mixture of urine and acetonitrile is passed through the column. By passing the mixture, NaCl is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected acetonitrile is removed with a syringe and mixed with 30.0μL 1-undecanol (extraction solvent). In the second step, the 5.00mLK2CO3 solution (2% w/v) is rapidly injected into the above mixture placed in a test tube for further DLLME-SFO. Under the optimum conditions, calibration curves are linear in the range of 1-3000μgL(-1) and limit of detections (LODs) are in the range of 0.5-2μgL(-1). The extraction recoveries and enrichment factors ranged from 78 to 84% and 157 to 168, respectively. Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 100μgL(-1) of amphetamines were in the range of 3.5-4.5% and 4-5%, respectively. The method was successfully applied for the determination of amphetamines in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 90-108%. PMID:26828152

  13. Determination of 3,5,6-trichloro-2-pyridinol, phoxim and chlorpyrifos-methyl in water samples using a new pretreatment method coupled with high-performance liquid chromatography.

    PubMed

    Peng, Guilong; Lu, Ying; He, Qiang; Mmereki, Daniel; Zhou, Guangming; Chen, Junhua; Tang, Xiaohui

    2015-12-01

    A novel low-density solvent-based vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction with the solidification of floating organic droplet method coupled with high-performance liquid chromatography was developed for the determination of 3,5,6-trichloro-2-pyridinol, phoxim and chlorpyrifos-methyl in water samples. In this method, the addition of a surfactant could enhance the speed of the mass transfer from the sample solution into the extraction solvent. The extraction solvent could be dispersed into the aqueous by the vortex process. The main parameters affecting the extraction efficiency were investigated and the optimum conditions were established as follows: 80 μL 1-undecanol as extraction solvent, 0.2 mmol/L of Triton X-114 selected as the surfactant, the vortex time was fixed at 60 s with the vortex agitator set at 3000 rpm, the concentration of acetic acid in sample solution was 0.4% v/v and 1.0 g addition of NaCl. Under the optimum conditions, the enrichment factors were from 172 to 186 for the three analytes. The linear ranges were from 0.5 to 500 μg/L with a coefficient of determination (r(2) ) of between 0.9991 and 0.9995. Limits of detections were varied between 0.05 and 0.12 μg/L. The relative standard deviations (n = 6) ranged from 0.26 to 2.62%. PMID:26475036

  14. Automated headspace solid-phase microextraction and on-fiber derivatization for the determination of clenbuterol in meat products by gas chromatography coupled to mass spectrometry.

    PubMed

    Jiang, Yong; Ni, Yongnian

    2015-02-01

    A method was developed for the determination of clenbuterol in meat using stable-isotope-dilution gas chromatography with mass spectrometry coupled with solid-phase microextraction and on-fiber derivatization. The samples were first homogenized with hydrochloric acid followed by protein deposition. After headspace solid-phase microextraction and on-fiber derivatization, the content of clenbuterol was measured with the aid of stable-isotope dilution. The condition of solid-phase microextraction was optimized by central composite design. The relative standard deviations, limit of detection, and recoveries for clenbuterol were 4.2-9.2%, 0.48 μg/kg, and 96-104%, respectively. The proposed method was satisfactory for analysis of real samples as compared with the Chinese standard method. PMID:25403577

  15. Comparison of hollow fiber liquid-phase microextraction and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction for the determination of drugs of abuse in biological samples by gas chromatography-mass spectrometry.

    PubMed

    Meng, Liang; Zhang, Wenwen; Meng, Pinjia; Zhu, Binling; Zheng, Kefang

    2015-05-01

    Two microextraction techniques based on hollow fiber liquid-phase microextraction (HF-LPME) and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) had been applied for the determination of drugs of abuse (methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, methcathinone, ketamine, meperidine, and methadone) in urine and blood samples by gas chromatography-mass spectrometry. Parameters affecting extraction efficiency have been investigated and optimized for both methods. Under the optimum conditions, linearities were observed for all analytes in the range 0.0030-10 μg/ml with the correlation coefficient (R) ranging from 0.9985 to 0.9995 for HF-LPME and in the range 0.0030-10 μg/ml with the R ranging from 0.9985 to 0.9994 for DLLME. The recovery of 79.3-98.6% with RSDs of 1.2-4.5% was obtained for HF-LPME, and the recovery of 79.3-103.4% with RSDs of 2.4-5.7% was obtained for DLLME. The LODs (S/N=3) were estimated to be in the range from 0.5 to 5 ng/ml and 0.5 to 4 ng/ml, respectively. Compared with HF-LPME, the UA-LDS-DLLME technique had the advantages of less extraction time, suitability for batches of sample pretreatment simultaneously, and higher extraction efficiency, while HF-LPME has excellent sample clean-up effect, and is a robust and suitable technique for various sample matrices with better repeatability. Both methods were successfully applied to the analysis of drugs of abuse in real human blood sample. PMID:25801996

  16. Application of low-temperature glassy carbon films in solid-phase microextraction.

    PubMed

    Giardina, M; Olesik, S V

    2001-12-15

    Low-temperature glassy carbon (LTGC) films were investigated as a sorbent coating for solid-phase microextraction because of its uniquely selective adsorptive characteristics. The selectivity of these coatings is primarily controlled by shape characteristics of the solute molecule and the final processing temperature used to form the LTGC, demonstrating unique adsorptive characteristics compared to commercial phases. The LTGC films were prepared by first coating porous silica particles with a diethylnyl oligomer precursor and then heat curing at temperatures between 300 and 1000 degrees C to form the LTGC. Then, using a sol-gel process, the LTGC-coated silica particles were immobilized onto stainless steel fibers and subsequently used for headspace and liquid extractions followed by GC-FID analysis. The selectivity of the LTGC is demonstrated by the extraction of a variety of aromatic hydrocarbons as well as the taste and odor contaminants geosmin, 2-methylisoborneol, and 2,4,6-trichloroanisole commonly found in water supplies. The data show that the LTGC coating has the highest affinity for molecules with the greatest cross-sectional surface area and polarizability and that this selective mechanism increases as a function of LTGC processing temperature. PMID:11791552

  17. Sensitive determination of mercury by a miniaturized spectrophotometer after in situ single-drop microextraction.

    PubMed

    Yang, Fangwen; Liu, Rui; Tan, Zhiqiang; Wen, Xiaodong; Zheng, Chengbin; Lv, Yi

    2010-11-15

    An in situ single-drop microextraction (SDME) method was developed for trace mercury determination by a miniaturized spectrophotometer, in which a simple and cheap light-emitting diode (LED) was employed as the light source, and a handheld charge coupled device (CCD) was served as the detector. A droplet of 0.006% dithizone-CCl(4) (m/v) was used as extraction phase and hanged on a rolled PTFE tube. LED light was adjusted carefully to pass through the centre of the droplet and the entrance slit of the CCD detector. The radiation intensities of 475 nm before and after SDME (I(0) and I(i)) were recorded for quantification. Under the optimum conditions, the system provided a linear range of 2-50 μg L(-1), with a correlation coefficient of 0.9983 and a limit of detection (3σ) of 0.2 μg L(-1). The enrichment factor was about 69. The present method showed the merits of high sensitivity, simplicity, rapidity, low reagent consumption and field analysis potential. Finally, this method was successfully applied for the determination of the total mercury in spiked tap water sample, spiked river water sample and certified reference material (GBW (E) 080393, simulated water). PMID:20696521

  18. Conductive polymeric ionic liquids for electroanalysis and solid-phase microextraction.

    PubMed

    Young, Joshua A; Zhang, Cheng; Devasurendra, Amila M; Tillekeratne, L M Viranga; Anderson, Jared L; Kirchhoff, Jon R

    2016-03-01

    Three novel electropolymerizable thiophene-based ionic liquids (ILs) were synthesized and characterized as potential candidates for developing selective extraction media for chemical analysis. Electropolymerization of the bis[(trifluoromethyl)sulfonyl]imide ([NTf2](-)) analogs successfully produced uniform polymeric thin-films on macro- and microelectrode substrates from both vinyl and methylimidazolium IL monomer derivatives. The resultant conducting polymer IL (CPIL) films were characterized by electrochemical methods and found to exhibit attractive behavior towards anionic species while simultaneously providing an exclusion barrier toward cationic species. Thermogravimetric analysis of the thiophene-based IL monomers established a high thermal stability, particularly for the methylimidazolium IL, which was stable until temperatures above 350 °C. Subsequently, the methylimidazolium IL was polymerized on 125 μm platinum wires and utilized for the first time as a sorbent coating for headspace solid-phase microextraction (HS-SPME). The sorbent coating was easily prepared in a reproducible manner, provided high thermal stability, and allowed for the gas chromatographic analysis of polar analytes. The normalized response of the poly[thioph-C6MIm][NTf2]-based sorbent coating exhibited higher extraction efficiency compared to an 85 μm polyacrylate fiber and excellent fiber-to-fiber reproducibility. Therefore, the electropolymerizable thiophene-based ILs were found to be viable new materials for the preparation of sorbent coatings for HS-SPME. PMID:26873467

  19. Crosslinked polymeric ionic liquids as solid-phase microextraction sorbent coatings for high performance liquid chromatography.

    PubMed

    Yu, Honglian; Merib, Josias; Anderson, Jared L

    2016-03-18

    Neat crosslinked polymeric ionic liquid (PIL) sorbent coatings for solid-phase microextraction (SPME) compatible with high-performance liquid chromatography (HPLC) are reported for the first time. Six structurally different PILs were crosslinked to nitinol supports and applied for the determination of select pharmaceutical drugs, phenolics, and insecticides. Sampling conditions including sample solution pH, extraction time, desorption solvent, desorption time, and desorption solvent volume were optimized using design of experiment (DOE). The developed PIL sorbent coatings were stable when performing extractions under acidic pH and remained intact in various organic desorption solvents (i.e., methanol, acetonitrile, acetone). The PIL-based sorbent coating polymerized from the IL monomer 1-vinyl-3-(10-hydroxydecyl) imidazolium chloride [VC10OHIM][Cl] and IL crosslinker 1,12-di(3-vinylbenzylimidazolium) dodecane dichloride [(VBIM)2C12] 2[Cl] exhibited superior extraction performance compared to the other studied PILs. The extraction efficiency of pharmaceutical drugs and phenolics increased when the film thickness of the PIL-based sorbent coating was increased while many insecticides were largely unaffected. Satisfactory analytical performance was obtained with limits of detection (LODs) ranging from 0.2 to 2 μg L(-1) for the target analytes. The accuracy of the analytical method was examined by studying the relative recovery of analytes in real water samples, including tap water and lake water, with recoveries varying from 50.2% to 115.9% and from 48.8% to 116.6%, respectively. PMID:26896916

  20. Monodisperse microporous carbon nanospheres: An efficient and stable solid phase microextraction coating material.

    PubMed

    Zheng, Juan; Wang, Kun; Luo, Erlun; Wu, Dingcai; Zhu, Fang; Jiang, Ruifen; Su, Chengyong; Wei, Chaohai; Ouyang, Gangfeng

    2015-07-16

    The monodisperse microporous carbon nanospheres (MMCNSs) were applied in solid phase microextraction for the first time. The MMCNSs-fiber was prepared by sol-gel technique and good repeatability and reproducibility were obtained, due to the excellent monodispersity of the MMCNSs. The sol-gel-MMCNSs fiber exhibited superior extraction ability for polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs), compared with the commercial polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber and the fiber prepared with its precursor, the monodisperse microporous polystyrene nanospheres (MMPNSs). Moreover, the fiber has good thermostability and strong acid/base durability. The sol-gel-MMCNSs fiber was then employed to detect PAHs and OCPs in aqueous samples by combining with gas chromatography-mass spectrometer (GC-MS). Under the optimized conditions, the detection limits of the proposed method ranged from 0.10 to 5.5 ng L(-1). Furthermore, the method was successfully utilized for the analysis of PAHs and OCPs in real samples, with satisfactory recoveries in the range of 81.0-120% for the Pearl River water samples and 72.8-118% for the coking wastewater samples. PMID:26073808

  1. Design and optimization of a total vaporization technique coupled to solid-phase microextraction.

    PubMed

    Rainey, Christina L; Bors, Dana E; Goodpaster, John V

    2014-11-18

    Solid-phase microextraction (SPME) is a popular sampling technique in which chemical compounds are collected with a sorbent-coated fiber and then desorbed into an analytical instrument such as a liquid or gas chromatograph. Typically, this technique is used to sample the headspace above a solid or liquid sample (headspace SPME), or to directly sample a liquid (immersion SPME). However, this work demonstrates an alternative approach where the sample is totally vaporized (total vaporization SPME or TV-SPME) so that analytes partition directly between the vapor phase and the SPME fiber. The implementation of this technique is demonstrated with polydimethylsiloxane-divinylbenzene (PDMS-DVB) and polyacrylate (PA) coated SPME fibers for the collection of nicotine and its metabolite cotinine in chloroform extracts. The most important method parameters were optimized using a central composite design, and this resulted in an optimal extraction temperature (96 °C), extraction time (60 min), and sample volume (120 μL). In this application, large sample volumes up to 210 μL were analyzed using a volatile solvent such as chloroform at elevated temperatures. The sensitivity of TV-SPME is nearly twice that of liquid injection for cotinine and nearly 6 times higher for nicotine. In addition, increased sampling selectivity of TV-SPME permits detection of both nicotine and cotinine in hair as biomarkers of tobacco use where in the past the detection of cotinine has not been achieved by conventional SPME. PMID:25313649

  2. Analysis of freely dissolved alcohol ethoxylate homologues in various seawater matrixes using solid-phase microextraction.

    PubMed

    Droge, Steven T J; Sinnige, Theo L; Hermens, Joop L M

    2007-04-01

    Solid-phase microextraction fibers (SPME) were tested as tools to determine freely dissolved alcohol ethoxylate (AE) surfactants in seawater matrixes. Partitioning of a wide range of AE homologues into a 35-mum polyacrylate fiber coating was linearly related to aqueous concentrations as low as submicrograms per liter, with high reproducibility. The exposure time needed to reach equilibrium between aqueous phase and the SPME fiber depended on the fiber-water partitioning coefficient (Kfw) of the AE homologue. Specific attention was given to the influence of various matrixes on the analysis via SPME. The presence of sediment increases the uptake kinetics of AE homologues for which diffusion in the aqueous phase is rate limiting. The Kfw in equilibrated systems was not affected by the presence of other homologues, micelles, or varying amounts of sediment phase. SPME is therefore a suitable tool for analysis of AE in sorption studies and sediment toxicity tests. A strong linear relation was observed between Kfw and the hydrophobicity of the AE homologue, using estimated octanol-water partition coefficients. This relation can be used to predict the partitioning coefficient of any AE homologue to the SPME fiber, which facilitates the analysis of complex mixtures. PMID:17338502

  3. Determination of phenolic compounds in honey using dispersive liquid-liquid microextraction.

    PubMed

    Campone, Luca; Piccinelli, Anna Lisa; Pagano, Imma; Carabetta, Sonia; Di Sanzo, Rosa; Russo, Mariateresa; Rastrelli, Luca

    2014-03-21

    Honey is a valuable functional food rich in phenolic compounds with a broad spectrum of biological activities. Analysis of the phenolic compounds in honey is a very promising tool for the quality control, the authentication and characterization of botanical origin, and the nutraceutical research. This work describes a novel approach for the rapid analysis of five phenolic acids and 10 flavonoids in honey. Phenolic compounds were rapidly extracted and concentrated from diluted honey by dispersive liquid-liquid microextraction (DLLME) and then analyzed using high performance liquid chromatography with UV absorbance detection (HPLC-UV). Some important parameters, such as the nature and volume of extraction and dispersive solvents, pH and salt effect were carefully investigated and optimized to achieve the best extraction efficiency. Under the optimal conditions, an exhaustive extraction for twelve of the investigated analytes (recoveries >70%), with a precision (RSD<10%) highly acceptable for complex matrices, and detection and quantification limits at ppb levels (1.4-12 and 4.7-40ngg(-1), respectively) were attained. The proposed method, compared with the most widely used method in the analysis of phenolic compounds in honey, provided similar or higher extraction efficiency, except in the case of the most hydrophilic phenolic acids. The capability of DLLME to the extraction of other honey phytochemicals, such as abscisic acid, was also demonstrated. The main advantages of developed method are the simplicity of operation, the rapidity to achieve a very high sample throughput and low cost. PMID:24565235

  4. Electromembrane surrounded solid phase microextraction using electrochemically synthesized nanostructured polypyrrole fiber.

    PubMed

    Mohammadkhani, Elham; Yamini, Yadollah; Rezazadeh, Maryam; Seidi, Shahram

    2016-04-22

    Electromembrane surrounded solid phase microextraction using conductive polymers as the sorbent is carried out for the first time for extraction of two antidepressants including amitriptyline (AMI) and doxepin (DOX), as model analytes. The polypyrrole coating was prepared and utilized as both cathode and SPME sorbent. Different variables such as the conditions for preparation of polypyrrole fiber, pH of the donor and the acceptor phases, applied voltage, and extraction time were optimized. Under the optimized conditions, figures of merit of the proposed method were investigated in human whole blood and urine samples. Intra- and inter-assay precisions ranged between 3.1-7.5% and 7.6-12.3%, respectively were obtained in different extraction media. Detection limits of 0.15 and 0.05 for AMI and 0.3 and 0.1ngmL(-1) for DOX were achieved in the urine and blood samples, respectively. Linearity of the method was studied up to 50.0ngmL(-1) for both analytes and coefficients of determination better than 0.9966 were achieved. Regardless of the high sample cleanup, which makes the proposed method suitable for analysis of drugs from complicated matrices, clean chromatograms were obtained. Finally, the proposed method was applied for analysis of AMI and DOX in different real samples and reasonable data were obtained. PMID:27033980

  5. Determining chemical activity of (semi)volatile compounds by headspace solid-phase microextraction.

    PubMed

    Legind, Charlotte N; Karlson, Ulrich; Burken, Joel G; Reichenberg, Fredrik; Mayer, Philipp

    2007-04-01

    This research introduces a new analytical methodology for measuring chemical activity of nonpolar (semi)volatile organic compounds in different sample matrices using automated solid-phase microextraction (SPME). The chemical activity of an analyte is known to determine its equilibrium concentration in the SPME fiber coating. On this basis, SPME was utilized for the analytical determination of chemical activity, fugacity, and freely dissolved concentration using these steps: (1) a sample is brought into a vial, (2) the SPME fiber is introduced into the headspace and equilibrated with the sample, (3) the SPME fiber is injected into the GC for thermal desorption and analysis, and (4) the method is calibrated by SPME above partitioning standards in methanol. Model substances were BTEX, naphthalene, and alkanes, which were measured in a variety of sample types: liquid polydimethylsiloxane (PDMS), wood, soil, and nonaqueous phase liquid (NAPL). Variable sample types (i.e., matrices) had no influence on sampling kinetics because diffusion through the headspace was rate limiting for the overall sampling process. Sampling time was 30 min, and relative standard deviations were generally below 5% for homogeneous solutions and somewhat higher for soil and NAPL. This type of activity measurement is fast, reliable, almost solvent free, and applicable for mixed-media sampling. PMID:17313185

  6. Analysis of lignocellulose derived phenolic monomers by headspace solid-phase microextraction and gas chromatography.

    PubMed

    Kolb, Michaela; Schieder, Doris; Faulstich, Martin; Sieber, Volker

    2013-09-13

    A headspace solid-phase microextraction method with subsequent GC-MS (HS-SPME/GC-MS) was established for the quantitative analysis of volatile lignin derived phenolic monomers in complex aqueous solutions. Extraction was done using a polyacrylate fiber. The optimization of HS-SPME - parameters was performed using a multi component model solution of six representative phenolic monomers identified in liquid hot water (LHW) supernatants of hydrothermally treated lignocellulosic biomass: p-coumaric acid, guaiacol, vanillin, acetosyringone, 4-hydroxy-3-methoxyphenylacetone, and acetophenone. Plackett-Burman design was applied for pre-evaluation and 2(3) central composite designs with star points for parameter optimization. LOQ (S/N>10) and LOD (S/N>3) were determined for 12 phenols yielding LOQ of <0.005-618nM and LOD of <0.005-412nM. Within-day and between-day tests (n=6) showed different results for the tested phenols. RSD ranged from 2% to 30% and recovery rates from 99% to 160% in LHW matrix. Tests on storage of LHW supernatants for several weeks indicated a considerable influence of temperature on the stability of the solutions which may even have to be taken into account for auto sampler handling. All in all the method allows a fast and solvent free analysis requiring low sample volumes making it a powerful tool for screening or high-throughput analysis of aqueous solutions of lignin derived aromatics. PMID:23932028

  7. Determination of mitragynine in urine matrices by bar adsorptive microextraction and HPLC analysis.

    PubMed

    Neng, N R; Ahmad, S M; Gaspar, H; Nogueira, J M F

    2015-11-01

    Bar adsorptive microextraction combined with liquid desorption followed by high performance liquid chromatography with diode array detection (BAµE-LD/HPLC-DAD) is proposed for the determination of the psychoactive alkaloid mitragynine (MG) in human urine matrices. By using a modified N-vinylpyrrolidone polymer (P2) sorbent phase, high selectivity and efficiency is achieved. Assays performed by BAµE(P2)-LD/HPLC-DAD on 25 mL water samples spiked at the 8.0 µg L(-1) level yielded average recoveries around 100% of MG, under optimized experimental conditions. The analytical performance showed good precision (RSD<15%), appropriated detection limits of 0.10 µg L(-1) and linear dynamic ranges (0.6-24.0 μg L(-1)) with convenient determination coefficients of 0.9924. By using the standard addition method, the application of the present methodology for the determination of MG in human urine matrices after Kratom consumer, allowed very good performances. The proposed methodology proved to be a suitable alternative to monitor MG in biological fluid matrices, showing to be easy to implement, reliable, sensitive and requiring low sample volumes, when compared with other sorbent-based methods. PMID:26452798

  8. Carbonized polydopamine as coating for solid-phase microextraction of organochlorine pesticides.

    PubMed

    Huang, Zhenzhen; Chua, Pey Ee; Lee, Hian Kee

    2015-06-19

    A facile preparation route for coating a stainless steel fiber with carbonaceous material derived from polydopamine is reported in this work. The self-oxidation induced polymerization of dopamine in alkaline solution enables growth of polydopamine on the inert surface of the fiber. The robust adhesion of dopamine to metal oxides ensured sufficient stability of the polymer coating. After carbonization of the polymer coating, the obtained carbon coated fiber was utilized for solid-phase microextraction and exhibited effectiveness in the extraction of organochlorine pesticides (OCPs) from aqueous solution. Extraction time, agitation speed and salt addition were optimized. The possible interference of humic acid on the extraction of these analytes was also investigated. The results showed that most of the analytes could be detected efficiently in the presence of humic acid at a concentration of 20mg/L. Under the optimized conditions, enrichment factors of 102-757 were obtained for the selected OCPs in aqueous solution. The proposed method provided low limits of detection (1.4-15 ng/L), good linearity (correlation coefficients>0.9971) and acceptable precision (relative standard deviations<16.3%). PMID:25943831

  9. Facile preparation and applications of graphitic carbon nitride coating in solid-phase microextraction.

    PubMed

    Xu, Na; Wang, Yiru; Rong, Mingcong; Ye, Zhifeng; Deng, Zhuo; Chen, Xi

    2014-10-17

    In this study, graphitic carbon nitride (g-C3N4) was used as a coating material for solid-phase microextraction (SPME) applications. Coupled to gas chromatography (GC), the extraction ability of the SPME fiber was investigated and compared with the commercial fibers of 100 μm PDMS and 85 μm CAR/PDMS using six target analytes including deltamethrin, nerolidol, amphetamine, dodecane, ametryn and acrylamide. The g-C3N4 coating revealed excellent extraction ability and durability comparing with those of the commercial fibers due to its loose structure and unique physicochemical properties. The repeatability for each single fiber was found to be 3.46% and reproducibility for fiber to fiber was 8.53%. The g-C3N4 SPME fiber was applied to the determination of acrylamide in potato chips, the linearity and detection limit was 0.5-250 μg g(-1) and 0.018 μg g(-1), respectively. PMID:25218628

  10. Collection and separation of extract in dispersive liquid-liquid microextraction with hollow fiber.

    PubMed

    Wang, Kun; Li, Na; Lei, Lei; Yang, Xiao; Wang, Zhibing; Li, Dan; Zang, Shuang; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei

    2016-05-01

    Dispersive liquid-liquid microextraction combined with collection of the extraction phase with the hollow fiber was applied to the extraction of estrogens from environmental water samples. 1-Undecanol with relatively lower toxicity was used as the extraction solvent. The hollow fiber was used to collect the extraction phase containing the analytes from the aqueous phase. Hollow fibers collecting the extraction phase were eluted with acetonitrile and the resulting eluate was analyzed by high performance liquid chromatography. Several parameters, including pH of sample, the type and volume of the extraction and dispersive solvent, salt concentration, extraction time, and collection time were optimized. Under the optimal experimental conditions, the limits of detection for estriol, 17α-estradiol, and ethynylestradiol were 4.58, 1.41, and 1.41 μg L(-1), respectively. When the present method was applied to the analysis of real water samples, the recoveries of estrogens at two spiked levels were in the range of 55.8-107.4%. In this method, the separation of the extraction phase and aqueous phase becomes easy with no need for centrifugation, refrigeration-thaw, or any special device. The hollow fiber was commercially available and the collection procedure was easy to perform, which make the present method have potential for automation and wide promotion. Small sizes of pores on the walls of the hollow fibers can block large molecules, which makes the present method have the potential for the treatment of complex matrices. PMID:26894762

  11. Liquid-phase microextraction of organophosphorus pesticides using supramolecular solvent as a carrier for ferrofluid.

    PubMed

    Zohrabi, Parvin; Shamsipur, Mojtaba; Hashemi, Mahdi; Hashemi, Beshare

    2016-11-01

    A liquid-phase microextraction based on application of supramolecular solvent as a carrier for ferrofluid has been developed for the extraction and determination of three organophosphorus pesticides (OPPs). The ferrofluid was produced from combination of oleic acid coated magnetic particles and supramolecular solvent as the extractant solvent. Ferrofluid can be attracted by a magnet, and no centrifugation step was needed for phase separation. A response surface methodology (RSM) based on central composite design (CCD) was used for efficient optimization of the main variables in the extraction procedure. Under the optimum experimental conditions, the calibration curves found to be linear in the range of 0.5-400µgL(-1) with correlation coefficients ranging from 0.9967 to 0.9984. The intra-day and inter-day precision (RSD %) for 100 and 200µgL(-1) of each pesticides were in the range of 2.0-5.3% and 2.6-5.7%, respectively. The limit of detection (S/N=3), ranged from 0.1 to 0.35μgL(-1). The proposed method was successfully applied to the extraction and determination of organophosphorus pesticide residues in water and fruit juice samples. PMID:27591622

  12. Hierarchical Graphene coating for highly sensitive solid phase microextraction of organochlorine pesticides.

    PubMed

    Wang, Fuxin; Liu, Shuqin; Yang, Hao; Zheng, Juan; Qiu, Junlang; Xu, Jianqiao; Tong, Yexiang; Zhu, Fang; Ouyang, Gangfeng

    2016-11-01

    Graphene, a novel class of carbon nanostructures, has received great attention as sorbents due to its fascinating structures, ultrahigh specific surface area, and good extraction ability. In this paper, a new type of hierarchical graphene was synthesized through employing a mild and environment-friendly method. Such 3D interconnected graphene own a high specific surface area up to 524m(2)g(-1), which is about 2.5 fold larger than the graphene, since the synthetic material has interlayer pores between nanosheets and in-plane pores. Then a superior solid-phase microextraction fiber was fabricated by sequentially coating the stainless steel fiber with silicone sealant film and hierarchical graphene powder. Since the novel hierarchical graphene possessed large surface area and good adsorption property, the as-prepared fiber exhibited good extraction properties of the organochlorine pesticides (OCPs). As for the analytical performance, the as-prepared fiber achieved low detection limits (0.08-0.80ngL(-1)) and wide linearity (10-30,000ngL(-1)) under the optimal conditions. The repeatability (n=5) for single fiber were between 5.1% and 11%, while the reproducibility (n=3) of fiber-to-fiber were range from 6.2% to14%. Moreover, the fiber was successfully applied to the analysis of OCPs in the Pearl River water. PMID:27591607

  13. Determination of toluene in brain of freely moving mice using solid-phase microextraction technique.

    PubMed

    Nakajima, Daisuke; Tin-Tin-Win-Shwe; Kakeyama, Masaki; Fujimaki, Hidekazu; Goto, Sumio

    2006-07-01

    For the purpose of measuring the pharmacokinetics of inhaled toluene in the brain of mice, we developed a method for the direct detection of toluene by gas chromatography/mass spectrometry (GC/MS). The method uses a solid-phase microextraction (SPME) fiber inserted into the mouse' hippocampus (CA1) through a cannula fixed onto the animal. BALB/c mice were exposed to 0, 0.9, 9, 50 and 90 ppm toluene for 30 min. The toluene level detected near the hippocampus by this method after exposure to 0.9 ppm toluene in air showed no significant difference from the level found in the non-exposure control group; however, the toluene level increased significantly after exposure to concentrations of 9, 50 and 90 ppm. These increases were concentration-dependent. In addition, the pharmacokinetics of toluene in the brain of mice exposed to 50 ppm toluene showed that the toluene level decreased rapidly after the exposure, and returned to control levels after 60 min. This study describes the method which has successfully detected toluene levels in the brain of conscious, free-moving mice for the first time. PMID:16457888

  14. Headspace solid-phase microextraction analysis of volatile sulphides and disulphides in wine aroma.

    PubMed

    Mestres, M; Busto, O; Guasch, J

    1998-05-29

    Sulphur compounds (S-compounds) are important constituents of wine off-flavours. Headspace solid-phase microextraction (HS-SPME) combined with gas chromatography coupled to flame photometric detection (GC-FPD) was used to develop a suitable method to analyse volatile sulphides and disulphides. This is a very simple and fast technique which gives good reproducibility at microgram/l levels (relative standard deviations < 10%). The analytes were extracted from the headspace of the samples by using either polydimethylsiloxane or polyacrylate coated fused-silica fibers in an SPME unit. Then, the fiber was inserted into the injector of a gas chromatograph and the extracted S-compounds were thermally desorbed. The influence of different parameters, such as ionic strength, stirring, headspace volume, ethanol concentration, time and temperature of extraction, was studied. The extraction of the fibers varies considerably for the different sulphur compounds studied. The most volatile compounds were the least extracted by the coating fibers tested. The standard additions technique, applied to real samples, gave the recoveries > 94%. The detection limits range between 3 micrograms/l and 50 ng/l. The overall process was successfully applied to identify and quantify S-compounds in white and red wines. PMID:9652119

  15. Application of a single-drop microextraction for the analysis of organophosphorus pesticides in juice.

    PubMed

    Zhao, Ercheng; Han, Lijun; Jiang, Shuren; Wang, Qiuxia; Zhou, Zhiqiang

    2006-05-12

    In this study, a new method for the determination of organophosphorus pesticides (OPPs) (ethoprophos, diazinon, parathion methyl, fenitrothion, malathion, isocarbophos and quinaphos) in orange juice was developed. Single-drop microextraction (SDME) parameters, such as organic solvent, drop volume, agitation rate, extraction time, and salt concentration were optimized through analysis of OPPs in fortified water. The orange juice was simply centrifuged and diluted with water, extracted by SDME and analyzed by gas chromatography (GC) equipped with a flame photometric detection (FPD). Fortification tests were conducted for concentrations between 10 and 500 microg/L; mean relative recoveries for each pesticide were all above 76.2% and below 108.0%. Limits of detection of the method for orange juice were below 5 microg/L for all target pesticides. The repeatability of the proposed method, expressed as relative standard deviation varied between 4.6 and 14.1% (n=5). The proposed method is acceptable in the analysis of OPPs pesticides in juice matrices. PMID:16569410

  16. Measuring pyrethroids in sediment pore water using matrix-solid phase microextraction.

    PubMed

    Hunter, Wesley; Yang, Yu; Reichenberg, Fredrik; Mayer, Philipp; Gan, Jianying

    2009-01-01

    Pyrethroids are hydrophobic insecticides commonly used in both agricultural and urban environments. Their high toxicity to aquatic organisms, including benthic invertebrates, and detection in the sediment at many locations in California, U.S.A., have spawned interest in understanding their bioavailability in bed sediments. A recent study showed good correlation between uptake of 14C-permethrin in Chironomus tentans and solid-phase microextraction (SPME) fibers in sediments. The present study was directed at the development of an SPME technique applicable to trace levels of nonlabeled pyrethroids in sediment. Disposable polydimethylsiloxane fibers were used to detect freely dissolved pore-water concentrations of bifenthrin, fenpropathrin, cis-permethrin, trans-permethrin, cyfluthrin, cypermethrin, and esfenvalerate under agitated and static conditions. Partition equilibrium between fiber and sediment was reached in <5 d when the samples were agitated on a shaker at low speed, while much longer times (>23 d) were needed without agitation. Polydimethylsiloxane to water partition ratios (K(PDMS)) of the seven pyrethroids were measured separately and ranged from 2.83 x 10(5) to 1.89 x 10(6). When applied to field-contaminated sediments, agitated matrix-SPME was able to detect pore-water concentrations as low as 0.1 ng/L. The method developed in the present study may be coupled with bioassays to gain mechanistic understanding of factors affecting pyrethroid toxicities, and applied to field samples to better predict sediment toxicities from pyrethroid contamination. PMID:18712946

  17. Determination of MTBE in a recreational harbor using solid-phase microextraction.

    PubMed

    Zuccarello, Joseph L; Ganske, Jane A; Green, David B

    2003-06-01

    Discovery of the fuel additive methyl tert-butyl ether (MTBE) in groundwater, surface water, and stormwater has prompted studies of its sources, transport and fate. More limited data, however, is available on the extent of contamination of coastal waters, as well as the persistence of MTBE in the marine environment. We apply here the combination of solid phase microextraction and gas chromatography-mass spectrometry to the detection of sub-to-low microgram/l concentrations of MTBE in seawater samples. Analysis of samples collected at the Marina del Rey harbor, a shallow recreational harbor near Los Angeles, CA, show MTBE contamination in the low microgram/l level. MTBE measurements were made at different depths, from the surface to the bottom, at five sites within the harbor during months showing no measurable precipitation. The highest concentration of MTBE (18 microgram/l) was found at the boat launching ramp, and the lowest (0.2 microgram/l) near the harbor entrance, approximately 2.3 km from the ramp. The levels of MTBE measured, as well as their variation over the study period, are fully consistent with recreational boating as the primary source of contamination. No evidence for MTBE contamination from the adjacent stormwater control channel was noted. PMID:12668039

  18. Solid-phase microextraction of volatile compounds from the chopped leaves of three species of Eucalyptus.

    PubMed

    Zini, Cláudia A; Zanin, Kelen D; Christensen, Eva; Caramão, Elina B; Pawliszyn, Janusz

    2003-04-23

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography and ion-trap mass spectrometry has been used to identify biogenic volatile organic compounds present in the headspace of chopped leaves of Eucalyptus (E.) dunnii, E. citriodora, and E. saligna. A simple HS-SPME method entailing 30 min of extraction at 30 degrees C was developed for this purpose. Thirty compounds were identified in the headspace of 60 juvenile chopped Eucalyptus leaves, and another 30 were tentatively identified. The presence of compounds such as (E)-4,8-dimethyl-1,3,7-nonatriene (DMNT), (E,E)-4,8,12-trimethyl-1,3,7,11-tridecatetraene (TMNT), (E,E)-alpha-farnesene, (E,E,E)-3,7,11,15-tetramethyl-1,3,6,10,14-hexadecapentaene (TMHP), beta-caryophyllene, alpha-humulene, germacrene D, and beta-cubebene in the headspace of the leaves but not in the essential oils from the same Eucalyptus trees and information about the infochemical roles of some of these compounds in other living plant systems suggest they might play a bioactive role in Eucalyptus leaves. PMID:12696957

  19. Solid phase microextraction of volatile constituents from individual fresh Eucalyptus leaves of three species.

    PubMed

    Betts, T J

    2000-03-01

    Methyl polysiloxane solid-phase microextraction fibres were used for ten minutes to adsorb volatile constituents from headspace above all or part of a single cut up fresh eucalyptus leaf kept warm at 37 degrees C. The fibres were desorbed at 200 degrees C for programmed gas chromatography (40-187 degrees C) on a methyl polysiloxane capillary. Substances were identified by mass spectra and/or authentic sample retention. Results do not correspond to published values for steam distilled oils, being richer in sesquiterpenes, of which three are common to three different species; and also in esters in two species. Five Eucalyptus citriodora leaves from the same tree over different months gave very similar analyses to a fibre in 10 min of 72.9-80.5% citronellal, 3.5-5.4% citronellol, 1.0-3.8% citronellyl acetate, 9.2-11.8% caryophyllene and 1.4-1.7% bicyclogermacrene. Six E. nicholii leaves yielded 67.2-73.7% cineole and 4.6-9.7% limonene along with 10.5-16.5% sesquiterpenes, mostly hydrocarbons, particularly bicyclogermacrene. E. globulus leaves gave only 54.0-61.3% cineole, with 19.5-24.3% alpha-pinene, 6.7-9.1% limonene and 2.1-5.4% alpha-terpinyl acetate; along with 3.6-7.7% sesquiterpenes, particularly aromadendrene, but no bicyclogermacrene. PMID:10763604

  20. Extraction of Citrus paradisi Volatile Components by Headspace Single-Drop Microextraction and Statistical Modeling.

    PubMed

    Sadeghian, F; Ebrahimi, P; Shakeri, A; Jamali, M R

    2016-08-01

    In present study, headspace single-drop microextraction (HS-SDME) was applied for the extraction and preconcentration of the volatile components of the plant sample into a microdrop surface. The extraction occurred by suspending a microliter drop of the solvent from the tip of a microsyringe to the headspace of a ripe fruit sample (grapefruit Citrus paradisi) in a sealed vial for a preset extraction time. Then the microdrop was retracted back into the microsyringe and injected directly into a gas chromatography injection port. The chemical composition of the SDME extracts was confirmed according to their mass spectra, and quantitative analysis was performed by gas chromatography-flame ionization detector (GC-FID). Response surface methodology along with Box-Behnken design was applied to optimize the extraction condition of four components, d-limonene, β-myrcene, α-pinene and β-pinene, from the peel of grapefruit. Parameters considered for SDME include the kind of the extracting solvent, size of drop, extraction temperature and extraction time. The optimized condition was microdrop volume of 1 µL, extraction time of 2 min and sample temperature of 50°C. PMID:27048646

  1. Mesoporous TiO₂ nanoparticles for highly sensitive solid-phase microextraction of organochlorine pesticides.

    PubMed

    Liu, Shuqin; Xie, Lijun; Zheng, Juan; Jiang, Ruifeng; Zhu, Fang; Luan, Tiangang; Ouyang, Gangfeng

    2015-06-01

    Mesoporous TiO2 nanoparticles were synthesized with the hydrothermal method and characterized by powder X-ray diffraction (PXRD) and transmission electron microscope (TEM). Then a superior solid-phase microextraction (SPME) fiber was fabricated by sequentially coating the stainless steel fiber with silicone sealant film and mesoporous TiO2 powder. The developed fiber possessed a homogeneous surface and a long life-span up to 100 times at direct immersing (DI) extraction mode. Under the optimized conditions, the extraction efficiencies of the self-made 17 μm TiO2 fiber for six organochlorine pesticides (OCPs) were higher than those of the two commercial fibers (65 μm PDMS/DVB and 85 μm PA fibers) which were much thicker than the former. As for analytical performance, low detection limits (0.08-0.60 ng L(-1)) and wide linearity (5-5000 ng L(-1)) were achieved under the optimal conditions. The repeatabilities (n=5) for single fiber were between 2.8 and 12.3%, while the reproducibilities (n=3) of fiber-to-fiber were in the range of 3.7-15.7%. The proposed fiber was successfully applied to the sensitive analysis of OCPs in real water samples and four of the six analytes were detected from the rainwater and the lake water samples. PMID:26002332

  2. A solid-phase microextraction chamber method for analysis of manure volatiles.

    PubMed

    Miller, Daniel N; Woodbury, Bryan L

    2006-01-01

    Odors from livestock operations are a complex mixture of volatile carbon, sulfur, and nitrogen compounds. Currently, detailed volatiles analysis is both time consuming and requires specialized equipment and methods. This work describes a new method that utilizes a dynamic flux chamber, solid-phase microextraction (SPME), and gas chromatography-mass spectroscopy (GC-MS) to describe and compare the odorous compounds emitted from cattle and swine feces. Evaluation of method parameters produced a protocol for comparing relative emissions based on fixed sample temperature (20 degrees C) and exposed surface area (approximately 523 cm(2)), air flow rates (1 L min(-1) or 16 cm s(-1)), SPME exposure time (5 min), and chamber cleaning procedures (70% ethanol rinse and drying for 30 min at 105 degrees C) to minimize cross-contamination between samples. A variety of volatile organic compounds (VOCs) including alcohols, volatile fatty acids, aromatic ring compounds, ketones, esters, and sulfides were routinely detected and the relative emissions from fresh and incubated (37 degrees C overnight) swine and cattle feces were compared as a measure of potential to produce odorants during manure storage. Differences in the types and relative quantities of volatiles emitted were detected when animal species (cattle or swine), diet, fecal incubation, or sample storage conditions (20, 4, or -20 degrees C) were varied. PMID:17071909

  3. Graphenized pencil lead fiber: facile preparation and application in solid-phase microextraction.

    PubMed

    Liu, Qian; Cheng, Mengting; Long, Yanmin; Yu, Miao; Wang, Thanh; Jiang, Guibin

    2014-01-17

    Graphenized pencil lead fiber was facilely prepared by in situ chemical exfoliation of graphite in pencil lead fiber to few-layered graphene sheets via a one-pot, one-step pressurized oxidation reaction for the first time. This new fiber was characterized and demonstrated to be a highly efficient but low-cost solid-phase microextraction (SPME) fiber. The extraction performance of the fiber was evaluated with four bisphenol analogs [bisphenol A (BPA), bisphenol S (BPS), bisphenol AF (BPAF), and tetrabromobisphenol A (TBBPA)] as model analytes in direct SPME mode. Unlike commercially available fibers, the graphenized pencil lead fiber showed an excellent chemical stability in highly saline, acidic, alkaline and organic conditions due to its coating-free configuration. The fiber also showed a very long lifespan. Furthermore, high extraction efficiency and good selectivity for the analytes with a wide polarity range could be obtained due to the exceptional properties of graphene. The detection limits (LODs) for the analytes were in the range of 1.1-25ng/L. The fiber was successfully applied in the analysis of tap water and effluent samples from a waste water treatment plant with spike recoveries ranging from 68.5 to 105.1%. Therefore, the graphenized pencil lead fiber provides a high performance, cheap, robust, and reliable tool for SPME. PMID:24332350

  4. Dispersive Liquid-Liquid Microextraction for HPLC-UV Determination of PAHs in Milk.

    PubMed

    Mahmoudpour, Mansour; Mohtadinia, Javad; Ansarin, Masood; Nemati, Mahboob

    2016-03-01

    A simple and rapid analytical method for the extraction and quantification of four polycyclic aromatic hydrocarbons in milk sample has been developed using dispersive liquid-liquid microextraction followed by the use of HPLC. Benzo(a)pyrene, benzo(a)anthracene, and benzo(b)fluoranthene were used as model compounds; the milk sample was spiked with these compounds to assess the extraction procedure. Experimental parameters that influence the extraction efficiency, including the nature and volume of the disperser and extraction solvents, pH, and the volume of milk sample, were optimized. Under the optimum extraction conditions (extraction solvent: chloroform, 200 μL; dispersive solvent: acetonitrile, 700 μL; and extraction time 5 s or less), the performance of the proposed method was evaluated. The chromatographic peak area was linear with concentrations in the range of 0.2-10 ng/mL(-1) and with correlation coefficients ranging from 0.9968 to 0.9985. The LODs, based on a S/N ratio of 3, ranged from 0.06 to 0.18 ng/mL(-1). The RSDs varied from 3.68 to 9.7% (n = 3). The recoveries of these compounds were from 88.38 to 100%. The performance of the present method was evaluated for the determination of polycyclic aromatic hydrocarbons in various types of milk samples. PMID:26960830

  5. Solid-phase microextraction to determine micropollutant-macromolecule partition coefficients.

    PubMed

    Bridle, Helen L; Heringa, Minne B; Schäfer, Andrea I

    2016-08-01

    Aqueous micropollutants such as estradiol can have a large environmental impact-even at low concentrations. Part of understanding this impact involves determining the extent to which the micropollutants interact with macromolecules in water. In environmental samples, relevant macromolecules to which micropollutants bind are referred to as dissolved organic matter, and the most common examples of these in freshwater and coastal seawater are fulvic and humic acids. In living organisms, the most common macromolecules that affect bioavailability of a drug (or toxin) are proteins such as albumin. Using [2, 4, 6, 7 - (3)H]estradiol as an example compound, this protocol uses solid-phase microextraction and scintillation detection as analytical tools to quantify the amount of radiolabeled micropollutant available in solution. The measured free concentration after exposure to various concentrations of macromolecule (dissolved organic matter or protein) or micropollutant is used to determine the partition coefficient in the case of micropollutant-macromolecule interactions. The calibration and preparatory studies take at least 8 d, and the steps to determine the partition coefficient can be completed within 3 d. The protocol could be modified such that nonlabeled compounds are studied; instead of detection of activity by a liquid scintillation counter (LSC), the compounds can be quantified using gas chromatography-mass spectrometry (GC-MS) or liquid chromatography (LC)-MS(/MS). PMID:27362336

  6. Cooling/heating-assisted headspace solid-phase microextraction of polycyclic aromatic hydrocarbons from contaminated soils.

    PubMed

    Ghiasvand, Ali Reza; Pirdadeh-Beiranvand, Masoumeh

    2015-11-01

    A simple, low-cost, and effective cooling/heating-assisted headspace solid-phase microextraction (CHA-HS-SPME) device, capable of direct cooling the fiber to low temperatures and simultaneous heating the sample matrix to high temperatures, was fabricated and evaluated. It was able to cool down the commercial and handmade fibers for the effective tapping of volatile and semi-volatile species in the headspace of complex solid matrices, with minimal manipulation compared with conventional SPME. The CHA-HS-SPME system can create large temperature gaps (up to 200 °C) between the fiber and the sample matrix, because the cooling process is directly applied onto the fiber. Different effective experimental parameters for the fabrication of the CHA-HS-SPME device as well as for the extraction and determination of polycyclic aromatic hydrocarbons (PAHs) from solid samples were evaluated and optimized. The proposed device coupled to GC-FID was successfully applied for the extraction and determination of PAHs in contaminated soils without any sample pretreatment step. Good agreement was observed between the results obtained by the proposed CHA-HS-SPME-GC-FID method and those achieved by validated method. PMID:26572839

  7. Multivariate optimization of the factors influencing the solid-phase microextraction of pyrethroid pesticides in water.

    PubMed

    Casas, Vanessa; Llompart, Maria; García-Jares, Carmen; Cela, Rafael; Dagnac, Thierry

    2006-08-18

    A method based on solid-phase microextraction (SPME) and gas chromatography with micro-electron capture detection (GC-microECD) has been optimized for the analysis of pyrethroids in water samples. The influence of parameters such as temperature, fibre coating, salting-out effect and sampling mode on the extraction efficiency has been studied by means of a mix-level factorial design, which allowed the study of main effects as well as two factor interactions. Finally, a method based on direct SPME at 50 degrees C, using polydimethylsiloxane fibre is proposed. The method showed good linearity (R2>0.995) and repeatability (RSD

  8. Solid-phase microextraction gas chromatography-mass spectrometry determination of fragrance allergens in baby bathwater.

    PubMed

    Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2009-07-01

    A method based on solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized for the determination of fragrance allergens in water samples. This is the first study devoted to this family of cosmetic ingredients performed by SPME. The influence of parameters such as fibre coating, extraction and desorption temperatures, salting-out effect and sampling mode on the extraction efficiency has been studied by means of a mixed-level factorial design, which allowed the study of the main effects as well as two-factor interactions. Excluding desorption temperature, the other parameters were, in general, very important for the achievement of high response. The final procedure was based on headspace sampling at 100 degrees C, using polydimethylsiloxane/divinylbenzene fibres. The method showed good linearity and precision for all compounds, with detection limits ranging from 0.001 to 0.3 ng mL(-1). Reliability was demonstrated through the evaluation of the recoveries in different real water samples, including baby bathwater and swimming pool water. The absence of matrix effects allowed the use of external standard calibration to quantify the target compounds in the samples. The proposed procedure was applied to the determination of allergens in several real samples. All the target compounds were found in the samples, and, in some cases, at quite high concentrations. The presence and the levels of these chemicals in baby bathwater should be a matter of concern. PMID:19458938

  9. A new interface for coupling solid phase microextraction with liquid chromatography.

    PubMed

    Chen, Yong; Sidisky, Leonard M

    2014-03-19

    A modified Rheodyne 7520 microsample injector was used as a new solid phase microextraction (SPME)-liquid chromatography (LC) interface. The modification was focused on the construction of a new sample rotor, which was built by gluing two sample rotors together. The new sample rotor was further reinforced with 3 pieces of stainless steel tubing. The enlarged central flow passage in the new sample rotor was used as a desorption chamber. SPME fiber desorption occurred in static mode. But all desorption solvent in the desorption chamber was injected into LC system with the interface. The analytical performance of the interface was evaluated by SPME-LC analysis of PAHs in water. At least 90% polycyclic aromatic hydrocarbons (PAHs) were desorbed from a polyacrylonitrile (PAN)/C18 bonded fuse silica fiber in 30s. And injection was completed in 20s. About 10-20% total carryovers were found on the fiber and in the interface. The carryover in the interface was eliminated by flushing the desorption chamber with acetonitrile at 1mL min(-1) for 2min. The repeatability of the method was from 2% to 8%. The limit of detection (LOD) was in the mid pg mL(-1) range. The linear ranges were from 0.1 to 100ng mL(-1). The new SPME-LC interface was reliable for coupling SPME with LC for both qualitative and quantitative analysis. PMID:24594813

  10. Ionic liquid based hollow fiber supported liquid phase microextraction of ultraviolet filters.

    PubMed

    Ge, Dandan; Lee, Hian Kee

    2012-03-16

    Hollow fiber protected liquid phase microextraction using an ionic liquid as supported phase and acceptor phase (IL-HF-LPME) is proposed for the determination of four ultraviolet (UV) filters (benzophenone, 3-(4-methylbenzylidene)-camphor, 2-hydroxy-4-methoxybenzophenone and 2,4-dihydroxybenzophenone) in water samples for the first time. In the present study, four different ILs 1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate) [HMIM][FAP], 1-butyl-1-methylpyrrolidinium tris(pentafluoroethyl)trifluorophosphate [BMPL][FAP], 1-butyl-3-methylimidazolium phosphate ([BMIM][PO(4)]) and 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF(6)]) were evaluated as extraction solvent. Only [HMIM][FAP] showed high chemical affinity to the analytes which permits a selective isolation of the UV filters from the sample matrix, allowing also their preconcentration. IL-HF-LPME and high performance liquid chromatography provides repeatability from 1.1% to 8.2% and limits of detection between 0.3 and 0.5 ng/ml. Real water samples spiked with the analytes extracted were analyzed, and yielded relative recoveries ranging from 82.6% to 105.9%. PMID:22307149

  11. Determination of diphenylether herbicides in water samples by solid-phase microextraction coupled to liquid chromatography.

    PubMed

    Sheu, Hong-Li; Sung, Yu-Hsiang; Melwanki, Mahaveer B; Huang, Shang-Da

    2006-11-01

    Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, < 7%), correlation coefficient (> 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden. PMID:17313105

  12. Tailored micro-extraction method for Raman/SERS detection of indigoids in ancient textiles.

    PubMed

    Platania, Elena; Lofrumento, Cristiana; Lottini, Elisabetta; Azzaro, Elena; Ricci, Marilena; Becucci, Maurizio

    2015-08-01

    Indigoid dyes are well known as vat dyes. In their oxidized dichetonic form they are stable and insoluble in water, whereas in their reduced form, commonly known as leuco, they are soluble in water and able to be attached to fabric for dyeing purposes. These blue dyes are usually easily detectable in art objects by means of Raman spectroscopy by adopting for analyses a laser line at a high wavelength, such as a 785 nm diode laser. Unfortunately, in ancient artworks, that are often highly degraded, it is not always possible to collect high quality Raman spectra, which makes the analysis and identification of these compounds particularly challenging. In this work, we present a tailor-made methodology for the extraction and the recognition of indigoid dyes in works of art, which exploits the solubility of these compounds in their reduced form. Excellent Raman and surface enhanced Raman spectroscopy (SERS) spectra of indigo were acquired after micro-extraction on ancient and reference textiles, confirming the reliability of the presented procedure. Moreover, the methodology has been applied also for the extraction of the indigoid dye Tyrian purple on a reference textile, showing excellent results. This analytical method has been found to be extremely safe both for the reference textiles and the investigated ancient textiles, thus being a promising procedure for the selective analysis and detection of indigoid compounds in objects of artistic relevance. PMID:26082395

  13. [Solid phase microextraction (SPME) of sample preparation during of a complex biological matrix in biotransformation studies].

    PubMed

    Kroll, C; Borchert, H H

    1998-03-01

    Within the scope of the investigation of drug metabolism in keratinocytes solid phase microextraction (SPME) was investigated as a suitable method for sample preparation. The application of SPME is based on the fact, that a amount of analyte is absorbed by the polymer fiber at equilibrium, and the fiber is localized on a tip of a GC-syringe. The stable nitroxyl radical TEMPO (2,2,6,6-tetramthylpiperidine-1-oxyl) and its apolar metabolite 2,2,6,6-tetramethylpiperidine were analyzed by SPME and subsequent GC using thymol as internal standard. By means of the headspace-technique and an apolar fiber the recovery rate of TEMPO and the metabolite was nearly 100% and the precision was high. However, the results of the direct SPME were unsatisfactory. In comparison with conventional liquid/liquid extraction and solid phase extraction SPE the SPME proved the best results with regard to recovery rate and precision. Furthermore, the main advantages of SPME are the renunciation of organic solvents, the saving of time, the possibility to reuse the fiber about 100-150 times and the option for a complete automatisation of the extraction procedure. PMID:9547519

  14. Solid-phase microextraction fiber development for sampling and analysis of volatile organohalogen compounds in air.

    PubMed

    Attari, Seyed Ghavameddin; Bahrami, Abdolrahman; Shahna, Farshid Ghorbani; Heidari, Mahmoud

    2014-01-01

    A green, environmental friendly and sensitive method for determination of volatile organohalogen compounds was described in this paper. The method is based on a homemade sol-gel single-walled carbon nanotube/silica composite coated solid-phase microextraction to develop for sampling and analysis of Carbon tetrachloride, Benzotrichloride, Chloromethyl methyl ether and Trichloroethylene in air. Application of this method was investigated under different laboratory conditions. Predetermined concentrations of each analytes were prepared in a home-made standard chamber and the influences of experimental parameters such as temperature, humidity, extraction time, storage time, desorption temperature, desorption time and the sorbent performance were investigated. Under optimal conditions, the use of single-walled carbon nanotube/silica composite fiber showed good performance, high sensitive and fast sampling of volatile organohalogen compounds from air. For linearity test the regression correlation coefficient was more than 98% for analyte of interest and linear dynamic range for the proposed fiber and the applied Gas Chromatography-Flame Ionization Detector technique was from 1 to 100 ngmL(-1). Method detection limits ranged between 0.09 to 0.2 ngmL(-1) and method quantification limits were between 0.25 and 0.7 ngmL(-1). Single-walled carbon nanotube/silica composite fiber was highly reproducible, relative standard deviations were between 4.3 to 11.7 percent. PMID:25279223

  15. Ionic liquids-based crosslinked copolymer sorbents for headspace solid-phase microextraction of polar alcohols.

    PubMed

    Feng, Juanjuan; Sun, Min; Wang, Xusheng; Liu, Xia; Jiang, Shengxiang

    2012-07-01

    Halogen-based polymeric ionic liquid (PIL) fibers, which have proved efficient for solid-phase microextraction (SPME) of polar compounds, were with very limited fiber lifetimes. In this work, a novel crosslinked PIL sorbent with satisfactory stability and durability was prepared in situ via crosslinking polymerization processes on microstructured-silver coated stainless steel wire. 1,1'-(1,6-Hexanediyl)bis(1-vinylimidazolium) bibromide ionic liquid was synthesized and used as the crosslinking agent, with 1-vinyl-3-octylimidazolium bromide as monomer. Extraction properties of the fiber for polar alcohols in polar aqueous matrix were examined using headspace SPME (HS-SPME) coupled to gas chromatography-flame ionization detection (GC-FID). Under the optimized extraction and desorption conditions, the established method exhibited high extraction capacity. Wide linear ranges were obtained with correlation coefficients (R) ranging from 0.9947 to 0.9999. Limits of detection were in the range of 0.5-20 μg L⁻¹. Compared with the non-crosslinked PIL fiber, the proposed crosslinked PIL fiber was with higher thermal stability and durability and longer lifetime. Four different liquor beverages were analyzed as real samples and good results were obtained. PMID:22673810

  16. Extraction optimization of Loratadine by supramolecular solvent-based microextraction and its determination using HPLC.

    PubMed

    Peyrovi, Moazameh; Hadjmohammadi, Mohammadreza

    2015-02-01

    Optimization of supramolecular solvent-based microextraction (SSME) of Loratadine and its determination with high-performance liquid chromatography (HPLC) with ultra violet (UV) detection were investigated. A factorial design (FD) and a central composite face-centered (CCF) were applied to evaluate the SSME procedure. The effect of four parameters on extraction efficiency was investigated. The factors studied were decanoic acid amount, percentage of tetrahydrofuran (THF) (v/v), pH and extraction time. According to half factorial design results, the effective parameters were decanoic acid amount, THF percentage (v/v) and pH. Then, a CCF was applied to obtain optimal condition. The optimized conditions were obtained at 110mg of decanoic acid, 10% of THF and pH=3. The limits of detection were in the range of 0.3-0.4ng/ml. Linearity of the method was determined to be in the range of 1.0-400.0ng/ml for distilled water and 1.3-400.0ng/ml for plasma. The extraction recovery was >92%. RSD for intra and inter day (n=5) of extraction of Loratadine were 3.1% and 6.2%, respectively. The developed method was successfully applied for the determination of Loratadine in distilled water and plasma samples. PMID:25579114

  17. Volatiles fingerprint of Artemisia umbelliformis subsp. eriantha by headspace-solid phase microextraction GC-MS.

    PubMed

    Reale, Samantha; Pace, Loretta; D'Archivio, Angelo Antonio; De Angelis, Francesco; Marcozzi, Giordana

    2014-01-01

    Artemisia umbelliformis subsp. eriantha is a protected species, whose essential oil is used in liqueur industry. Volatile profiles of fresh leaves and flowers from wild plants in comparison with regenerated in vitro plants introduced in experimental fields within an Italian national park were evaluated by headspace-solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GC-MS). The chromatographic profiles appear to be qualitatively similar. The content of thujones, the characteristic metabolites of this species, is comparable with that obtained by analysis of essential oils. Principal component analysis of the HS-SPME-GC-MS data supports the possibility of differentiating scent blends of genetically identical plants, and even flowers and leaves from the same individual. HS-SPME-GC-MS is shown to be a very efficient method to analyse and to describe the pattern of components of A. umbelliformis subsp. eriantha cultivars' scents. It represents a rapid screening method highly recommended for the study of protected species, because it is non-destructive and it only requires small amounts of fresh material. PMID:23962361

  18. Dispersive liquid-liquid microextraction of thiram followed by microvolume UV-vis spectrophotometric determination.

    PubMed

    Rastegarzadeh, Saadat; Pourreza, Nahid; Larki, Arash

    2013-10-01

    A novel and simple method for the sensitive determination of trace amounts of fungicide thiram is developed by combination of dispersive liquid-liquid microextraction (DLLME) and microvolume UV-vis spectrophotometry. The method is based on the conversion of thiram to a yellow product in the presence of ethanolic potassium hydroxide and copper sulfate, and its extraction into CCL4 using DLLME technique. In this method the ethanol existing in ethanolic KOH plays as disperser solvent and a cloudy solution is formed by injection of only CCl4 as extractant solvent into sample solution. Under the optimum conditions, the calibration graph was linear over the range of 25-1000 ng mL(-1) of thiram with limit of detection of 11.5 ng mL(-1). The relative standard deviation (RSD) for 100 and 500 ng mL(-1) of thiram was 2.7 and 1.1% (n=8), respectively. The proposed method was successfully applied to determination of thiram in water and plant seed samples. PMID:23756257

  19. Determination of aromatic compounds in water by solid phase microextraction and ultraviolet absorption spectroscopy. 1. Methodology

    SciTech Connect

    Wittkamp, B.L.; Hawthorne, S.B.; Tilotta, D.C.

    1997-03-15

    A simple method is described for determining aromatic compounds (i.e., benzene, toluene, ethylbenzene, etc.) in water that combines solid phase microextraction (SPME) and ultraviolet (UV) absorption spectroscopy. The extraction medium consists of a small `chip` of poly(dimethylsiloxane) (total volume of nearly 80 {mu}L) that is immersed in a water sample contaminated with an aromatic compound. Equilibrium is first allowed to establish between the analyte in the water and the extraction medium, and the concentration of the aromatic compound is then determined directly in the sorbent chip by UV spectroscopy. Calibration information on this new method was obtained for 11 aromatic compounds commonly found in unleaded gasoline (e.g., benzene, toluene, naphthalene, etc). It was found that equilibrium is established in the range of 30-50 min, with the exception of 1-methylnaphthalene and naphthalene, which equilibrated within 100 min. Detection limits for the aromatic compounds at their equilibration times range from 0.40 to 12 ppb except for benzene (97 ppb). Relative standard deviations of the SPME-UV measurements are 3-12%. 17 refs., 3 figs., 5 tabs.

  20. Headspace Solid-phase Microextraction for the Determination of Volatile Organic Compounds in Larix Gmelini Particles

    NASA Astrophysics Data System (ADS)

    Liu, Y.; Shen, J.; Zhu, X. D.

    As an important bio-material, volatile organic compounds (VOCs) emissions of wood composites have increasing more concerns. The headspace solid-phase microextraction (HSSPME) was used to extract the VOCs emissions from larix gmelini particles. The HSSPME procedure was compared to conventional static headspace (HS) analysis for the VOCs emissions. Both methods gave the similar results, but the HSSPME was much more sensitive and exhibited better precision. Several parameters of the extraction and desorption procedure were studied and optimized (such as extraction temperature, extraction time, adsorption time, desorption time). The optimal parameters were obtained as extraction temperature 60 °C, extraction time 40 min, adsorption time 30 min and desorption time 40 min.The components of VOCs emissions in the samples were identified according to the GC-MS total ion chromatograms. The characteristic emissions obtained by HSSPME-GC-MS were alpha-pinene, beta-phellandrene, hexanal and 3- carene. Being a rapid, simple and practically non-interfering technique, HSSPME was successfully applied to analyze VOCs emissions in wood-composites.

  1. Oxygenated hydrocarbons in ambient air: Methods and measurements using solid-phase microextraction

    SciTech Connect

    Zhou, J.; McLaren, R.

    1999-07-01

    A method is described for the measurement of oxygenated and aromatic hydrocarbons in ambient air that combines the use of solid-phase microextraction with GC-MS. The method has proven to be sensitive enough to measure a range of species above the detection limit at urban and rural locations. Advantages and disadvantages of the method are discussed following the discussion of calibration and measurement methods. Measured mixing ratios are reported for oxygenated and aromatic hydrocarbons in the urban city of Toronto and at a rural forested site in Borden, Ontario. Correlations between different species are used to identify possible sources. At the Borden site, measurements at two levels on a tower through the forest canopy are used to discuss possible sources of species at that site. A unifying theme for both sites is the observation of similar and high median levels of methanol, acetone and acetaldehyde. The comparison of data from the urban and forested sites in this study do not provide evidence for a significant biogenic source of methanol as seen in the southern USA, although it is not discounted.

  2. Solid-phase microextraction may catalize hydrogenation when using hydrogen as carrier in gas chromatography.

    PubMed

    Fiorini, D; Boarelli, M C

    2016-07-01

    When hydrogen is used as carrier gas, carbon-carbon double bonds may be hydrogenated in the hot gas chromatograph (GC) injector if introduced by solid-phase microextraction (SPME). SPME fibers coated with polydimethylsiloxane (PDMS)/carboxen/divinylbenzene (DVB), PDMS/carboxen, polyacrylate, PDMS/DVB and PDMS on fused silica, stableflex or metal alloy core have been tested with fatty acid methyl esters (FAMEs) from olive oil. Using coatings containing DVB, hydrogenation took place with high conversion rates (82.0-92.9%) independently of the core material. With all fibers having a metal core, hydrogenation was observed to a certain extent (27.4-85.3%). PDMS, PDMS/carboxen and polyacrylate coated fibers with a fused silica or stableflex core resulted in negligible hydrogenation (0.2-2.5%). The occurrence of hydrogenation was confirmed also with other substances containing carbon-carbon double bonds (n-alkenes, alkenoic acids, mono- and polyunsaturated fatty acid methyl and ethyl esters). PMID:27236484

  3. Knitting aromatic polymers for efficient solid-phase microextraction of trace organic pollutants.

    PubMed

    Liu, Shuqin; Hu, Qingkun; Zheng, Juan; Xie, Lijun; Wei, Songbo; Jiang, Ruifen; Zhu, Fang; Liu, Yuan; Ouyang, Gangfeng

    2016-06-10

    A series of knitting aromatic polymers (KAPs) were successfully synthesized using a simple one-step Friedel-Crafts alkylation of aromatic monomers and were characterized by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, and X-ray photoelectron spectroscopy (XPS). Then, as-synthesized KAPs with large surface areas, unique pore structures and high thermal stability were prepared as solid-phase microextraction (SPME) coatings that exhibited good extraction abilities for a series of benzene compounds (i.e., benzene, toluene, ethylbenzene and m-xylene, which are referred to as BTEX) and polycyclic aromatic hydrocarbons (PAHs). Under the optimized conditions, the methodologies established for the determination of BTEX and PAHs using the KAPs-triPB and KAPs-B coatings, respectively, possessed wide linear ranges, low limits of detection (LODs, 0.10-1.13ngL(-1) for BTEX and 0.05-0.49ngL(-1) for PAHs) and good reproducibility. Finally, the proposed methods were successfully applied to the determination of BTEX and PAHs in environmental water samples, and satisfactory recoveries (93.6-124.2% for BTEX and 77.2-113.3% for PAHs) were achieved. This study provides a benchmark for exploiting novel microporous organic polymers (MOPs) for SPME applications. PMID:27155913

  4. Biocompatible Solid-Phase Microextraction Nanoelectrospray Ionization: An Unexploited Tool in Bioanalysis.

    PubMed

    Gómez-Ríos, Germán Augusto; Reyes-Garcés, Nathaly; Bojko, Barbara; Pawliszyn, Janusz

    2016-01-19

    In recent years, different geometrical configurations of solid-phase microextraction (SPME) have been directly coupled to mass spectrometry, resulting in benefits such as diminishing matrix effects, improvement of detection limits, and considerable enhancement of analysis throughput. Although SPME fibers have been used for years, their potential for quantitative analysis when directly combined with mass spectrometry has not been explored to its full extent. In this study, we present the direct coupling of biocompatible SPME (Bio-SPME) fibers to mass spectrometry via nanoelectrospray ionization (nano-ESI) emitters as a powerful tool for fast quantitative analysis of target analytes in biofluids. Total sample preparation time does not exceed 2 min, and by selecting an appropriate fiber length and sample vessel, sample volumes ranging between 10 and 1500 μL can be used. Despite the short extraction time of the technique, limits of detection in the subnanogram per milliliter with good accuracy (≥90%) and linearity (R(2) > 0.999) were attained for all the studied probes in phosphate-buffered saline (PBS), urine, and whole blood. Given that Bio-SPME-nano-ESI efficiently integrates sampling with analyte extraction/enrichment, sample cleanup (including elimination of matrix effects in the form of particles), and ionization, our results demonstrated that it is an advantageous configuration for bioanalytical applications such as therapeutic drug monitoring, doping in sports, and pharmacological studies in various matrixes. PMID:26648347

  5. Electrodeposited apatite coating for solid-phase microextraction and sensitive indirect voltammetric determination of fluoride ions.

    PubMed

    Mao, Yuehong; Chen, Yufei; Chu, Lin; Zhang, Xiaoli

    2013-10-15

    Electrodeposition was used to prepare a new solid phase microextraction (SPME) coatings. Two apatite SPME coatings, dicalcium phosphate dihydrate (DCPD or brushite) and hydroxyapatite (HAP) were validly and homogeneously one-step electrodeposited on glassy carbon electrode (GCE) under different conditions. The coatings were characterized by XRD, FTIR, SEM, CV and EIS. The apatite SPME coatings showed excellent and selective adsorbability to fluoride ions. A novel indirect voltammetric strategy for sensitive detection of fluoride was proposed using K3Fe(CN)6 as indicating probe. The detection principle of fluoride ions was based on the increment of steric hindrance after fluoride adsorption, which resulting in the decrease of the amperometric signal to Fe(CN)6(3-). The liner ranges were 0.5-20.0 μmol/L for n-DCPD/GCE with the limit of detection of 0.14 μmol/L and 0.1-50.0 μmol/L for n-HAP/GCE with the limit of detection of 0.069 μmol/L, respectively. The developed method was applied to the analysis of water samples (lake, spring and tap water) and the recovery values were found to be in the range of 90-106%. PMID:24054624

  6. Magnetism-Enhanced Monolith-Based In-Tube Solid Phase Microextraction.

    PubMed

    Mei, Meng; Huang, Xiaojia; Luo, Qing; Yuan, Dongxin

    2016-02-01

    Monolith-based in-tube solid phase microextraction (MB/IT-SPME) has received wide attention because of miniaturization, automation, expected loading capacity, and environmental friendliness. However, the unsatisfactory extraction efficiency becomes the main disadvantage of MB/IT-SPME. To overcome this circumstance, magnetism-enhanced MB/IT-SPME (ME-MB/IT-SPME) was developed in the present work, taking advantage of magnetic microfluidic principles. First, modified Fe3O4 nanoparticles were mixed with polymerization solution and in situ polymerized in the capillary to obtain a magnetic monolith extraction phase. After that, the monolithic capillary column was placed inside a magnetic coil that allowed the exertion of a variable magnetic field. The effects of intensity of magnetic field, adsorption and desorption flow rate, volume of sample, and desorption solvent on the performance of ME-MB/IT-SPME were investigated in detail. The analysis of six steroid hormones in water samples by the combination of ME-MB/IT-SPME with high-performance liquid chromatography with diode array detection was selected as a paradigm for the practical evaluation of ME-MB/IT-SPME. The application of a controlled magnetic field resulted in an obvious increase of extraction efficiencies of the target analytes between 70% and 100%. The present work demonstrated that application of different magnetic forces in adsorption and desorption steps can effectively enhance extraction efficiency of MB/IT-SPME systems. PMID:26742590

  7. Polythiophene as a novel fiber coating for solid-phase microextraction.

    PubMed

    Li, Xiang; Li, Chunmei; Chen, Jianmin; Li, Chunlei; Sun, Cheng

    2008-07-11

    The efficiency of polythiophene (PTh) was investigated as a new fiber for solid-phase microextraction (SPME). The PTh film was directly electrodeposited on the surface of a stainless steel wire in boron trifluoride diethyl etherate (BFEE) solution using cyclic voltammetry (CV) technique. PTh fibers were used for the extraction of some organochlorine pesticides (OCPs) from water samples. The extracted analytes were transferred to an injection port of gas chromatography using a laboratory-designed SPME device. The results obtained prove the ability of PTh material as a new fiber for sampling of organic compounds from water samples. This behavior is due most probably to the granulated surface of PTh film, which produces large surface areas. In this work, the optimum conditions for the preparation and conditioning of fibers and the extraction of analytes from water samples were obtained. In the optimum conditions, the limit of detection of the proposed method is 0.5-10 ng L(-1) for analysis of OCPs from aqueous samples, and the calibration graphs were linear in a concentration range of 10-10,000 ng L(-1) (R(2)>0.982) for most of organochlorine pesticides. Single fiber repeatability and fiber-to-fiber reproducibility were less than 12 and 18% (n=5), respectively. The PTh fiber was used to monitor the OCPs in real water samples, and the results compared favorably with the data determined by commercially available carbowax/divinylbenzene (CW/DVB) fiber. PMID:18533166

  8. Sequential dispersive liquid-liquid microextraction for the determination of aryloxyphenoxy-propionate herbicides in water.

    PubMed

    Li, Songqing; Gao, Peng; Zhang, Jiaheng; Li, Yubo; Peng, Bing; Gao, Haixiang; Zhou, Wenfeng

    2012-12-01

    A novel dispersive liquid-liquid microextraction (DLLME) method followed by HPLC analysis, termed sequential DLLME, was developed for the preconcentration and determination of aryloxyphenoxy-propionate herbicides (i.e. haloxyfop-R-methyl, cyhalofop-butyl, fenoxaprop-P-ethyl, and fluazifop-P-butyl) in aqueous samples. The method is based on the combination of ultrasound-assisted DLLME with in situ ionic liquid (IL) DLLME into one extraction procedure and achieved better performance than widely used DLLME procedures. Chlorobenzene was used as the extraction solvent during the first extraction. Hydrophilic IL 1-octyl-3-methylimidazolium chloride was used as a dispersive solvent during the first extraction and as an extraction solvent during the second extraction after an in situ chloride exchange by bis[(trifluoromethane)sulfonyl]imide. Several experimental parameters affecting the extraction efficiency were studied and optimized with the design of experiments using MINITAB® 16 software. Under the optimized conditions, the extractions resulted in analyte recoveries of 78-91%. The correlation coefficients of the calibration curves ranged from 0.9994 to 0.9997 at concentrations of 10-300, 15-300, and 20-300 μg L(-1). The relative SDs (n = 5) ranged from 2.9 to 5.4%. The LODs for the four herbicides were between 1.50 and 6.12 μg L(-1). PMID:23109344

  9. Gas-Purged Headspace Liquid Phase Microextraction System for Determination of Volatile and Semivolatile Analytes

    PubMed Central

    Zhang, Meihua; Bi, Jinhu; Yang, Cui; Li, Donghao; Piao, Xiangfan

    2012-01-01

    In order to achieve rapid, automatic, and efficient extraction for trace chemicals from samples, a system of gas-purged headspace liquid phase microextraction (GP-HS-LPME) has been researched and developed based on the original HS-LPME technique. In this system, semiconductor condenser and heater, whose refrigerating and heating temperatures were controlled by microcontroller, were designed to cool the extraction solvent and to heat the sample, respectively. Besides, inert gas, whose gas flow rate was adjusted by mass flow controller, was continuously introduced into and discharged from the system. Under optimized parameters, extraction experiments were performed, respectively, using GP-HS-LPME system and original HS-LPME technique for enriching volatile and semivolatile target compounds from the same kind of sample of 15 PAHs standard mixture. GC-MS analysis results for the two experiments indicated that a higher enrichment factor was obtained from GP-HS-LPME. The enrichment results demonstrate that GP-HS-LPME system is potential in determination of volatile and semivolatile analytes from various kinds of samples. PMID:22448341

  10. Graphene coating bonded onto stainless steel wire as a solid-phase microextraction fiber.

    PubMed

    Sun, Min; Feng, Juanjuan; Bu, Yanan; Wang, Xiaojiao; Duan, Huimin; Luo, Chuannan

    2015-03-01

    A graphene coating bonded onto stainless steel wire was fabricated and investigated as a solid-phase microextraction fiber. The coating was characterized by scanning electron microscopy and energy-dispersive X-ray spectrometer. The coating with rough and crinkled structure was about 1 μm. These characteristics were helpful for promoting extraction. Using five n-alkanes (n-undecane, n-dodecane, n-tridecane, n-tetradecane and n-hexadecane) as analytes, the fiber was evaluated in direct-immersion mode by coupling with gas chromatography (GC). Through optimizing extraction and desorption conditions, a sensitive SPME-GC analytical method was established. SPME-GC method provided wide linearity range (0.2-150 μg L(-1)) and low limits of determination (0.05-0.5 μg L(-1)). It was applied to analyze rain water and a soil sample, and analytes were quantified in the range of 0.85-1.96 μg L(-1) and 0.09-3.34 μg g(-1), respectively. The recoveries of samples spiked at 10 μg L(-1) were in the range of 90.1-120% and 80.6-94.2%, respectively. The fiber also exhibited high thermal and chemical stability, due to the covalent bonds between graphene coating and wire, and the natural resistance of graphene for thermal, acid and basic conditions. PMID:25618658

  11. Dispersive liquid-liquid microextraction of thiram followed by microvolume UV-vis spectrophotometric determination

    NASA Astrophysics Data System (ADS)

    Rastegarzadeh, Saadat; Pourreza, Nahid; Larki, Arash

    2013-10-01

    A novel and simple method for the sensitive determination of trace amounts of fungicide thiram is developed by combination of dispersive liquid-liquid microextraction (DLLME) and microvolume UV-vis spectrophotometry. The method is based on the conversion of thiram to a yellow product in the presence of ethanolic potassium hydroxide and copper sulfate, and its extraction into CCL4 using DLLME technique. In this method the ethanol existing in ethanolic KOH plays as disperser solvent and a cloudy solution is formed by injection of only CCl4 as extractant solvent into sample solution. Under the optimum conditions, the calibration graph was linear over the range of 25-1000 ng mL-1 of thiram with limit of detection of 11.5 ng mL-1. The relative standard deviation (RSD) for 100 and 500 ng mL-1 of thiram was 2.7 and 1.1% (n = 8), respectively. The proposed method was successfully applied to determination of thiram in water and plant seed samples.

  12. Application of solid-phase microextraction for determining phenylurea herbicides and their homologous anilines from vegetables.

    PubMed

    Berrada, H; Font, G; Moltó, J C

    2004-07-01

    Residues of metobromuron, monolinuron and linuron herbicides and their aniline homologous were analyzed in carrots, onions and potatoes by solid-phase microextraction (SPME) performed with a polyacrylate fiber. A juice was obtained from food samples that were further diluted, and an aliquot was extracted after sodium chloride (14%) addition and pH control. At pH 4 only the phenylureas were extracted. A new extraction at pH 11 allowed the extraction of phenylureas plus homologous aniline metabolites. Determination was carried out by gas chromatography with nitrogen-phosporus detection (NPD) the identity of the determined compounds was studied by gas chromatography-mass spectrometry. Limits of quantification (LOQs) obtained with NPD and MS (selected-ion monitoring) were in the microg/kg order allowing determination of maximum residue levels (MRLs) established in the Spanish regulations. MRLs ranged from 0.02 to 0.1 mg/kg depending on the kind of food and herbicide. Under the proposed conditions matrix effects were low enough to permit calibration with samples proceeding from ecological (non-pesticide treated) crops. Twelve commercial samples of each carrots, onions and potatoes were analyzed and only three samples of potatoes contained residues of linuron at levels below MRLs. PMID:15296383

  13. [Analysis of emodin and its metabolites based on hollow fiber liquid phase microextraction].

    PubMed

    Tian, Jie; Chen, Xuan; Bai, Xiaohong

    2012-05-01

    Hollow fiber liquid phase microextraction (HFLPME) coupled with high performance liquid chromatography (HPLC) has been developed to analyze the emodin and its metabolites in plasma and urine samples. The abilities of the absorption and metabolism for the active components in traditional Chinese medicines between the male and female rats were compared, and the biological metabolism and transmutation of the analyte were detailed discussed. Emodin and its metabolites in plasma and urine samples were extracted into n-octanol (acceptor) in hollow fiber. The acceptor phase was dried and dissolved by 50 microL methanol and then analyzed by HPLC. Under the optimal conditions, the linearities of the analytes were all very good in biological samples (r > 0.9960), the detection limits of the analytes were within the ranges of 0.1-3.0 microg/L. The enrichment factors were 12.2 to 26.3. The relative standard deviations for intra-day and inter-day precision were lower than 11.0%. The average recoveries of the analytes in plasma and urine samples were all in the range of 97.9% to 103%. HFLPME-HPLC can eliminate interference from complex biological samples, improve the sensitivity and reduce the detection limit, thus this method is suitable for the determination of trace compounds in complex sample. PMID:22934415

  14. Solid-phase microextraction for cannabinoids analysis in hair and its possible application to other drugs.

    PubMed

    Strano-Rossi, S; Chiarotti, M

    1999-01-01

    This paper describes the application of solid-phase microextraction (SPME) to cannabis testing in hair. Fifty milligrams of hair was washed with petroleum ether, hydrolyzed with NaOH, neutralized, deuterated internal standard was added and directly submitted to SPME. The SPME was analyzed by GC-MS. The limit of detection was 0.1 ng/mg for cannabinol (CBN) and delta9-tetrahydrocannabinol (THC) and 0.2 ng/mg for cannabidiol (CBD). THC was detected in a range spanning from 0.1 to 0.7 ng/mg. CBD concentrations ranged from 0.7 to 14.1 ng/mg, and CBN concentrations ranged from 0.4 to 0.7 ng/mg. The effectiveness of different decontamination procedures was also studied on passively contaminated hair. The proposed method is also suitable for the analysis of methadone in hair; cocaine and cocaethylene can be detected in hair with SPME extraction after enzymatic hydrolysis. PMID:10022202

  15. Ionic liquid coated copper wires and tubes for fiber-in-tube solid-phase microextraction.

    PubMed

    Sun, Min; Feng, Juanjuan; Bu, Yanan; Luo, Chuannan

    2016-08-01

    A fiber-in-tube solid-phase microextraction (SPME) device was developed by filling eleven copper wires into a copper tube, and all of those were functionalized with ionic liquids. Its morphology and surface properties were characterized by scanning electron microscopy. It was connected into high performance liquid chromatography (HPLC) equipment by replacing the sample loop of six-port injection valve, building the online SPME-HPLC system. In the optimization of extraction conditions, sampling rate, sample volume, pH of sample and desorption time were investigated with five estrogens as model analytes. Under the optimum conditions, an online SPME-HPLC analysis method was achieved, showing enrichment efficiency from 611 to 1661 and a good linearity of 0.06-60μgL(-1) with low detection limits of 0.02-0.05μgL(-1). It was applied to detect estrogens analytes in two water samples, with recoveries in the range of 85-114%. Relative standard deviation (n=3) of extraction repeatability is in the range of 1.9-3.0%. Relative standard deviation of extraction tubes (n=3) is in the range of 12-19%. The extraction mechanism is probably related to hydrophobic, π-π and dipole-dipole interactions between ionic liquids coating and estrogens analytes. PMID:27381811

  16. Characterisation of whiskeys using solid-phase microextraction with gas chromatography-mass spectrometry.

    PubMed

    Fitzgerald, G; James, K J; MacNamara, K; Stack, M A

    2000-10-27

    The application of solid-phase microextraction and gas chromatography-mass spectrometry to the detection of flavour volatiles present in Irish and Scottish whiskeys was investigated. A method was developed to characterise these volatiles which included the extraction, identification and quantification of 17 congeners which included fusel alcohols, acetates and esters. The method validation produced the optimum fibre [85 microm poly(acrylate)], extraction time (35 min), sample volume size (3 ml) and desorption time (5 min). The impact of salt on the absorption process was also studied. Characteristic profiles were determined for each whiskey and the flavour congeners were quantified using 4-methyl-2-pentanol as the internal standard. Calibration ranges were determined for each of the congeners with coefficients of linearity ranging from 0.993 (butan-1-ol) to 0.999 (ethyl laurate) and relative standard deviations ranging from 2.5% (2-methylbutan-1-ol) to 21% (furfural) at a concentration of 18.2 mg/l. Detection limits ranged from 0.1 mg/l (ethyl caprate) to 21 mg/l (butan-2-ol). PMID:11093670

  17. SOLID PHASE MICROEXTRACTION SAMPLING OF FIRE DEBRIS RESIDUES IN THE PRESENCE OF RADIONUCLIDE SURROGATE METALS

    SciTech Connect

    Duff, M; Keisha Martin, K; S Crump, S

    2007-03-23

    The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating highly radioactive fire debris (FD) evidence while maintaining evidentiary value. One experimental method for the isolation of FD residue from radionuclide metals involves using solid phase microextraction (SPME) fibers to remove the residues of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most (radioactive) metals. The focus of this research was to develop an examination protocol that was applicable to safe work in facilities where high radiation doses are shielded from the workers (as in radioactive shielded cells or ''hot cells''). We also examined the affinity of stable radionuclide surrogate metals (Co, Ir, Re, Ni, Ba, Cs, Nb, Zr and Nd) for sorption by the SPME fibers. This was done under exposure conditions that favor the uptake of FD residues under conditions that will provide little contact between the SPME and the FD material (such as charred carpet or wood that contains commonly-used accelerants). Our results from mass spectrometric analyses indicate that SPME fibers show promise for use in the room temperature head space uptake of organic FD residue (namely, diesel fuel oil, kerosene, gasoline and paint thinner) with subsequent analysis by gas chromatography (GC) with mass spectrometric (MS) detection. No inorganic forms of ignitable fluids were included in this study.

  18. Evaluation of solid-phase microextraction in detection of contraband drug vapors

    NASA Astrophysics Data System (ADS)

    Orzechowska, Grazyna E.; Poziomek, Edward J.; Tersol, Vangielynn; Homstead, Juliana

    1997-02-01

    Solid phase microextraction (SPME) has emerged as a rapid alternative to conventional sample extraction techniques. SPME can be used in solids, liquids, and sample headspace. Compounds are sorbed by a stationary phase coated on a fused silica fiber. The compounds are desorbed, and analyzed using gas chromatography (GC), and high performance liquid chromatography (HPLC). As a part of the present work we have found that SPME can also be used conveniently with ion mobility spectrometry (IMS). Cocaine and heroin vapors sorbed on a SPME fiber were detected using IMS. The use of SPME-GC or SPME-HPLC has been reported in analysis of urine samples containing cocaine and its metabolites. We are evaluating SPME-IMS, and SPME-GC systems for the detection of cocaine and heroin and their decomposition products in the headspace above surfaces. This is part of our research on the surface decomposition of contraband drugs for detection applications. This paper will give a variety of examples in the use of SPME in the detection of contraband drugs and their reaction/decomposition products in the vapor state. An example is the detection of cocaine in the headspace above cocaine HCl at room temperature.

  19. Determination of Trace Levels of Irgarol in Estuarine Water Matrices by Bar Adsorptive Microextraction.

    PubMed

    Calado, Bruno Boto; Ahmad, Samir Marcos; Almeida, Carlos; Neng, Nuno da Rosa; Nogueira, José Manuel Florêncio

    2016-09-01

    Bar adsorptive microextraction (BAµE), using selective sorbent phases, followed by liquid desorption in combination with large volume injection-gas chromatography coupled to mass spectrometry (BAµE-LD/LVI-GC-MS), is proposed for the determination of trace levels of irgarol in estuarine water matrices. While we compared several polymers and activated carbons, one of the latter coatings showed much higher selectivity through BAµE. Assays performed on 25 mL of ultra-pure water sample fortified at 0.6 µg/L levels of irgarol yielded recoveries of 74.5 ± 8.6%, under optimized experimental conditions. The proposed analytical procedure showed convenient detection limits (16.0 ng/L) and good linear dynamic range (0.2-16.0 µg/L), with determination coefficients of 0.9982. Good precision was also achieved with RSD lower than 12.0%. The application of the present analytical approach on estuarine water samples by using the standard addition methodology revealed good sensitivity and linearity. The proposed methodology, using nanostructured sorbents and operating under the floating sampling technology, proved to be a suitable analytical alternative to monitor irgarol in estuarine water matrices. Moreover, it is easy to implement, reliable, sensitive, require low sample volume and have the possibility to choose the most selective sorbent coating according to the target compound involved. PMID:27207994

  20. Aflatoxin B1 in eggs and chicken livers by dispersive liquid-liquid microextraction and HPLC.

    PubMed

    Amirkhizi, Behzad; Arefhosseini, Seyed Rafie; Ansarin, Masoud; Nemati, Mahboob

    2015-01-01

    A rapid, low-cost and simple technique has been developed for the determination of aflatoxin B1 (AFB1) in eggs and livers using high-performance liquid chromatography (HPLC) with UV detection. In this study, the presence of AFB1 was investigated in 150 eggs and 50 chicken livers from the local market of Tabriz, Iran. AFB1 was extracted with a mixture of acetonitrile:water (80:20) and cleaned up by dispersive liquid-liquid microextraction which is a very economical, fast and sensitive method. AFB1 was quantified by HPLC-UV without need for any complex derivatisation in samples to enhance the detection. The results showed that 72% of the liver and 58% of the egg samples were contaminated with AFB1 ranging from 0.30 to 16.36 µg kg (̶1). limit of detection and limit of quantification for AFB1 were 0.08 and 0.28 µg kg (̶ 1), respectively. The proposed method is suitable for fast analysing of AFB1 in egg and liver samples. PMID:26160230

  1. A strategy to enhance the antifouling property of coating for direct immersion solid phase microextraction.

    PubMed

    Wu, Mian; Zhang, Haibo; Zeng, Baizhao; Zhao, Faqiong

    2015-03-01

    This paper presents a new approach for improving the antifouling property of solid-phase microextraction (SPME) coating. The SPME fiber was fabricated by electrodeposition of polyaniline (PANI) on stainless steel wire, followed by covering with an external layer of Nafion. The Nafion layer was able to block the interfering components in the matrix while the fiber was used for the direct extraction of several parabens. At the same time, the selectivity and stability of the SPME fiber was also improved. The adsorption coefficient and saturation-adsorption amount were determined, which showed that the extraction capability of the resulting fiber was similar to that of the original PANI fiber toward parabens. In addition, the fiber exhibited enhanced robustness in direct contact with complex matrix such as orange juice. After it was used for 110-150 adsorption-desorption cycles, its extraction efficiency decreased by 14-16% compared with the maximum measured value. This was a dramatic improvement when compared with the PANI fiber. Hence, the fiber was suitable for direct immersion SPME. PMID:25650353

  2. Solid phase microextraction: measurement of volatile organic compounds (VOCs) in Dhaka City air pollution.

    PubMed

    Hussam, A; Alauddin, M; Khan, A H; Chowdhury, D; Bibi, H; Bhattacharjee, M; Sultana, S

    2002-08-01

    A solid phase microextraction (SPME) technique was applied for the sampling of volatile organic compounds (VOCs) in ambient air polluted by two stroke autorickshaw engines and automobile exhausts in Dhaka city, Bangladesh. Analysis was carried out by capillary gas chromatography (GC) and GC-mass spectrometry (MS). The methodology was tested by insitu sampling of an aromatic hydrocarbon mixture gas standard with a precision of +/-5% and an average accuracy of 1-20%. The accuracy for total VOCs concentration measurement was about 7%. VOC's in ambient air were collected by exposing the SPME fiber at four locations in Dhaka city. The chromatograms showed signature similar to that of unburned gasoline (petrol) and weathered diesel containing more than 200 organic compounds; some of these compounds were positively identified. These are normal hydrocarbons pentane (n-C5H2) through nonacosane (n-C29H60), aromatic hydrocarbons: benzene, toluene, ethylbenzene, n-propylbenzene, n-butylbenzene, 1,3,5-trimethylbenzene, xylenes, and 1-isocyanato-3-methoxybenzene. Two samples collected near an autorickshaw station contained 783000 and 1479000 microg/m3 of VOCs. In particular, the concentration of toluene was 50-100 times higher than the threshold limiting value of 2000 microg/m3. Two other samples collected on street median showed 135000 microg/m3 and 180000 microg/m3 of total VOCs. The method detection limit of the technique for most semi-volatile organic compounds was 1 microg/m3. PMID:15328688

  3. Development and evaluation of a new in vivo solid-phase microextraction sampler.

    PubMed

    Togunde, Oluranti P; Lord, Heather; Oakes, Ken D; Servos, Mark R; Pawliszyn, Janusz

    2013-01-01

    The use of solid-phase microextraction (SPME) as a nonlethal technique for in vivo sampling of pharmaceutical residue in fish tissue has been documented in the literature. However, there is need to improve its simplicity and robustness for wider applications in the laboratory and field. The objective of this research is to develop and improve the SPME device for sampling of pharmaceuticals in fish tissue. The practical application of the new device was demonstrated in the field where some wild fish (Esox masquinongy) were caught in the river and sampled by the device. The samples were analyzed using LC coupled with MS/MS (LC-MS/MS). The new in vivo SPME device with a PDMS extraction phase (sorbent) was demonstrated to a robust tool by both experts and nonexpert of the method and it is simpler than the traditional device. The detection limit of the method in gel and fish tissue was 0.01-0.26 ng/g. The interday reproducibility in gel and fish homogenized fish tissue was 8-16% RSD. This study demonstrates that the new device will provide a platform or opportunity for rapid sampling of carbamazepine, diazepam, and nordiazepam in fish muscle with acceptable precision. PMID:23255404

  4. Graphene-coated fiber for solid-phase microextraction of triazine herbicides in water samples.

    PubMed

    Wu, Qiuhua; Feng, Cheng; Zhao, Guangying; Wang, Chun; Wang, Zhi

    2012-01-01

    Graphene is a novel and interesting carbon material that could be used for the separation and purification of some chemical compounds. In this investigation, graphene was used as a novel fiber-coating material for the solid-phase microextraction (SPME) of four triazine herbicides (atrazine, prometon, ametryn and prometryn) in water samples. The main parameters that affect the extraction and desorption efficiencies, such as the extraction time, stirring rate, salt addition, desorption solvent and desorption time, were investigated and optimized. The optimized SPME by graphene-coated fiber coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) was successfully applied for the determination of the four triazine herbicides in water samples. The linearity of the method was in the range from 0.5 to 200 ng/mL, with the correlation coefficients (r) ranging from 0.9989 to 0.9998. The limits of detection of the method were 0.05-0.2 ng/mL. The relative standard deviations varied from 3.5 to 4.9% (n=5). The recoveries of the triazine herbicides from water samples at spiking levels of 20.0 and 50.0  ng/mL were in the range between 86.0 and 94.6%. Compared with two commercial fibers (CW/TPR, 50 μm; PDMS/DVB, 60 μm), the graphene-coated fiber showed higher extraction efficiency. PMID:22162195

  5. Use of solid phase microextraction to estimate toxicity: relating fiber concentrations to toxicity--part I.

    PubMed

    Ding, Yuping; Landrum, Peter F; You, Jing; Harwood, Amanda D; Lydy, Michael J

    2012-09-01

    Use of solid-phase microextraction (SPME) fibers as a dose metric for toxicity testing was evaluated for hydrophobic pesticides to the midge Chironomus dilutus and the amphipod Hyalella azteca. Test compounds included p,p'-dichlorodiphenyltrichloroethane (p,p'-DDT), p,p'-dichlorodiphenyldichloroethane (p,p'-DDD), p,p'-dichlorodiphenyldichloroethylene (p,p'-DDE), permethrin, bifenthrin, tefluthrin, and chlorpyrifos. Acute water toxicity tests were determined for 4- and 10-d exposures in both species. Median lethal and sublethal concentrations were expressed both on a water concentration (LC50 and EC50) and on an equilibrium SPME fiber concentration (LC50(fiber) and EC50(fiber)) basis. A significant log dose-response relationship was found between log fiber concentration and organism mortality. It has been shown in the literature that equilibrium SPME fiber concentrations reflect the bioavailable concentrations of hydrophobic contaminants, so these fiber concentrations should be a useful metric for assessing toxic effects from the bioavailable contaminant providing a framework to expand the use of SPME fibers beyond estimation of bioaccumulation. PMID:22767390

  6. Assessing bioavailability and toxicity of permethrin and DDT in sediment using matrix solid phase microextraction.

    PubMed

    Ding, Yuping; Landrum, Peter F; You, Jing; Lydy, Michael J

    2013-01-01

    Matrix solid phase microextraction (matrix-SPME) was evaluated as a surrogate for the absorbed dose in organisms to estimate bioavailability and toxicity of permethrin and dichlorodiphenyltrichloroethane (DDT) in laboratory-spiked sediment. Sediments were incubated for 7, 28, and 90 days at room temperature to characterize the effect of aging on bioavailability and toxicity. Sediment toxicity was assessed using two freshwater invertebrates, the midge Chironomus dilutus and amphipod Hyalella azteca. Disposable polydimethylsiloxane fibers were used to estimate the absorbed dose in organisms and to examine bioavailability and toxicity. The equilibrium fiber concentrations substantially decreased with an increase in sediment aging time, indicating a reduction in bioavailability. Based on median lethal fiber concentrations (fiber LC50), toxicity of permethrin was not significantly different among the different aging times. Due to the substantial degradation of DDT to dichlorodiphenyldichloroethane (DDD) in sediment, sediment toxicity to C. dilutus increased, while it decreased for H. azteca with extended aging times. A toxic unit-based fiber LC50 value represented the DDT mixture (DDT and DDD) toxicity for both species. Significant linear relationships were found between organism body residues and the equilibrium fiber concentrations for each compound, across aging times. The study suggested that the matrix-SPME fibers mimicked bioaccumulation in the organisms, and enabled estimation of body residues, and could potentially be used in environmental risk assessment across matrices (e.g. sediment and water) to measure bioavailability and toxicity of hydrophobic pesticides. PMID:23086182

  7. Investigation of the kinetic process of solid phase microextraction in complex sample.

    PubMed

    Jiang, Ruifen; Xu, Jianqiao; Lin, Wei; Wen, Sijia; Zhu, Fang; Luan, Tiangang; Ouyang, Gangfeng

    2015-11-01

    The presence of complex matrix in the aquatic system affects the environmental behavior of hydrophobic organic compounds (HOCs). In the current study, an automated solid-phase microextraction (SPME) desorption method was employed to study the effect of 2-hydroxypropyl-β-cyclodextrin (β-HPCD) on the kinetic process of 5 selected polyaromatic hydrocarbons (PAHs) desorbing from the fiber in aqueous sample. The results showed that the added β-HPCD facilitated the desorption rates of PAHs from SPME fiber coating, and the enhancement effect can be predicted by a proposed theoretical model. Based on this model, the kinetic parameters of organic compounds desorbing from the SPME fiber can be determined, and the calculated results showed good agreement with the experimental data. In addition, the effect of temperature on the desorption kinetic was investigated. The results found that the SPME desorption time constant increased as the sampling temperature elevated, and followed the Arrhenius equation. Also, the temperature facilitated the desorption of HOCs from the bound matrix so that increased the lability degrees of the bound compounds. Finally, a calibration method based on the proposed theoretical model was developed and applied for the analysis of unknown sample. PMID:26572846

  8. Highly porous silica-polyaniline nanocomposite as a novel solid-phase microextraction fiber coating.

    PubMed

    Gholivand, Mohammad B; Abolghasemi, Mir M; Fattahpour, Peyman

    2012-01-01

    A highly porous fiber-coated SBA-15/polyaniline material was prepared for solid-phase microextraction (SPME). The SBA-15/polyaniline nanocomposite was synthesized via chemical polymerization. The prepared SBA-15/polyaniline particles were analyzed by scanning electron microscopy analysis. The prepared nanomaterial was immobilized onto a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). In optimum conditions (extraction temperature 60°C, extraction time 40 min, ionic strength 20%, stirring rate: 500 rpm, desorption temperature 260°C, desorption time 2 min), the repeatability for one fiber (n=3), expressed as relative standard deviation (RSD%), was between 5.3 and 8.6% for the test compounds. For deionized water, spiked with selected PAHs, the detection limits for the studied compounds were between 2 and 20 pg/mL. PMID:22144100

  9. Preparation and characterization of porous carbon material-coated solid-phase microextraction metal fibers.

    PubMed

    Zhu, Fang; Guo, Jiaming; Zeng, Feng; Fu, Ruowen; Wu, Dingcai; Luan, Tiangang; Tong, Yexiang; Lu, Tongbu; Ouyang, Gangfeng

    2010-12-10

    Two kinds of porous carbon materials, including carbon aerogels (CAs), wormhole-like mesoporous carbons (WMCs), were synthesized and used as the coatings of solid-phase microextraction (SPME) fibers. By using stainless steel wire as the supporting core, six types of fibers were prepared with sol-gel method, direct coating method and direct coating plus sol-gel method. Headspace SPME experiments indicated that the extraction efficiencies of the CA fibers are better than those of the WMC fibers, although the surface area of WMCs is much higher than that of CAs. The sol-gel-CA fiber (CA-A) exhibited excellent extraction properties for non-polar compounds (BTEX, benzene, toluene, ethylbenzene, o-xylene), while direct-coated CA fiber (CA-B) presented the best performance in extracting polar compounds (phenols). The two CA fibers showed wide linear ranges, low detection limits (0.008-0.047μgL(-1) for BTEX, 0.15-5.7μgL(-1) for phenols) and good repeatabilities (RSDs less than 4.6% for BTEX, and less than 9.5% for phenols) and satisfying reproducibilities between fibers (RSDs less than 5.2% for BTEX, and less than 9.9% for phenols). These fibers were successfully used for the analysis of water samples from the Pearl River, which demonstrated the applicability of the home-made CA fibers. PMID:21074162

  10. Analysis of volatile components from Melipona beecheii geopropolis from Southeast Mexico by headspace solid-phase microextraction.

    PubMed

    Torres-González, Ahira; López-Rivera, Paulina; Duarte-Lisci, Georgina; López-Ramírez, Ángel; Correa-Benítez, Adriana; Rivero-Cruz, J Fausto

    2016-01-01

    A head space solid-phase microextraction method combined with gas chromatography-mass spectrometry was developed and optimised to extract and analyse volatile compounds of Melipona beecheii geopropolis. Seventy-three constituents were identified using this technique in the sample of geopropolis collected. The main compounds detected include β-fenchene (14.53-15.45%), styrene (8.72-9.98%), benzaldehyde (7.44-7.82%) and the most relevant volatile components presents at high level in the geopropolis were terpenoids (58.17%). PMID:26118891

  11. Investigation by solid-phase microextraction and gas chromatography/mass spectrometry of trail pheromones in ants.

    PubMed

    Tullio, Alessandra Di; Angelis, Francesco De; Reale, Samantha; Grasso, Donato A; Visicchio, Roberto; Castracani, Cristina; Mori, Alessandra; Moli, Francesco Le

    2003-01-01

    The Dufour's gland content of workers of two ant species of the genus Messor has been analyzed by solid-phase microextraction and gas chromatography with mass spectrometry (GC/MS). The structures of the compounds in the pheromonal mixtures have been determined. In both cases only one intact gland, inserted in a properly dimensioned capillary vial, is sufficient to produce a clean and fully interpretable GC/MS profile. It is worth noting that, for the first time in Messor ants, farnesol has been detected as a minor component of glandular secretion in Messor capitatus. PMID:12955735

  12. Optimization of headspace solid-phase microextraction for the determination of pesticide residues in vegetables and fruits.

    PubMed

    Chai, Meekin; Tan, Guanhuat; Lal, Asha

    2008-02-01

    A headspace solid-phase microextraction method has been developed for the determination of 8 pesticides in vegetables and fruits by using gas chromatography with an electron capture detector. Two types of fibers (polyacrylate, 85 microm and polydimethylsiloxane, 100 microm) have been assayed and compared. The main factors: extraction and desorption parameters, ionic strength, and the effects of dilution and organic solvents, were studied and optimized. The optimized procedures resulted in more than 80% recovery for all the investigated vegetable and fruit samples with RSD values below 10%. PMID:18270422

  13. Optimisation of specialty malt volatile analysis by headspace solid-phase microextraction in combination with gas chromatography and mass spectrometry.

    PubMed

    Vandecan, Sem M G; Saison, Daan; Schouppe, Nina; Delvaux, Filip; Delvaux, Freddy R

    2010-06-25

    The objective of this study was to develop a technique for analysing 14 flavour components, relevant for specialty malts. Therefore, a method was developed for the analysis of these components in dry ground malt using headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry. A procedure was optimised for the optimal amount of sample, fibre selection, extraction temperature and extraction time. Afterwards, the method was calibrated and validated by the quantification of the specialty malt flavour components in a colour, a caramel and a roasted malt. PMID:20541643

  14. Solid-phase microextraction coupled with high performance liquid chromatography: a complementary technique to solid-phase microextraction-gas chromatography for the analysis of pesticide residues in strawberries.

    PubMed

    Wang, Z; Hennion, B; Urruty, L; Montury, M

    2000-11-01

    Solid-phase microextraction coupled with high performance liquid chromatography has been studied for the analysis of methiocarb, napropamide, fenoxycarb and bupirimate in strawberries. The strawberries were blended and centrifuged. Then, an aliquot of the resulting extracting solution was subjected to solid-phase microextraction (SPME) on a 60 microns polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 45 min at room temperature. The extracted pesticides on the SPME fibre were desorbed into SPME/high performance liquid chromatography (HPLC) interface for HPLC analysis with diode-array detection (DAD). The method is organic solvent-free for the whole extraction process and is simple and easy to manipulate. The detection limits were shown to be at low microgram kg-1 level and the linear response covered the range from 0.05 to 2 mg kg-1 of pesticides in strawberries with a regression coefficient larger than 0.99. A good repeatability with RSDs between 2.92 and 9.25% was obtained, depending on compounds. PMID:11271705

  15. Speciation of AsIII and AsV in fruit juices by dispersive liquid–liquid microextraction and hydride generation-atomic fluorescence spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A new procedure was developed to speciate and quantify As(III) and As(V) in fruit juices. At pH 3.0, As(III) and ammonium pyrrolidine dithiocarbamate (APDC) formed a complex, which was extracted into carbon tetrachloride by dispersive liquid–liquid microextraction (DLLME) and subsequently quantified...

  16. Quantification of Selected Aroma-Active Compounds in Strawberries by Headspace Solid-Phase Microextraction Gas Chromatography and Correlation with Sensory Descriptive Analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Selected aroma-active compounds in strawberries were quantified using headspace solid-phase microextraction and gas chromatography. Ten strawberry cultivars grown in California and Oregon were studied. The standard curves were built in a synthetic matrix and quantification was achieved using multipl...

  17. Surface enhanced Raman spectroscopy hyphenated with surface microextraction for in-situ detection of polycyclic aromatic hydrocarbons on food contact materials.

    PubMed

    Zhang, Min; Zhang, Xiaoli; Shi, Yu-E; Liu, Zhen; Zhan, Jinhua

    2016-09-01

    Highly bioaccumulated polycyclic aromatic hydrocarbons (PAHs) have cause health concerns because of their carcinogenic properties. PAHs could migrate to food from contaminated food contact materials. In this study, a hyphenated technique combining surface enhanced Raman spectroscopy (SERS) with surface microextraction was developed for in-situ on site screening of PAHs on food contact materials. Methanol and 1-propanethiol-modified silver nanoparticles (PTH-Ag NPs) were used to perform the in-situ microextraction and detection of PAHs, respectively. The SERS spectra can be obtained by a portable Raman spectrometer. The vibration of the C-C bond of PTH at 1030cm(-1) was chosen as an internal standard peak. The PTH-Ag NPs showed high uniformity with an RSD of 2.96%. A plot of the normalized SERS intensity against fluoranthene concentration showed a linear relationship (R(2)=0.98). The detection limit could reach 0.27ngcm(-2). The in-situ microextraction-SERS hyphenated technique for the detection of three PAHs at five food contact materials was demonstrated. The method can be also applied to detect PAH mixtures. This in-situ microextraction-SERS hyphenated method demonstrated its ability to rapidly screen PAHs on contaminated food contact materials free from complex sample pretreatment. PMID:27343612

  18. Quantitative Analysis of Bisphenol A Leached from Household Plastics by Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (SPME-GC-MS)

    ERIC Educational Resources Information Center

    Johnson, Bettie Obi; Burke, Fernanda M.; Harrison, Rebecca; Burdette, Samantha

    2012-01-01

    The measurement of trace levels of bisphenol A (BPA) leached out of household plastics using solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS) is reported here. BPA is an endocrine-disrupting compound used in the industrial manufacture of polycarbonate plastic bottles and epoxy resin can liners. This experiment…

  19. MICROEXTRACTION OF NINE HALOACETIC ACIDS IN DRINKING WATER AT MICROGRAM PER LITER LEVELS WITH ELECTROSPRAY-MASS SPECTROMETRY OF STABLE ASSOCIATION COMPLEXES

    EPA Science Inventory

    Haloacetic acids are disinfection by-products of the chlorination of drinking water. This paper presents the analysis of all nine chloro- and bromo-haloacetic acids (HAA9) at sub- ug L-1 by microextraction with detection by electrospray mass spectrometry. The haloacetic acids are...

  20. SIMPLE METHOD FOR ESTIMATING POLYCHLORINATED BIPHENYL CONCENTRATIONS ON SOILS AND SEDIMENTS USING SUBCRITICAL WATER EXTRACTION COUPLED WITH SOLID-PHASE MICROEXTRACTION. (R825368)

    EPA Science Inventory

    A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a seale...

  1. Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

    PubMed

    Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

    2015-05-01

    A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (<10%) for phenols. Four real soil samples were analyzed by the proposed method to assess its applicability. Experimental results showed that the soil samples were free of our target compounds, and average recoveries were in the range of 87.9-110%. These findings indicate that accelerated solvent extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples. PMID:25676868

  2. On-line sample processing involving microextraction techniques as a front-end to atomic spectrometric detection for trace metal assays: a review.

    PubMed

    Miró, Manuel; Hansen, Elo Harald

    2013-06-11

    Within the last decade, liquid-phase microextraction (LPME) and micro-solid phase extraction (μSPE) approaches have emerged as substitutes for conventional sample processing procedures for trace metal assays within the framework of green chemistry. This review surveys the progress of the state of the art in simplification and automation of microextraction approaches by harnessing to the various generations of flow injection (FI) as a front end to atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS) or inductively coupled plasma atomic emission spectrometry or mass spectrometry (ICP-AES/MS). It highlights the evolution of flow injection analysis and related techniques as vehicles for appropriate sample presentation to the detector and expedient on-line matrix separation and pre-concentration of trace levels of metals in troublesome matrices. Rather than being comprehensive this review is aimed at outlining the pros and cons via representative examples of recent attempts in automating green sample preparation procedures in an FI or sequential injection (SI) mode capitalizing on single-drop microextraction, dispersive liquid-phase microextraction and advanced sorptive materials including carbon and metal oxide nanoparticles, ion imprinted polymers, superparamagnetic nanomaterials and biological/biomass sorbents. Current challenges in the field are identified and the synergetic combination of flow analysis, nanotechnology and metal-tagged biomolecule detection is envisaged. PMID:23708278

  3. Comparison of characteristic flavor and aroma volatiles in melons and standards using solid phase microextraction (SPME) and Stir Bar Sorptive Extraction (SBSE) with GC-MS.

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Stir bar sorptive extraction (SBSE) is a technique for extraction and analysis of organic compounds in aqueous matrices, similar in theory to solid phase microextraction (SPME). SBSE has been successfully used to analyze several organic compounds, including food matrices. When compared with SPME, ...

  4. HIGH LEVELS OF MONOAROMATIC COMPOUNDS LIMIT THE USE OF SOLID-PHASE MICROEXTRACTION OF METHYL TERTIARY BUTYL ETHER AND TERTIARY BUTYL ALCOHOL

    EPA Science Inventory

    Recently, two papers reported the use of solid-phase microextraction (SPME) with polydimethylsiloxane(PDMS)/Carboxen fibers to determine trace levels of methyl tertiary butyl ether (MTBE) and tertiary butyl alcohol (tBA) in water. Attempts were made to apply this technique to th...

  5. Evaluation of headspace solid-phase microextraction for analysis of phosphine residues in wheat.

    PubMed

    Ren, Yong Lin; Padovan, Benjamin; Desmarchelier, James M

    2012-01-01

    In headspace (HS) analysis, a fumigant is released from a commodity into a gas-tight container by grinding, heating, or microwaves. A new technique uses HS-solid-phase microextraction (SPME) for additional preconcentration of fumigant. HS-SPME was tested for detection of phosphine (PH3), chosen for examination because of its wide use on stored commodities. PH3 was applied to 50 g wheat in separate 250 mL sealed flasks, which were equipped either with a septum for conventional HS analysis or with one of four HS-SPME fibers [100 microm polydimethylsiloxane (PDMS), 85 microm carboxen (CAR)/PDMS, 75 microm CAR/PDMS, and 65 pm PDMS/divinylbenzene (DVB)]. The wheat was heated at 45 degrees C for 20 min. In conventional HS analysis, a gaseous aliquot (80 pL) was taken from the HS and injected into the GC instrument. In the HS-SPME procedure, the fiber was removed from the HS and exposed in the heated injection port of the GC instrument. In all cases, PH3 was determined under the same chromatographic conditions with a GC pulsed flame photometric detector. In a comparison of the efficacy of the fibers, the bipolar fibers (CAR/PDMS and PDMS/DVB) contained more PH3 than the aliquot in the conventional HS analysis; larger size bipolar fibers extracted PH3 more efficiently than smaller fibers (e.g., 85 > 75 > 65 microm). The nonpolar fiber (PDMS) contained no PH3. Four fortification levels of PH3 on wheat were tested: 0.01, 0.05, 0.1, and 0.3 microg/g. The response of each bipolar fiber increased with the fortification levels, but the conventional HS analysis detected no fumigant at the lowest fortification level of 0.01 mg/g. Under the conditions of the validation study, the LOD was in the range of 0.005-0.01 ng PH3/g wheat. PMID:22649943

  6. Effect of Henry's law constant and operating parameters on vacuum-assisted headspace solid phase microextraction.

    PubMed

    Psillakis, Elefteria; Mousouraki, Antonia; Yiantzi, Evangelia; Kalogerakis, Nicolas

    2012-06-29

    Nonequilibrium headspace solid-phase microextraction (HSSPME) sampling under vacuum conditions may dramatically improve extraction kinetics compared to regular HSSPME at room temperature. This paper investigates the effects of organic analyte properties and sampling parameters (headspace volume and sample agitation) on vacuum-assisted HSSPME (Vac-HSSPME). It was found that at room temperature, acceleration effects on extraction rates induced by reducing the total pressure of the sample container are important for those compounds where the Henry's law constant, K(H), is close or below the reported threshold values for low K(H) solutes. For these compounds evaporation rate is controlled by mass transfer resistance in the thin gas-film adjacent to the gas/sample interface and reducing the total pressure will increase evaporation rates and result in a faster overall extraction process. Conversely, for analytes with an intermediate K(H) value, Vac-HSSPME is not expected to improve extraction rates compared to regular HSSPME given that mass transfer resistance in the liquid-film becomes important. In accordance with the theory, at equilibrium, the amount of analyte extracted by the SPME fiber is not affected by the pressure conditions inside the sample container. Furthermore, Vac-HSSPME extraction kinetics for low K(H) analytes were marginally affected by the tested change in headspace volume as evaporation rates dramatically increase under reduced pressure conditions and the sample responds much faster to the concentration drops in the headspace when compared to regular HSSPME. At equilibrium however, increasing the headspace volume may result in a loss of sensitivity for Vac-HSSPME similar to that observed for regular HSSPME. As expected, stirring the liquid sample was found to improve Vac-HSSPME. Finally, the method yielded a linearity of 0.998 and detection limits in the ppt level. The precision varied between 1.8% and 8.4%. PMID:22621889

  7. Solid-phase Microextraction (SPME) with Stable Isotope Calibration for Measuring Bioavailability of Hydrophobic Organic Contaminants

    PubMed Central

    Cui, Xinyi; Bao, Lianjun; Gan, Jay

    2014-01-01

    Solid-phase microextraction (SPME) is a biomimetic tool ideally suited for measuring bioavailability of hydrophobic organic compounds (HOCs) in sediment and soil matrices. However, conventional SPME sampling requires the attainment of equilibrium between the fiber and sample matrix, which may take weeks or months, greatly limiting its applicability. In this study, we explored the preloading of polydimethylsiloxane fiber with stable isotope labeled analogs (SI-SPME) to circumvent the need for long sampling time, and evaluated the performance of SI-SPME against the conventional equilibrium SPME (Eq-SPME) using a range of sediments and conditions. Desorption of stable isotope-labeled analogs and absorption of PCB-52, PCB-153, bifenthrin and cis-permethrin were isotropic, validating the assumption for SI-SPME. Highly reproducible preloading was achieved using acetone-water (1:4, v/v) as the carrier. Compared to Eq-SPME that required weeks or even months, the fiber concentrations (Cf) under equilibrium could be reliably estimated by SI-SPME in 1 d under agitated conditions or 20 d under static conditions in spiked sediments. The Cf values predicted by SI-SPME were statistically identical to those determined by Eq-SPME. The SI-SPME method was further applied successfully to field sediments contaminated with PCB 52, PCB 153, and bifenthrin. The increasing availability of stable isotope labeled standards and mass spectrometry nowadays makes SI-SPME highly feasible, allowing the use of SPME under non-equilibrium conditions with much shorter or flexible sampling time. PMID:23930601

  8. Strengths and weaknesses of in-tube solid-phase microextraction: A scoping review.

    PubMed

    Fernández-Amado, M; Prieto-Blanco, M C; López-Mahía, P; Muniategui-Lorenzo, S; Prada-Rodríguez, D

    2016-02-01

    In-tube solid-phase microextraction (in-tube SPME or IT-SPME) is a sample preparation technique which has demonstrated over time its ability to couple with liquid chromatography (LC), as well as its advantages as a miniaturized technique. However, the in-tube SPME perspectives in the forthcoming years depend on solutions that can be brought to the environmental, industrial, food and biomedical analysis. The purpose of this scoping review is to examine the strengths and weaknesses of this technique during the period 2009 to 2015 in order to identify research gaps that should be addressed in the future, as well as the tendencies that are meant to strengthen the technique. In terms of methodological aspects, this scoping review shows the in-tube SPME strengths in the coupling with LC (LC-mass spectrometry, capillary LC, ultra-high-pressure LC), in the new performances (magnetic IT-SPME and electrochemically controlled in-tube SPME) and in the wide range of development of coatings and capillaries. Concerning the applicability, most in-tube SPME studies (around 80%) carry out environmental and biomedical analyses, a lower number food analyses and few industrial analyses. Some promising studies in proteomics have been performed. The review makes a critical description of parameters used in the optimization of in-tube SPME methods, highlighting the importance of some of them (i.e. type of capillary coatings). Commercial capillaries in environmental analysis and laboratory-prepared capillaries in biomedical analysis have been employed with good results. The most consolidated configuration is in-valve mode, however the cycle mode configuration is frequently chosen for biomedical analysis. This scoping review revealed that some aspects such as the combination of in-tube SPME with other sample treatment techniques for the analysis of solid samples should be developed in depth in the near future. PMID:26772124

  9. Quantum dot-based headspace single-drop microextraction technique for optical sensing of volatile species.

    PubMed

    Costas-Mora, Isabel; Romero, Vanesa; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2011-03-15

    Core-shell CdSe/ZnS quantum dots (QDs) dispersed in a droplet of organic solvent have been applied for the first time as luminescent probes for the selective detection of volatile species. Luminescence quenching caused by volatile species was examined after their trapping onto a drop using the headspace single-drop microextraction (HS-SDME) approach along with microvolume fluorospectrometry. The novel method is characterized by low reagent and sample consumption, especially regarding QDs, a reduction about 500-fold for each analysis being attained in comparison with luminescent probing in aqueous phase using conventional luminescence spectrometers with 1 cm quartz cells for measurement. To assess QDs as luminescent probes along with HS-SDME, 14 volatile species were tried. Strong luminescence quenching (i.e., I(0)/I > 2.5) was observed for species such as CH(3)Hg(+) and Se(IV) after hydridation with NaBH(4). Moderate luminescent quenching (I(0)/I ≈ 2) was observed for species such as Hg(II) after its conversion into Hg(0), H(2)S, and methylcyclopentadienyl-manganese tricarbonyl (MMT). Small luminescence quenching effects (i.e., 1< I(0)/I <2) were caused by other hydride forming species such as As(III), Sb(III), Te(IV), and Bi(III), as well as SnBu(4), volatile amines, and endosulfan. Detection limits of 6.3 × 10(-9) and 1.6 × 10(-7) M were obtained for Se(IV) and CH(3)Hg(+), respectively. Repeatability expressed as relative standard deviation (N = 7) was about 5%. QD-HS-SDME-μvolume-fluorospectrometry allows one to carry out matrix separation, preconcentration, and confinement of QDs, hence achieving a selective, sensitive, fast, environmentally friendly, and miniaturized luminescence assay. PMID:21344872

  10. Electrically enhanced microextraction for highly selective transport of three β-blocker drugs.

    PubMed

    Seidi, Shahram; Yamini, Yadollah; Rezazadeh, Maryam

    2011-12-15

    Facilitated transport of three β-blocker drugs including atenolol (ATE), betaxolol (BET) and propranolol (PRO) was investigated under electrical field across a supported liquid membrane (SLM) using phosphoric acid derivatives as selective ion carriers, dissolved in 2-nitro phenyl octyl ether (NPOE). In the presence of di-(2-ethylhexyl) phosphate (DEHP) and tris-(2-ethylhexyl) phosphate (TEHP) in the membrane phase, the three β-blockers showed completely different transport behaviors which enabled highly selective separation of the drugs. Each β-blocker migrated from 3 mL of sample solutions, through a thin layer of specific organic solvent immobilized in the pores of a porous hollow fiber, and into a 15 μL acidic aqueous acceptor solution present inside the lumen of the fiber. The influences of fundamental parameters affecting the transport of target drugs including type of ion carrier for selective separation of each drug and its concentration in the membrane phase, extraction voltage, time of transport, pH of donor and acceptor phases, stirring speed of donor phase and salt effect were studied and optimized. After microextraction process, the extracts were analyzed by high-performance liquid chromatography with ultraviolet detection. Under optimal conditions, ATE was selectively extracted from different saliva samples with recovery of 37%, which corresponded to preconcentration factor of 74. A good linearity was achieved for calibration curve with a coefficient of determination higher than 0.997. Limits of detection and intra-day precision (n=3) were less than 2 μg L(-1) and 8.8%, respectively. PMID:21856103

  11. Determination of organophosphorus pesticides in soil by dispersive liquid-liquid microextraction and gas chromatography.

    PubMed

    Yang, Zhonghua; Liu, Yu; Liu, Donghui; Zhou, Zhiqiang

    2012-01-01

    In this article, a rapid and sensitive sample pretreatment technique for the determination of organophosphorus pesticides (OPPs) in soil samples is developed by using dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography-flame photometric detection. Experimental conditions, including the kind of extraction and disperser solvent and their volumes, the extraction time, and the salt addition, are investigated, and the following experiment factors are used: 20 µL chlorobenzene as the extraction solvent; 1.0 mL acetonitrile as the disperser solvent; no addition of salt; and an extraction time of 1 min. Under the optimum conditions, the linearities for the three target OPPs (ethoprophos, chlorpyriphos, and profenofos) are obtained by five points in the concentration range of 2.5-1500 µg/kg, and three replicates are used for each point. Correlation coefficients vary from 0.9987 to 0.9997. The repeatability is tested by spiking soil samples at a concentration level of 5.0 µg/kg. The relative standard deviation (n = 3) varied between 2.0% and 6.6%. The limits of detection, based on a signal-to-noise ratio (S/N) of 3, range from 200 to 500 pg/g. This method is applied to the analysis of the spiked samples S1, S2, and S3, which are collected from the China Agriculture University's orchard, lawn, and garden, respectively. The recoveries for each target analyte are in the range between 87.9% and 108.0%, 87.4% and 108.0%, and 86.7% and 107.2%, respectively. PMID:22291051

  12. Application of hollow fiber liquid phase microextraction for the determination of insecticides in water.

    PubMed

    Lambropoulou, Dimitra A; Albanis, Triantafyllos A

    2005-04-22

    In the present work, a novel sample pre-treatment technique for the determination of trace concentrations of some insecticide compounds in aqueous samples has been developed and applied to the determination of the selected analytes in environmental water samples. The extraction procedure is based on coupling polypropylene hollow fiber liquid phase microextraction (HF-LPME) with gas chromatography by flame thermionic detection (GC-FTD). For the development of the method, seven organophosphorous insecticides (dichlorvos, mevinphos-cis, ethoprophos, chlorpyrifos methyl, phenthoate, methidathion and carbofenothion) and one carbamate (carbofuran) were considered as target analytes. Several factors that influence the efficiency of HF-LPME were investigated and optimized including agitation, organic solvent, sample volume, exposure time, salt additives and pH. The optimized methodology exhibited good linearity with correlation coefficient = 0.990. The analytical precision for the target analytes ranged from 4.3 to 11.1 for within-day variation and 4.6 to 12.0% for between-day variation. The detection limits for all analytes were found in the range from 0.001 to 0.072 microg/L, well below the limits established by the EC Drinking Water Directive (EEC 80/778). Relative recoveries obtained by the proposed method from drinking and river water samples ranged from 80 to 104% with coefficient of variations ranging from 4.5 to 10.7%. The present methodology is easy, rapid, sensitive and requires small sample volumes to screen environmental water samples for insecticide residues. PMID:15881459

  13. Analysis of phenolic acids as chloroformate derivatives using solid phase microextraction-gas chromatography.

    PubMed

    Citová, Ivana; Sladkovský, Radek; Solich, Petr

    2006-07-28

    In the presented study, a simple and original procedure of phenolic acids derivatization treated by ethyl and methyl chloroformate performed in an aqueous media consisting of acetonitrile, water, methanol/ethanol and pyridine has been modified and optimized. Seven phenolic acid standards-caffeic, ferulic, gallic, p-coumaric, protocatechuic, syringic and vanillic were derivatized into corresponding methyl/ethyl esters and subsequently determined by the means of gas chromatography connected to the flame-ionisation detector (FID). Some selected validation parameters as linearity, detection and quantitation limits and peak area repeatability were valued. The total time of gas chromatography (GC) analysis was 24 min for methyl chloroformate and 30 min for ethyl chloroformate derivatization. The more suitable methyl chloroformate derivatization was used for further experiments on the possibility of multiple pre-concentration by the direct solid phase microextraction technique (SPME). For this purpose, polyacrylate (PA), polydimethylsiloxane (PDMS), carboxen/polydimethylsiloxane (CAR/PDMS) and polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibres were tested and the extraction conditions concerning time of extraction, temperature and time of desorption were optimized. The most polar PA fibre gave the best results under optimal extraction conditions (50 min extraction time, 25 degrees C extraction temperature and 10 min desorption time). As a result, the total time of SPME-GC analysis was 74 min and an increase in method sensitivity was reached. The limits of quantitation (LOQ) of p-coumaric, ferulic, syringic and vanillic acid esters after SPME pre-concentration were 0.02, 0.17, 0.2 and 0.2 microg mL(-1), respectively, showing approximately 10 times higher sensitivity in comparison with the original GC method. PMID:17723529

  14. Directly heated high surface area solid phase microextraction sampler for rapid field forensic analyses.

    PubMed

    Ramsey, Scott A; Mustacich, Robert V; Smith, Philip A; Hook, Gary L; Eckenrode, Brian A

    2009-11-01

    A high-surface area solid phase microextraction (HSA-SPME) sampler is described for dynamic sampling at high air velocities (up to several hundred centimeters per second). The sampling device consists of a thin wire coated with carboxen/polydimethylsiloxane (carboxen/PDMS) material, wound in the annular space between two concentric glass tubes, providing a large trapping surface from which analytes may then be thermally desorbed with little power consumption upon resistive heating of the wire. Desorbed analytes are focused and reconcentrated on a microtrap that is subsequently resistively heated to introduce analytes for GC or GC/MS analysis. Benzene, toluene, ethylbenzene, and xylenes (BTEX) included in a 39-component toxic organics (TO-14) gas mixture were used to evaluate the efficiency of the HSA-SPME sampler. Quantitation of trace-level BTEX compounds present during weapons cleaning was completed using stepwise calibration. Detection limits of 0.2-6.9 pptr(v) were observed for these analytes using single ion monitoring GC/MS analysis, and an improvement in sensitivity of several orders of magnitude was achieved when compared to standard dynamic flow SPME with a commercially available 10 mm carboxen/PDMS fiber. The potential for rapid analyte uptake and improved sensitivity using the HSA-SPME design will make it possible to rapidly collect and analyze VOC samples in field settings using a portable hand-held pump and a small, low power GC/MS instrument. This system will be especially useful for situations involving forensics, public safety, and military defensive or intelligence needs where rapid, sensitive detection of airborne analytes is required. PMID:19795869

  15. Determination of Organophosphorus Pesticides in Soil by Dispersive Liquid–Liquid Microextraction and Gas Chromatography

    PubMed Central

    Yang, Zhonghua; Liu, Yu; Liu, Donghui; Zhou, Zhiqiang

    2012-01-01

    In this article, a rapid and sensitive sample pretreatment technique for the determination of organophosphorus pesticides (OPPs) in soil samples is developed by using dispersive liquid–liquid microextraction (DLLME) combined with gas chromatography–flame photometric detection. Experimental conditions, including the kind of extraction and disperser solvent and their volumes, the extraction time, and the salt addition, are investigated, and the following experiment factors are used: 20 µL chlorobenzene as the extraction solvent; 1.0 mL acetonitrile as the disperser solvent; no addition of salt; and an extraction time of 1 min. Under the optimum conditions, the linearities for the three target OPPs (ethoprophos, chlorpyriphos, and profenofos) are obtained by five points in the concentration range of 2.5–1500 µg/kg, and three replicates are used for each point. Correlation coefficients vary from 0.9987 to 0.9997. The repeatability is tested by spiking soil samples at a concentration level of 5.0 µg/kg. The relative standard deviation (n = 3) varied between 2.0% and 6.6%. The limits of detection, based on a signal-to-noise ratio (S/N) of 3, range from 200 to 500 pg/g. This method is applied to the analysis of the spiked samples S1, S2, and S3, which are collected from the China Agriculture University's orchard, lawn, and garden, respectively. The recoveries for each target analyte are in the range between 87.9% and 108.0%, 87.4% and 108.0%, and 86.7% and 107.2%, respectively. PMID:22291051

  16. Ionic liquid based dispersive liquid-liquid microextraction for the extraction of pesticides from bananas.

    PubMed

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Asensio-Ramos, María; Rodríguez-Delgado, Miguel Angel

    2009-10-23

    This paper describes a dispersive liquid-liquid microextraction (DLLME) procedure using room temperature ionic liquids (RTILs) coupled to high-performance liquid chromatography with diode array detection capable of quantifying trace amounts of eight pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox and fenazaquin) in bananas. Fruit samples were first homogenized and extracted (1g) with acetonitrile and after suitable evaporation and reconstitution of the extract in 10 mL of water, a DLLME procedure using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) as extraction solvent was used. Experimental conditions affecting the DLLME procedure (sample pH, sodium chloride percentage, ionic liquid amount and volume of disperser solvent) were optimized by means of an experimental design. In order to determine the presence of a matrix effect, calibration curves for standards and fortified banana extracts (matrix matched calibration) were studied. Mean recovery values of the extraction of the pesticides from banana samples were in the range of 69-97% (except for thiophanate-methyl and carbofuran, which were 53-63%) with a relative standard deviation lower than 8.7% in all cases. Limits of detection achieved (0.320-4.66 microg/kg) were below the harmonized maximum residue limits established by the European Union (EU). The proposed method, was also applied to the analysis of this group of pesticides in nine banana samples taken from the local markets of the Canary Islands (Spain). To the best of our knowledge, this is the first application of RTILs as extraction solvents for DLLME of pesticides from samples different than water. PMID:19700165

  17. Pesticide extraction from table grapes and plums using ionic liquid based dispersive liquid-liquid microextraction.

    PubMed

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Angel

    2009-12-01

    Room temperature ionic liquids (RTILs) have been used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of eight multi-class pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox, and fenazaquin) in table grapes and plums. The developed method involves the combination of DLLME and high-performance liquid chromatography with diode array detection. Samples were first homogenized and extracted with acetonitrile. After evaporation and reconstitution of the extract in water containing sodium chloride, a quick DLLME procedure that used the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) and methanol was developed. The RTIL dissolved in a very small volume of acetonitrile was directed injected in the chromatographic system. The comparison between the calibration curves obtained from standards and from spiked sample extracts (matrix-matched calibration) showed the existence of a strong matrix effect for most of the analyzed pesticides. A recovery study was also developed with five consecutive extractions of the two types of fruits spiked at three concentration levels. Mean recovery values were in the range of 72-100% for table grapes and 66-105% for plum samples (except for thiophanate-methyl and carbofuran, which were 64-75% and 58-66%, respectively). Limits of detection (LODs) were in the range 0.651-5.44 microg/kg for table grapes and 0.902-6.33 microg/kg for plums, representing LODs below the maximum residue limits (MRLs) established by the European Union in these fruits. The potential of the method was demonstrated by analyzing 12 commercial fruit samples (six of each type). PMID:19779926

  18. Multiple headspace solid-phase microextraction for quantifying volatile free fatty acids in cheeses.

    PubMed

    Rincón, Arturo A; Pino, Verónica; Ayala, Juan H; Afonso, Ana M

    2014-11-01

    Multiple headspace solid-phase microextraction (MHS-SPME) has been utilized for the quantitative determination of 9 volatile free fatty acids (FFAs) in cheeses, in combination with gas-chromatography and flame-ionization detection (GC-FID). Variables affecting HS-SPME and MHS-SPME were optimized to attain adequate sensitivity while allowing correct application of the MHS method. Thus, the MHS-SPME method was successfully performed when using 0.3g of cheese and 1 mL of NaCl (sat. solution), which is subjected to four consecutive extractions using the carboxen-polydimethylsyloxane (CAR-PDMS) as the commercial SPME coating, 40 min of HS extraction time at 45°C, and 6 min of desorption time in the GC injector at 290°C. The MHS-SPME permitted the calculation of β values, which range from 0.72±0.01-0.95±0.02, depending on the cheese studied. Later, this β parameter is used to perform quantitation for the 9 volatile FFAs after just a single HS-SPME extraction, using an external solvent calibration curve. The validity of the utilization of an external solvent calibration was tested with aqueous standards of volatile FFAs, getting average recoveries higher than 81.2%. Quantitation by MHS-SPME was free of matrix interferences despite measuring a complex cheese sample. The optimized method was validated, presenting inter-day reproducibility values (as RSD in %) lower than 13%, and limits of detection down to 7 µg kg(-1). The method was also compared with a conventional extraction method such as solid-phase extraction for the studied cheeses elaborated with goat milk, generating comparable results. To our knowledge, this is the first time that MHS-SPME has been applied to volatiles in cheeses. PMID:25127582

  19. Polypyrrole/hexagonally ordered silica nanocomposite as a novel fiber coating for solid-phase microextraction.

    PubMed

    Gholivand, Mohammad Bagher; Abolghasemi, Mir Mahdi; Fattahpour, Peyman

    2011-10-17

    A highly porous fiber coated polypyrrole/hexagonally ordered silica (PPy/SBA15) materials were prepared for solid-phase microextraction (SPME). The PPy/SBA15 nanocomposite was synthesized by an in situ polymerization technique. The resulting material was characterized by the scanning electron microscopy, thermogravimetric analysis and differential thermal analysis. The prepared nanomaterial was immobilized onto a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). A one at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, desorption time and desorption temperature. In optimum conditions (extraction temperature 70°C, extraction time 20 min, ionic strength 20% (WV(-1)), stirring rate 500 rpm, desorption temperature 270°C, desorption time 5 min) the repeatability for one fiber (n=3), expressed as relative standard deviation (R.S.D. %), was between 5.0% and 9.3% for the tested compounds. The quantitation limit for the studied compounds were between 13.3 and 66.6 pg mL(-1). The life span and stability of the PPy/SBA15 fiber are good, and it can be used more than 50 times at 260°C without any significant change in sorption properties. The developed method offers the advantage of being simple to use, with shorter analysis times, lower cost of equipment, thermal stability of fiber and high relative recovery in comparison to conventional methods of analysis. PMID:21907035

  20. Preparation and evaluation of graphene-coated solid-phase microextraction fiber.

    PubMed

    Chen, Jinmei; Zou, Jing; Zeng, Jingbin; Song, Xinhong; Ji, Jiaojiao; Wang, Yiru; Ha, Jaeho; Chen, Xi

    2010-09-23

    In this paper, a novel graphene (G) based solid-phase microextraction (SPME) fiber was firstly prepared by immobilizing the synthesized G on stainless steel wire as coating. The new fiber possessed a homogeneous, porous and wrinkled surface and showed excellent thermal (over 330°C), chemical and mechanical stability, and long lifespan (over 250 extractions). The SPME performance of the G-coated fiber was evaluated in detail through extraction of six pyrethroid pesticides. Although the thickness of G-coated fiber was only 6-8 μm, its extraction efficiencies were higher than those of two commercial fibers (PDMS, 100 μm; PDMS/DVB, 65 μm). This high extraction efficiency may be mainly attributed to huge delocalized π-electron system of G, which shows strong π-stacking interaction with pyrethroid pesticide. The G-coated fiber was applied in the gas chromatographic determination of six pyrethroids, and their limits of detection were found to be ranged from 3.69 to 69.4 ng L(-1). The reproducibility for each single fiber was evaluated and the relative standard deviations (RSDs) were calculated to be in the range from 1.9% to 6.5%. The repeatability of fiber-to-fiber and batch-to-batch was 4.3-9.2% and 4.1-9.9%. The method developed was successfully applied to three pond water samples, and the recoveries were 83-110% at a spiking of 1 μg L(-1). PMID:20869503

  1. Quick supramolecular solvent-based microextraction for quantification of low curcuminoid content in food.

    PubMed

    Caballero-Casero, Noelia; Ocak, Miraç; Ocak, Ümmüham; Rubio, Soledad

    2014-03-01

    There is a need to monitor the consumption of curcuminoids, an EU-permitted natural colour in food, to ensure that acceptable daily intakes are not exceeded, especially by young children. This paper describes a sensitive method able to quantify low contents of curcumin (CUR), demethoxycurcumin (DMC) and bis-demethoxycurcumin (BDMC) in foodstuffs. The method was based on a single-step extraction by use of a supramolecular solvent (SUPRAS) made up of reverse aggregates of decanoic acid, and direct analysis of the extract by use of liquid chromatography-photodiode array (PDA) detection. The extraction involved the stirring of 200 mg foodstuff with 600 μL SUPRAS for 15 min. No cleanup or concentration of the extracts was required. Curcuminoid solubilisation occurred via dispersion and hydrogen bonding. The method was used for the determination of curcuminoids in different types of foodstuff (snack, gelatine, yoghurt, mayonnaise, butter, candy and fish products) that encompassed a wide range of protein, fat, carbohydrate, sugar and water contents (0.85-11.04, 0-81.11, 0.06-75, 0.06-79.48, and 10.08-85.10 g, respectively, in each 100 g of food). Method quantification limits for the foodstuffs analysed were in the ranges 2.9-7.7, 2.8-11.2 and 3.3-9.0 μg kg(-1) for CUR, DMC and BDMC, respectively. The concentrations of curcuminoids detected in the foodstuffs and the recoveries obtained from fortified samples were in the ranges ND-284, ND-201 and ND-61.3 μg kg(-1), and 82-106, 89-106 and 90-102 %, for CUR, DMC and BDMC, respectively. The relative standard deviations were in the range 2-7 %. This method enabled quick and simple microextraction of curcuminoids with minimal solvent consumption, while delivering accurate and precise data. PMID:24170269

  2. [Rapid fabrication of molecularly imprinted polymer fibers for solid phase microextraction of bisphenol A].

    PubMed

    Hu, Mei; Zhang, Yijun; Yang, Jinghua; Zhou, Xiaomao; Wei, Zhuqing; Ding, Xiaoqing; Zhang, Yuping

    2015-02-01

    The rapid preparation of molecularly imprinted polymer (MIP) fibers was reported using bisphenol A (BPA) as the template molecular, acetonitrile (ACN) as the porogenic solvent, α-methacrylic acid (MAA) as the functional monomer, ethylene dimethacrylate (EDMA) as the crosslinker, and azodiisobutyronitrile (AIBN) as the thermal initiator. It was carried out within a capillary of 530 µm inner diameter (I. D.) by microwave irradiation in 7 min. The resulted BPA-MIP fibers were pushed out from the capillary, eluted in a vial and inserted in the capillary again followed by the application of the solid phase microextraction (SPME) procedure. The extraction performance was investigated in detail by varying the molar ratios between the template and the monomer (BPA/MAA), the concentration of NaCl, the extraction and desorption time, the pH value and the desorption solvents. The selectivity of the prepared MIP and non-molecularly imprinted polymer (NIP) fibers was comparatively evaluated by selecting two structurally-related compounds, phenol (P) and 4-phenylphenol (PP), and non-analogue dicyandiamide (DCD). The established method was successfully applied for the pretreatment and determination of BPA from beverage samples coupled to high performance liquid chromatography (HPLC). Under the optimal conditions, the linear range of BPA was 10-400 µg/L; the detection limit (LOD) was 0.45 µg/L and the recoveries spiked in the mineral water were 88.4%-102. 8%. The results demonstrated that the developed method can determine BPA in real samples with some advantages of simple pretreatment, rapid analysis, low limit of detection and low consumption of materials. PMID:25989683

  3. Whirling agitated single drop microextraction technique for the simultaneous analysis of Paraquat and Maneb in tissue samples of treated mice.

    PubMed

    Kumari, Rupender; Jha, Rakesh R; Singh, Mahendra P; Patel, Devendra K

    2016-05-01

    A new microextraction technique, whirling agitated single drop microextraction, has been proposed for the simultaneous analysis of Paraquat and Maneb in tissue samples before liquid chromatography with tandem mass spectrometry. This technique is based on the idea that the escalatory motion of the sample solution along with the extraction solvent increases the movement of molecules into the extraction solvent. In this technique, a simple handheld rotator was utilized to rapidly agitate the biphasic extraction system for the instantaneous extraction of targeted analytes. After extraction, the extracted phase was directly solidified by cooling in crushed ice and easily collected using a micro-spatula. The method showed good performance by achieving sensitive detection limits at 4.81 ng g(-1) (Paraquat) and 9.12 ng g(-1) (Maneb). Mean recoveries and enrichment factors were obtained >91.21% and up to 114 that ensured the preconcentration capacity of the method. The method precision was verified by evaluating intraday variation (n = 10) ≤4.57 (Paraquat) and ≤4.68 (Maneb) in terms of percent relative standard deviation. Additionally, method efficacy was assured by obtaining very little matrix interferences (≤3.11%). Moreover, the method suitability was also checked with its application on tissue samples of intraperitoneally treated mice with Paraquat and Maneb. PMID:26970105

  4. An Improved Pneumatic Nebulization Gas-Solid Microextraction Device Used to Detect Triazine Herbicides in White Spirit.

    PubMed

    Xu, Hui; Fei, Qiang; Shan, Hongyan; Huan, Yanfu; Mi, Hongyu; Zhang, Hanqi; Li, Guanghua; Feng, Guodong

    2016-01-01

    The pneumatic nebulization gas-solid microextraction device fascinating us is because it directly atomized organic samples to cross a solid-phase microextraction (SPME) cartridge without any pretreatment. In this work, both the spray chamber and SPME column of the extraction device were heated. We found that this would significantly improve the extraction efficiency of this method. Then, this method was used to detect seven triazine herbicides (atraton, desmetryn, atrazine, terbumeton, terbuthylazine, terbutryn, and dipropetryn) in drinking alcohol samples. The experimental results indicated that this extraction procedure could conveniently, efficiently and accurately concentrate any triazine herbicides from drinking alcohol samples. The limits of detection (LODs) were from 0.08 to 0.23 μg L(-1), the limits of quantification (LOQs) were from 0.27 to 0.78 μg L(-1). We used this method to detect triazine herbicides in five white spirit samples. Four concentrations were chosen (5, 25, 50 and 100 μg L(-1)) as the amounts of spikes to investigate the recovery and precision of the present PN-GSME method. The recoveries ranged from 95.91 to 106.67%. The relative standard deviations were not more than 6.51%. Also this method matches the requirement of the maximum residue limits of the European Union. PMID:26860563

  5. A novel procedure for phase separation in dispersive liquid-liquid microextraction based on solidification of the aqueous phase.

    PubMed

    March, J G; Cerdà, V

    2016-08-15

    In this paper, an alternative for handling the organic phase after a dispersive liquid-liquid microextraction using organic solvents lighter than water is presented. It is based on solidification (at -18°C) of the aqueous phase obtained after centrifugation, and the decantation, collection and analysis of the liquid organic layer. The extraction of nicotine in toluene, and its determination in eggplant samples was conducted as a proof of concept. The study has been carried out using standards prepared in water and the formation of the dispersion was assisted by sonication. The organic extract was analysed using gas chromatography coupled to mass spectrometry. Satisfactory analytical figures of merit as: limit of detection (0.4µgL(-1), 2ngg(-1) wet sample), limit of quantification (1.2µgL(-1), 6.5ngg(-1) wet sample), within-day precision (RSD=7%), and linearity interval (up to 384µgL(-1) nicotine) were achieved. It constituted a contribution to the handling of organic extracts after microextraction processes. PMID:27260454

  6. A preconcentration method for analysis of neonicotinoids in honey samples by ionic liquid-based cold-induced aggregation microextraction.

    PubMed

    Vichapong, Jitlada; Burakham, Rodjana; Santaladchaiyakit, Yanawath; Srijaranai, Supalax

    2016-08-01

    A preconcentration approach based on ionic liquid-based cold-induced aggregation microextraction for determination of neonicotinoid insecticide residues in honey samples before high-performance liquid chromatographic analysis has been developed. Room temperature ionic liquid [C4MIM][PF6] (extraction solvent) and SDS (emulsifier) was used for extraction of the target analytes. The parameters affecting the extraction efficiency were optimized. The optimum microextraction conditions were 200µL room temperature ionic liquids [C4MIM][PF6] containing 0.05molL(-1) SDS, 0.75g sodium carbonate, vortex agitation speed of 1800rpm for 30s and centrifugation at 3500rpm for 10min. Under optimum conditions, the high enrichment factors of 200 could be obtained, leading to low limit of detection (0.01µgL(-1) for all analytes) with the relative standard deviations lower than 2.68% and 5.38% for retention time and peak area, respectively. Good recoveries for the spiked target neonicotinoids at three different concentrations of honey samples were obtained in 86-100% and relative standard deviations were lower than 8.1%. The results demonstrated that the proposed method can be used as an alternative powerful method for the simultaneous determination of the studied insecticides in real honey samples. PMID:27216676

  7. Solvent-modified solid-phase microextraction for the determination of diazepam in human plasma samples by capillary gas chromatography.

    PubMed

    Krogh, M; Grefslie, H; Rasmussen, K E

    1997-02-21

    This paper describes microextraction and gas chromatographic analysis of diazepam from human plasma. The method was based on immobilisation of 1.5 microliters of 1-octanol on a polyacrylate-coated fiber designed for solid-phase microextraction. The solvent-modified fibre was used to extract diazepam from the samples. The plasma sample was pre-treated to release diazepam from the protein binding. The fibre was inserted into the modified plasma sample, adjusted to pH 5.5 an internal standard was added and the mixture was carefully stirred for 4 min. The fibre with the immobilised solvent and the enriched analytes was injected into the capillary gas chromatograph. The solvent and the extracted analytes were evaporated at 300 degrees C in the split-splitless injection port of the gas chromatograph, separated on a methylsilicon capillary column and detected with a nitrogen-phosphorus detector. The method was shown to be reproducible with a detection limit of 0.10 nmol/ml in human plasma. PMID:9080322

  8. Design of the extraction process for terpenes and other volatiles from allspice by solid-phase microextraction and hydrodistillation.

    PubMed

    Bajer, Tomáš; Ligor, Magdalena; Ligor, Tomasz; Buszewski, Bogusław

    2016-02-01

    Methods for the separation and determination of terpenes (mono- and sesqui-) and phenylpropanoids such as eugenol and methyleugenol from samples of allspice berries have been developed. Chromatographic analyses of isolated groups of compounds were carried out by means of gas chromatography coupled with mass spectrometry. A comparison of various types of solid-phase microextraction fibers was performed. The highest yields of terpenes were extracted by polydimethylsiloxane and divinylbenzene/Carboxen/polydimethylsiloxane fibers (almost the same for these two fibers), approximately twice as much as by Carbowax/divinylbenzene fiber. The highest amounts of monoterpenes were extracted by divinylbenzene/Carboxen/polydimethylsiloxane fiber, and the highest amounts of sesquiterpenes were extracted by polydimethylsiloxane fiber. Moreover, the effect of water addition on extraction yields as well as time and temperature of extraction were tested. Aroma profiles of extracts obtained by solid-phase microextraction and essential oil obtained by hydrodistillation of allspice berries were compared. The aroma profile of the divinylbenzene/Carboxen/polydimethylsiloxane fiber extract was similar to the aroma profile of essential oil. Particular characteristics of volatile allspice matters were presented. The linear retention indices for each compound were calculated. PMID:26632088

  9. Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

    PubMed

    Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

    2016-05-01

    Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples. PMID:27040110

  10. Fully-automated in-syringe dispersive liquid-liquid microextraction for the determination of caffeine in coffee beverages.

    PubMed

    Frizzarin, Rejane M; Maya, Fernando; Estela, José M; Cerdà, Víctor

    2016-12-01

    A novel fully-automated magnetic stirring-assisted lab-in-syringe analytical procedure has been developed for the fast and efficient dispersive liquid-liquid microextraction (DLLME) of caffeine in coffee beverages. The procedure is based on the microextraction of caffeine with a minute amount of dichloromethane, isolating caffeine from the sample matrix with no further sample pretreatment. Selection of the relevant extraction parameters such as the dispersive solvent, proportion of aqueous/organic phase, pH and flow rates have been carefully evaluated. Caffeine quantification was linear from 2 to 75mgL(-1), with detection and quantification limits of 0.46mgL(-1) and 1.54mgL(-1), respectively. A coefficient of variation (n=8; 5mgL(-1)) of a 2.1% and a sampling rate of 16h(-1), were obtained. The procedure was satisfactorily applied to the determination of caffeine in brewed, instant and decaf coffee samples, being the results for the sample analysis validated using high-performance liquid chromatography. PMID:27374593

  11. Towards a green analytical laboratory: microextraction techniques as a useful tool for the monitoring of polluted soils

    NASA Astrophysics Data System (ADS)

    Lopez-Garcia, Ignacio; Viñas, Pilar; Campillo, Natalia; Hernandez Cordoba, Manuel; Perez Sirvent, Carmen

    2016-04-01

    Microextraction techniques are a valuable tool at the analytical laboratory since they allow sensitive measurements of pollutants to be carried out by means of easily available instrumentation. There is a large number of such procedures involving miniaturized liquid-liquid or liquid-solid extractions with the common denominator of using very low amounts (only a few microliters) or even none of organic solvents. Since minimal amounts of reagents are involved, and the generation of residues is consequently minimized, the approach falls within the concept of Green Analytical Chemistry. This general methodology is useful both for inorganic and organic pollutants. Thus, low amounts of metallic ions can be measured without the need of using ICP-MS since this instrument can be replaced by a simple AAS spectrometer which is commonly present in any laboratory and involves low acquisition and maintenance costs. When dealing with organic pollutants, the microextracts obtained can be introduced into liquid or gas chromatographs equipped with common detectors and there is no need for the most sophisticated and expensive mass spectrometers. This communication reports an overview of the advantages of such a methodology, and gives examples for the determination of some particular contaminants in soil and water samples The authors are grateful to the Comunidad Autonóma de la Región de Murcia , Spain (Fundación Séneca, 19888/GERM/15) for financial support

  12. Screening of tropical fruit volatile compounds using solid-phase microextraction (SPME) fibers and internally cooled SPME fiber.

    PubMed

    Carasek, Eduardo; Pawliszyn, Janusz

    2006-11-15

    In this study, the optimization and comparison of an internally cooled fiber [cold fiber with polydimethylsiloxane (PDMS) loading] and several commercial solid-phase microextraction (SPME) fibers for the extraction of volatile compounds from tropical fruits were performed. Automated headspace solid-phase microextraction (HS-SPME) using commercial fibers and an internally cooled SPME fiber device coupled to gas chromatography-mass spectrometry (GC-MS) was used to identify the volatile compounds of five tropical fruits. Pulps of yellow passion fruit (Passiflora edulis), cashew (Anacardium occidentale), tamarind (Tamarindus indica L.), acerola (Malphigia glabra L.), and guava (Psidium guajava L.) were sampled. The extraction conditions were optimized using two experimental designs (full factorial design and Doehlert matrix) to analyze the main and secondary effects. The volatile compounds tentatively identified included alcohols, esters, carbonyl compounds, and terpernes. It was found that the cold fiber was the most appropriate fiber for the purpose of extracting volatile compounds from the five fruit pulps studied. PMID:17090108

  13. An automatic countercurrent liquid-liquid micro-extraction system coupled with atomic absorption spectrometry for metal determination.

    PubMed

    Mitani, Constantina; Anthemidis, Aristidis N

    2015-02-01

    A novel and versatile automatic sequential injection countercurrent liquid-liquid microextraction (SI-CC-LLME) system coupled with atomic absorption spectrometry (FAAS) is presented for metal determination. The extraction procedure was based on the countercurrent flow of aqueous and organic phases which takes place into a newly designed lab made microextraction chamber. A noteworthy feature of the extraction chamber is that it can be utilized for organic solvents heavier or lighter than water. The proposed method was successfully demonstrated for on-line lead determination and applied in environmental water samples using an amount of 120 μL of chloroform as extractant and ammonium diethyldithiophosphate as chelating reagent. The effect of the major experimental parameters including the volume of extractant, as well as the flow rate of aqueous and organic phases were studied and optimized. Under the optimum conditions for 6 mL sample consumption an enhancement factor of 130 was obtained. The detection limit was 1.5 μg L(-1) and the precision of the method, expressed as relative standard deviation (RSD) was 2.7% at 40.0 μg L(-1) Pb(II) concentration level. The proposed method was evaluated by analyzing certified reference materials and spiked environmental water samples. PMID:25435230

  14. Determining octanol-water partition coefficients for extremely hydrophobic chemicals by combining "slow stirring" and solid-phase microextraction.

    PubMed

    Jonker, Michiel T O

    2016-06-01

    Octanol-water partition coefficients (KOW ) are widely used in fate and effects modeling of chemicals. Still, high-quality experimental KOW data are scarce, in particular for very hydrophobic chemicals. This hampers reliable assessments of several fate and effect parameters and the development and validation of new models. One reason for the limited availability of experimental values may relate to the challenging nature of KOW measurements. In the present study, KOW values for 13 polycyclic aromatic hydrocarbons were determined with the gold standard "slow-stirring" method (log KOW 4.6-7.2). These values were then used as reference data for the development of an alternative method for measuring KOW . This approach combined slow stirring and equilibrium sampling of the extremely low aqueous concentrations with polydimethylsiloxane-coated solid-phase microextraction fibers, applying experimentally determined fiber-water partition coefficients. It resulted in KOW values matching the slow-stirring data very well. Therefore, the method was subsequently applied to a series of 17 moderately to extremely hydrophobic petrochemical compounds. The obtained KOW values spanned almost 6 orders of magnitude, with the highest value measuring 10(10.6) . The present study demonstrates that the hydrophobicity domain within which experimental KOW measurements are possible can be extended with the help of solid-phase microextraction and that experimentally determined KOW values can exceed the proposed upper limit of 10(9) . Environ Toxicol Chem 2016;35:1371-1377. © 2015 SETAC. PMID:26550770

  15. Ordered mesoporous polymers in situ coated on a stainless steel wire for a highly sensitive solid phase microextraction fibre

    NASA Astrophysics Data System (ADS)

    Zheng, Juan; Liang, Yeru; Liu, Shuqin; Ding, Yajuan; Shen, Yong; Luan, Tiangang; Zhu, Fang; Jiang, Ruifen; Wu, Dingcai; Ouyang, Gangfeng

    2015-07-01

    Development of facile and effective methods for fabrication of high-performance solid phase microextraction (SPME) fibres remains a great challenge. Herein, a new class of ordered mesoporous polymers (OMPs) in situ coated on a stainless steel wire were successfully developed and utilized as a highly sensitive and stable SPME fibre for the first time. Because of the highly ordered mesoporous structure of its OMP coating, the π-π interactions and the dispersion forces, the OMP-coated SPME fibre exhibited much better extraction properties as compared to the commercial PDMS fibre. The findings could provide a new benchmark for preparing well-defined porous materials for the SPME application.Development of facile and effective methods for fabrication of high-performance solid phase microextraction (SPME) fibres remains a great challenge. Herein, a new class of ordered mesoporous polymers (OMPs) in situ coated on a stainless steel wire were successfully developed and utilized as a highly sensitive and stable SPME fibre for the first time. Because of the highly ordered mesoporous structure of its OMP coating, the π-π interactions and the dispersion forces, the OMP-coated SPME fibre exhibited much better extraction properties as compared to the commercial PDMS fibre. The findings could provide a new benchmark for preparing well-defined porous materials for the SPME application. Electronic supplementary information (ESI) available: Experimental details, Fig. S1-S3 and Tables S1-S3. See DOI: 10.1039/c5nr02674a

  16. Liquid-liquid-solid microextraction and detection of nerve agent simulants by on-membrane Fourier transform infrared spectroscopy.

    PubMed

    Garg, Prabhat; Purohit, Ajay; Tak, Vijay K; Kumar, Ajeet; Dubey, D K

    2012-11-01

    A coupling of novel liquid-liquid-solid microextraction (LLSME) technique based on porous hydrophobic membrane and Fourier-transform infrared spectroscopy has been presented for the detection, identification and quantification of markers and simulants of nerve agents. Two isomers O,O'-dihexyl methylphosphonate (DHMP) and O,O'-dipentyl isopropylphosphonate (DPIPP) were chosen as model analytes for the study. In the present technique, organic phase was immobilised within the pores of membrane after fixing it in an assembly, which was then immersed into aqueous sample of target analytes for extraction. The analytes were directly determined on the surface of membrane by FTIR spectroscopy without elution. On comparison with solid phase microextraction (SPME), LLSME was found to be much more efficient. The method was optimised and quantitative analyses were performed using calibration curves obtained via Beer's law and employing processing of spectra obtained, via a multivariate calibration technique partial least square (PLS). Relative standard deviations (RSDs) for intraday repeatability and interday reproducibility were found to be in the range of 0.20-0.50% and 0.20-0.60%, respectively. Limit of detection (LOD) was achieved up to 15 ng mL(-1). Applicability of the method was tested with an unknown real sample obtained in an international official proficiency test (OPT). PMID:23084054

  17. Supramolecular-based dispersive liquid-liquid microextraction: a novel sample preparation technique utilizes coacervates and reverse micelles.

    PubMed

    Jafarvand, Sanaz; Shemirani, Farzaneh

    2011-02-01

    The present study reports a novel sample enrichment method termed supramolecular-based dispersive liquid-liquid microextraction (SM-DLLME). The SM solvent selected was made up of reversed micelles of decanoic acid dispersed in tetrahydrofuran (THF)-water. THF plays double role, not only acts as a disperser solvent but also causes self-assembly of decanoic acid. The contaminant used as a model was Malachite Green (MG). It was a cationic dye and was preconcentrated without any derivatization or ion-pair formation reaction. In SM-DLLME, the most important advantages of DLLME technique and preconcentration strategy based on the coacervation and reverse micelles have come together. Moreover, in this method, disadvantages of DLLME such as extraction capability of only hydrophobic analytes and hiring toxic and hazardous organic solvents as the extraction solvent and disadvantages of coacervation-based extraction method such as tedious, labor-intensive and time-consuming stirring procedure have been avoided. Several variables affecting the microextraction efficiency were investigated and optimized. Under the optimized conditions and preconcentration of only 5.00 mL of sample, the enhancement factor was 52, limit of detection (LOD) was 4 μg/L and relative standard deviations (RSDs) for 145 and 36 μg/L of MG in textile industry wastewater were 1.8 and 3.2%, respectively (n = 6). PMID:21254398

  18. Switchable polarity solvent for liquid phase microextraction of Cd(II) as pyrrolidinedithiocarbamate chelates from environmental samples.

    PubMed

    Yilmaz, Erkan; Soylak, Mustafa

    2015-07-30

    A switchable polarity solvent was synthesized from triethylamine (TEA)/water/CO2 (Dry ice) via proton transfer reaction has been used for the microextraction of cadmium(II) as pyrrolidinedithiocarbamate (APDC) chelate. Cd(II)-APDC chelate was extracted into the switchable polarity solvent drops by adding 2 mL 10 M sodium hydroxide solution. Analytical parameters affecting the complex formation and microextraction efficiency such as pH, amount of ligand, volume of switchable polarity solvent and NaOH, sample volume were optimized. The effects of foreign ions were found tolerably. Under optimum conditions, the detection limit was 0.16 μg L(-1) (3Sb/m, n = 7) and the relative standard deviation was 5.4% (n = 7). The method was validated by the analysis of certified reference materials (TMDA-51.3 fortified water, TMDA-53.3 fortified water and SPS-WW2 waste water, 1573a Tomato Leaves and Oriental Basma Tobacco Leaves (INCT-OBTL-5)) and addition/recovery tests. The method was successfully applied to determination of cadmium contents of water, vegetable, fruit and cigarette samples. PMID:26320638

  19. Determination of abamectin in citrus fruits using SPE combined with dispersive liquid-liquid microextraction and HPLC-UV detection.

    PubMed

    Rezaee, Mohammad; Mashayekhi, Hossein Ali; Saleh, Abolfazl; Abdollahzadeh, Yaser; Naeeni, Mohammad Hosein; Fattahi, Nazir

    2013-08-01

    A new pretreatment method, SPE combined with dispersive liquid-liquid microextraction, was proposed for the determination of abamectin in citrus fruit samples for the first time. In this method, fruit samples were extracted by ultrasound-assisted extraction followed by SPE. Then, the SPE was used as a disperser solvent in the next dispersive liquid-liquid microextraction step for further purification and enrichment of abamectin. The effects of various parameters on the extraction efficiency of the proposed method were investigated and optimized. Good linearity of abamectin was obtained from 0.005 to 10.0 mg/kg for B1a and from 0.05 to 10.0 mg/kg for B1b with correlation coefficient (r(2)) of 0.998 for B1a and 0.991 for B1b, respectively. The LODs were 0.001 and 0.008 mg/kg (S/N = 3) for B1a and B1b, respectively. The relative recoveries at three spiked levels were ranged from 87 to 96% with the RSD less than 11% (n = 3). The method has been successfully applied to the determination of abamectin in citrus fruit samples. PMID:23913592

  20. Ultrasound-assisted dispersive liquid-liquid microextraction for the speciation of traces of chromium using electrothermal atomic absorption spectrometry.

    PubMed

    López-García, Ignacio; Briceño, Marisol; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel

    2013-10-15

    A microextraction procedure for the speciation of very low concentrations (0.005-0.2 µg L(-1)) of chromium is discussed. To the aqueous sample (10 mL), diluted hydrochloric acid, sodium chloride and a small amount of tributylphosphate (80 µL) are incorporated, and the mixture is submitted to ultrasounds for 10 min. The organic phase recovered after centrifuging is injected into the electrothermal atomizer, and the signal due to hexavalent chromium obtained. The repetition of the procedure using another aliquot in which all the chromium present is oxidized to Cr (VI) allows the Cr(III) content to be obtained by difference. The enrichment factor is 240 and the detection limit 0.002 µg L(-1) chromium. The relative standard deviation for ten consecutive microextractions of a 0.1 µg L(-1) chromium solution is close to 8%. The procedure is applied to waters and to the leachates obtained from low cost toys made of plastic materials. PMID:24054574

  1. High-Throughput Determination of Octanol-Water Partition Coefficients by Ultrasound-Assisted Liquid-Phase Microextraction.

    PubMed

    Guo, Yugao; Ma, Shuo; Guan, Shan; Zhang, Yan; Pan, Jie

    2015-09-01

    A method of high-throughput determination, which is based on ultrasound-assisted liquid-phase microextraction, was developed to measure directly the partition coefficients of n-octanol-water. In ultrasound-assisted liquid-phase microextraction, ultrasonic energy can facilitate the mass transfer process of six or more microextractors simultaneously. Therefore, high-throughput determination of n-octanol-water partition coefficients can be performed favorably, and the equilibrium time of each microextractor can be decreased effectively. Several experimental parameters including ultrasonic power and frequency, centrifugation conditions, extractant volume and sample concentration were analyzed and optimized at 25°C. Under the optimum conditions, it only takes 2 min to reach extraction equilibrium, and the solutions of sample can be separated by centrifugation in 4 min. After centrifugation, the concentrations in n-octanol phases are analyzed with gas chromatography. The method was further evaluated with eight reference compounds and the findings demonstrated that this method is suitable to determine the partition coefficients of organic compounds accurately and quickly. Next, the method was exploited to measure the partition coefficients of n-octanol-water containing 20 organic compounds, which cover the [Formula: see text] values from 0.05 to 4.36, with comparatively low relative standard deviation (RSD) directly. The results of this study illustrated that the RSD (n = 6) was under 3%. PMID:25583971

  2. Potential of needle trap microextraction-portable gas chromatography-mass spectrometry for measurement of atmospheric volatile compounds

    NASA Astrophysics Data System (ADS)

    Feijó Barreira, Luís Miguel; Xue, Yu; Duporté, Geoffroy; Parshintsev, Jevgeni; Hartonen, Kari; Jussila, Matti; Kulmala, Markku; Riekkola, Marja-Liisa

    2016-08-01

    Volatile organic compounds (VOCs) play a key role in atmospheric chemistry and physics. They participate in photochemical reactions in the atmosphere, which have direct implications on climate through, e.g. aerosol particle formation. Forests are important sources of VOCs, and the limited resources and infrastructures often found in many remote environments call for the development of portable devices. In this research, the potential of needle trap microextraction and portable gas chromatography-mass spectrometry for the study of VOCs at forest site was evaluated. Measurements were performed in summer and autumn 2014 at the Station for Measuring Ecosystem-Atmosphere Relations (SMEAR II) in Hyytiälä, Finland. During the first part of the campaign (summer) the applicability of the developed method was tested for the determination of monoterpenes, pinonaldehyde, aldehydes, amines and anthropogenic compounds. The temporal variation of aerosol precursors was determined, and evaluated against temperature and aerosol number concentration data. The most abundant monoterpenes, pinonaldehyde and aldehydes were successfully measured, their relative amounts being lower during days when particle number concentration was higher. Ethylbenzene, p- and m-xylene were also found when wind direction was from cities with substantial anthropogenic activity. An accumulation of VOCs in the snow cover was observed in the autumn campaign. Results demonstrated the successful applicability of needle trap microextraction and portable gas chromatography-mass spectrometry for the rapid in situ determination of organic gaseous compounds in the atmosphere.

  3. Fibre selection based on an overall analytical feature comparison for the solid-phase microextraction of trihalomethanes from drinking water.

    PubMed

    San Juan, Pedro Manuel; Carrillo, José David; Tena, María Teresa

    2007-01-12

    This paper describes the optimization of solid-phase microextraction (SPME) conditions for three different fibres (Carboxen-polydimethylsiloxane (CAR-PDMS), divinylbenzene-Carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB)) used to determine trihalomethanes (THMs) in water by headspace solid-phase microextraction and gas chromatography (HS-SPME-GC). The influence of temperature and salting-out effect was examined using a central composite design for each fibre. Extraction time was studied separately at the optimum values found for temperature and sodium chloride concentration (40 degrees C and 0.36g mL-1). The HS-SPME-GC-MS method for each fibre was characterised in terms of linearity, detection (LOD) and quantification (LOQ) limits and repeatability. The fibre PDMS-DVB was selected as it provided a broader linear range, better repeatability and lower detection and quantification limits than the others, particularly CAR-PDMS fibre. The accuracy of the proposed method using the PDMS-DVB fibre was checked by a recovery study in both ultrapure and tap water. A blank analysis study showed the absence of memory effects for this fibre. The reproducibility (expressed as a percentage of relative standard deviation) was 6-11% and the detection limits were between 0.078 and 0.52microgL-1 for bromoform and chloroform, respectively. Finally, the method was applied to determine THM concentration in two drinking water samples. PMID:17109874

  4. Enhancement for trace analysis of sulfonamide antibiotics in water matrices using bar adsorptive microextraction (BAμE).

    PubMed

    Ide, A H; Ahmad, S M; Neng, N R; Nogueira, J M F

    2016-09-10

    In this study, the enhancement for trace analysis of sulfonamide antibiotics (sulfathiazole, sulfamethoxazole and sulfadimethoxine) and trimethoprim in water matrices is proposed using bar adsorptive microextraction combined with micro-liquid desorption followed by high-performance liquid chromatography with diode array detection (BAμE-μLD/HPLC-DAD). By comparing different polymers and activated carbons as sorbent coatings for BAμE, the polystyrene-divinylbenzene polymer (PS-DVB) showed the best selectivity for the compounds under study. Assays performed through BAμE(PS-DVB)-μLD on 25mL of ultrapure water samples spiked at the 8.0μgL(-1) level showed recoveries ranging from 63.8±1.5% to 84.2±1.9%, under optimized experimental conditions. The validated method provided satisfactory limits of detection (0.08-0.16μgL(-1)) and good linear dynamic ranges (0.16-8.00μgL(-1)) with determination coefficients higher than 0.9958. The proposed analytical methodology was applied to real matrices, such as tap, estuarine and wastewater samples using the standard addition method. It showed to be easy to implement, with good reproducibility, sensitivity and requiring small amount of sample. Furthermore, negligible consumption of organic solvents was used in compliance with the green analytical chemistry principles. When compared to other well-established microextraction approaches, BAμE demonstrated better performance concerning recovery yields and sensitivity. PMID:27519155

  5. Carbonaceous nanomaterials immobilised mixed matrix membrane microextraction for the determination of polycyclic aromatic hydrocarbons in sewage pond water samples.

    PubMed

    Mukhtar, Nurul Hazirah; See, Hong Heng

    2016-08-10

    In this study, the potential for carbonaceous nanomaterials to be used as adsorbents for the mixed matrix membrane (MMM) microextraction and preconcentration of organic pollutants was demonstrated. For this method, multiwall carbon nanotubes (MWCNT) and single layer graphene (SLG) nanoparticles were individually incorporated through dispersion in a cellulose triacetate (CTA) polymer matrix to form a MWCNT-MMM and SLG-MMM, respectively. The prepared membranes were evaluated for the extraction of selected polycyclic aromatic hydrocarbons (PAHs) present in sewage pond water samples. The extraction was performed by dipping a small piece of membrane (7 mm × 7 mm) in a stirred 7.5 mL sample solution to initiate the analyte adsorption. This step was followed by an analyte desorption into 60 μL of methanol prior to high performance liquid chromatography (HPLC) analysis. When the optimum SLG-MMM microextraction technique was applied to spiked sewage pond water samples, the detection limit of the method for the PAHs were in the range of 0.02-0.09 ng/mL, with relative standard deviations of between 1.4% and 7.8%. Enrichment factors of 54-100 were achieved with relative recoveries of 99%-101%. A comparison was also made between the proposed approach and standard solid phase extraction using polymeric bonded octadecyl (C18) cartridges. PMID:27282751

  6. Determination of trace levels of triazines in corn matrices by bar adsorptive microextraction with a molecularly imprinted polymer.

    PubMed

    Andrade, Felipe Nascimento; Ide, Alessandra Honjo; Neng, Nuno da Rosa; Lanças, Fernando Mauro; Nogueira, José Manuel Florêncio

    2016-02-01

    This manuscript addresses the determination of triazines (ametryn, atrazine, simazine, and terbutryn) in corn matrices using bar adsorptive microextraction coated with a selective molecularly imprinted polymer phase following microliquid desorption and high-performance liquid chromatography with diode array detection. The molecularly imprinted polymer was synthesized using atrazine as a template and methacrylic acid as a functional monomer. Assays performed in 25 mL of ultrapure water samples spiked at 8.0 μg/L yielded 80-120 % recoveries under the evaluated experimental conditions. The method showed an accuracy (0.2 < bias < 17.9%), precision (relative standard deviation <17.4%), convenient detection (0.2 μg/L), and quantification (0.7 μg/L) limits, as well as linear dynamic ranges (0.8-24.0 μg/L) with remarkable determination coefficients (R(2) > 0.9926). The proposed analytical method was applied to monitor triazines in three types of corn matrices using the standard addition methodology. Experiments performed in corn samples spiked with triazines at the trace level (8.0 μg/kg of each analyte) gave rise to recoveries (81.0-119.4%) with good reproducibility and robustness. The proposed methodology is also easy to implement and showed to be a good analytical alternative to monitor triazines in complex matrices, when compared with other sorption-based microextraction techniques. PMID:26632142

  7. Silver nanoparticle aggregates on metal fibers for solid phase microextraction-surface enhanced Raman spectroscopy detection of polycyclic aromatic hydrocarbons.

    PubMed

    Liu, Cuicui; Zhang, Xiaoli; Li, Limei; Cui, Jingcheng; Shi, Yu-e; Wang, Le; Zhan, Jinhua

    2015-07-01

    Solid phase microextraction (SPME), a solvent free technique for sample preparation, has been successfully coupled with GC, GC-MS, and HPLC for environmental analysis. In this work, a method combining solid phase microextraction with surface enhanced Raman spectroscopy (SERS) is developed for detection of polycyclic aromatic hydrocarbons (PAHs). Silver nanoparticle aggregates were deposited on the Ag-Cu fibers via layer-by-layer deposition, which were modified with propanethiol (PTH). The SERS-active SPME fiber was immersed in water directly to extract PAHs and then detected using a portable Raman spectrometer. The pronounced valence vibration of the C-C bond at 1030 cm(-1) was chosen as an internal standard peak for the constant concentration of PTH. The RSD values of the stability and the uniformity of the SERS-active SPME fiber are 2.97% and 5.66%, respectively. A log-log plot of the normalized SERS intensity versus fluoranthene concentration showed a linear relationship (R(2) = 0.95). The detection limit was 7.56 × 10(-10) M and the recovery rate of water samples was in the range of 95% to 115%. The method can also be applied to detection of PAH mixtures, and each component of the mixtures can be distinguished by Raman characteristic peaks. The SERS-active SPME fiber could be further confirmed by GC-MS. PMID:25988666

  8. Optimization of a NH4PF6-enhanced, non-organic solvent, dual microextraction method for determination of phthalate metabolites in urine by high performance liquid chromatography.

    PubMed

    Wu, Jia; Ye, Zhihan; Li, Xiaolong; Wang, Xuedong; Luo, Fangjun; Sheng, Bo; Li, Yiwei; Lyu, Jianxin

    2016-03-01

    In conventional ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) procedures, most of the IL disperser remains in the aqueous phase resulting in low recovery for moderately and weakly polar analytes due to the "carry-over effect". Herein, we successfully developed a "NH4PF6-enhanced, non-organic solvent, dual microextraction" method (ANSDM) for pretreatment of phthalate (PAE) metabolites with weak to moderate polarity. This method utilized in situ reaction of NH4PF6 as an ion-exchange reagent and disperser to realize two microextractions after using [C8MIM]PF6 as an extraction solvent and [C4MIM]BF4 as a disperser for conventional DLLME. Single-factor experiments, a two-level full factorial experimental design and central composite design were applied for optimizing operational parameters using 3D response surfaces and contour lines. Under optimized conditions, the newly developed method provided high extraction recoveries (93.8-99.1%) and low LODs (ca. 0.3μgL(-1)) for three phthalate metabolites in human urine. The primary advantages of the ANSDM method include: (1) integration of in situ reaction and conventional DLLME techniques to effectively extract both weak and moderately polar pollutants simultaneously; (2) non-organic solvent use in the microextraction procedure making the process safer and more environmental friendly; and (3) a time-saving, simple operation that is fully compatibility with HPLC analysis. To the best of our knowledge, our group is the first to develop the "non-organic solvent, dual microextraction" method and it has great potential as a sample pre-treatment technique for organic pollutants with weak to moderate polarity in biological and environmental matrices. PMID:26852090

  9. Modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction combined with spectrofluorimetry for trace determination of ofloxacin in pharmaceutical and biological samples

    PubMed Central

    Zeeb, M.; Ganjali, M.R.; Norouzi, P.

    2011-01-01

    Background and the purpose of the study Ofloxacin is a quinolone synthetic antibiotic, which acts against resistant mutants of bacteria by inhibiting DNA gyrase. This antibacterial agent is widely used in the treatment of respiratory tract, urinary tract and tissue-based infections, which are caused by Gram-positive and Gram-negative bacteria. In this work, an efficient modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction (M-IL-CIA-DLLME) was combined with spectrofluorimetry for trace determination of ofloxacin in real samples. Methods In this microextraction method, hydrophobic 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim] [PF6]) ionic liquid (IL) as a microextraction solvent was dispersed into a heated sample solution containing sodium hexafluorophosphate (NaPF6) (as a common ion) and the analyte of interest. Afterwards, the resultant solution was cooled in an ice-water bath and a cloudy condition was formed due to a considerable decrease of IL solubility. After centrifuging, the enriched phase was introduced to the spectrofluorimeter for the determination of ofloxacin. Results and major conclusion In this technique, the performance of the microextraction method was not influenced by variations in the ionic strength of the sample solution (up to 30% w/v). Furthermore, [Hmim][PF6] IL was chosen as a green microextraction phase and an alternative to traditional toxic organic solvents. Different parameters affecting the analytical performance were studied and optimized. At optimum conditions, a relatively broad linear dynamic range of 0.15-125 µg l-1 and a limit of detection (LOD) of 0.029 µg l-1 were obtained. The relative standard deviation (R.S.D.) obtained for the determination of five replicates of the 10 ml solution containing 50 µg l-1 ofloxacin was 2.7%. Finally, the combined methodology was successfully applied to ofloxacin determination in actual pharmaceutical formulations and biological samples. PMID

  10. Headspace solid-phase microextraction-gas chromatography-mass spectrometry characterization of propolis volatile compounds.

    PubMed

    Pellati, Federica; Prencipe, Francesco Pio; Benvenuti, Stefania

    2013-10-01

    In this study, a novel and efficient method based on headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-mass spectrometry (GC-MS), was developed for the analysis of propolis volatile compounds. The HS-SPME procedure, whose experimental parameters were properly optimized, was carried out using a 100 μm polydimethylsiloxane (PDMS) fiber. The GC-MS analyses were performed on a HP-5 MS cross-linked 5% diphenyl-95% dimethyl polysiloxane capillary column (30 m × 0.25 mm I.D., 1.00 μm film thickness), under programmed-temperature elution. Ninety-nine constituents were identified using this technique in the samples of raw propolis collected from different Italian regions. The main compounds detected include benzoic acid (0.87-30.13%) and its esters, such as benzyl benzoate (0.16-13.05%), benzyl salicylate (0.34-1.90%) and benzyl cinnamate (0.34-3.20%). Vanillin was detected in most of the samples analyzed in this study (0.07-5.44%). Another relevant class of volatile constituents is represented by sesquiterpene hydrocarbons, such as δ-cadinene (1.29-13.31%), γ-cadinene (1.36-8.85%) and α-muurolene (0.78-6.59%), and oxygenated sesquiterpenes, such as β-eudesmol (2.33-12.83%), T-cadinol (2.73-9.95%) and α-cadinol (4.84-9.74%). Regarding monoterpene hydrocarbons, they were found to be present at low level in the samples analyzed in this study, with the exception of one sample from Southern Italy, where α-pinene was the most abundant constituent (13.19%). The results obtained by HS-SPME-GC-MS were also compared with those of hydrodistillation (HD) coupled with GC-MS. The HS-SPME-GC-MS method developed in this study allowed us to determine the chemical fingerprint of propolis volatile constituents, thus providing a new and reliable tool for the complete characterization of this biologically active apiary product. PMID:23807002

  11. Dispersive liquid-liquid microextraction coupled to liquid chromatography for thiamine determination in foods.

    PubMed

    Viñas, Pilar; López-García, Ignacio; Bravo-Bravo, María; Briceño, Marisol; Hernández-Córdoba, Manuel

    2012-05-01

    A miniaturized dispersive liquid-liquid microextraction (DLLME) procedure coupled to liquid chromatography (LC) with fluorimetric detection was evaluated for the preconcentration and determination of thiamine (vitamin B(1)). Derivatization was carried out by chemical oxidation of thiamine with 5 × 10(-5) M ferricyanide at pH 13 to form fluorescent thiochrome. For DLLME, 0.5 mL of acetonitrile (dispersing solvent) containing 90 μL of tetrachloroethane (extraction solvent) was rapidly injected into 10 mL of sample solution containing the derivatized thiochrome and 24% (w/v) sodium chloride, thereby forming a cloudy solution. Phase separation was carried out by centrifugation, and a volume of 20 μL of the sedimented phase was submitted to LC. The mobile phase was a mixture of a 90% (v/v) 10 mM KH(2)PO(4) (pH 7) solution and 10% (v/v) acetonitrile at 1 mL min(-1). An amide-based stationary phase involving a ligand with amide groups and the endcapping of trimethylsilyl was used. Specificity, linearity, precision, recovery, and sensitivity were satisfactory. Calibration graph was carried out by the standard additions method and was linear between 1 and 10 ng mL(-1). The detection limit was 0.09 ng mL(-1). The selectivity of the method was judged from the absence of interfering peaks at the thiamine elution time for blank chromatograms of unspiked samples. A relative standard deviation of 3.2% was obtained for a standard solution containing thiamine at 5 ng mL(-1). The esters thiamine monophosphate and thiamine pyrophosphate can also be determined by submitting the sample to successive acid and enzymatic treatments. The method was applied to the determination of thiamine in different foods such as beer, brewer's yeast, honey, and baby foods including infant formulas, fermented milk, cereals, and purees. For the analysis of solid samples, a previous extraction step was applied based on an acid hydrolysis with trichloroacetic acid. The reliability of the procedure was

  12. Optimization of headspace solid-phase microextraction gas chromatography-atomic emission detection analysis of monomethylmercury.

    PubMed

    Geerdink, René Bernard; Breidenbach, Rembert; Epema, Onno Jacob

    2007-12-01

    Optimum conditions for headspace solid-phase microextraction (HS-SPME) in the analysis of monomethylmercury (MeHg) have been determined. Sodium tetra(n-)propylborate (NaBPr(4)) is used as derivatization reagent to promote volatility. A simple aluminium bar was used to cool the SPME fiber to about 2 degrees C during the equilibration phase just before extraction. HS-SPME was performed using different fibers. The 100 microm polydimethylsiloxane (PDMS) and 65 microm polydimethylsiloxane-divinylbenzene (PDMS-DVB) fibers showed the best results. Although the extraction efficiency for MeHg derivative of the polydimethylsiloxane-Carboxen (PDMS-CAR) fiber is similar to the other fibers, desorption of MeHg derivative from a PDMS-CAR fiber is poor. Factors affecting the HS-SPME process such as adsorption and desorption times, ionic strength (salting-out) and extraction temperature have been evaluated and optimized thoroughly. The highest extraction efficiency for the PDMS fiber was obtained by extraction at a low temperature (2 degrees C) immediately after equilibration at 30 degrees C. With the PDMS-DVB and PDMS-CAR fiber improvement of extraction efficiency at lower temperatures is negligible. Repeated extraction out of the same vial revealed that about 30% of MeHg derivative is extracted from the headspace with a PDMS fiber at 2 degrees C and about 70% with a PDMS-DVB fiber. Repeated extraction with two different fiber coatings showed that the PDMS-CAR fiber also extracts about 70% but that the desorption is incomplete. Attempts to improve the desorption failed due to degradation of the MeHg derivate at high injection temperatures. The limit of detection (3sigma) was 16 pg/L MeHg. The relative standard deviation (n = 8) for 100 pg/L of MeHg was found to be 5%. Linearity of the HS-SPME-GC-atomic emission detection method was established over at least two orders of magnitude in the range 0-2000 pg/L. Recovery of a surface water sample spiked at 2 ng/L was 85%. The

  13. Rapid determination of lead in water samples by dispersive liquid-liquid microextraction coupled with electrothermal atomic absorption spectrometry.

    PubMed

    Naseri, Mohammad Taghi; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub; Kiani, Armin

    2008-03-15

    The need for highly reliable methods for the determination of trace and ultratrace elements has been recognized in analytical chemistry and environmental science. A simple and powerful microextraction technique was used for the detection of the lead ultratrace amounts in water samples using the dispersive liquid-liquid microextraction (DLLME), followed by the electrothermal atomic absorption spectrometry (ET AAS). In this microextraction technique, a mixture of 0.50 mL acetone (disperser solvent), containing 35 microL carbon tetrachloride (extraction solvent) and 5 microL diethyldithiophosphoric acid (chelating agent), was rapidly injected by syringe into the 5.00 mL water sample, spiked with lead. In this process, the lead ions reacted with the chelating agent and were extracted into the fine droplets of CCl(4). After centrifugation (2 min at 5000 rpm), the fine CCl4 droplets were sedimented at the bottom of the conical test tube (25+/-1 microL). Then, 20 microL from the sedimented phase, containing the enriched analyte, was determined by ET AAS. The next step was the optimization of various experimental conditions, affecting DLLME, such as the type and the volume of the extraction solvent, the type and the volume of the disperser solvent, the extraction time, the salt effect, pH and the chelating agent amount. Moreover, the effect of the interfering ions on the analytes recovery was also investigated. Under the optimum conditions, the enrichment factor of 150 was obtained from only a 5.00 mL water sample. The calibration graph was linear in the range of 0.05-1 microg L(-1) with the detection limit of 0.02 microg L(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 0.50 microg L(-1) of lead was 2.5%. The relative lead recoveries in mineral, tap, well and sea water samples at the spiking level of 0.20 and 0.40 microg L(-1) varied from 93.5 to 105.0. The characteristics of the proposed method were compared with the cloud point

  14. Hollow fiber liquid-liquid-liquid microextraction followed by solid-phase microextraction and in situ derivatization for the determination of chlorophenols by gas chromatography-electron capture detection.

    PubMed

    Saraji, Mohammad; Ghani, Milad

    2015-10-30

    A method based on the combination of hollow fiber liquid-liquid-liquid microextraction and solid-phase microextraction (SPME) followed by gas chromatography-electron capture detection was developed for the determination of chlorophenols in water and wastewater samples. Silica microstructures fabricated on the surface of a stainless steel wire were coated by an organic solvent and used as a SPME fiber. The analytes were extracted through a hollow fiber membrane containing n-decane from sample solution to an alkaline aqueous acceptor phase. They were then extracted and in situ derivatized on the SPME fiber using acetic anhydride. Experimental parameters such as the type of extraction solvent, acceptor phase NaOH concentration, donor phase HCl concentration, the amount of derivatizing reagent, salt concentration, stirring rate and extraction time were investigated and optimized. The precision of the method for the analytes at 0.02-30μgL(-1) concentration level ranged from 7.1 to 10.2% (as intra-day relative standard deviation) and 6.4 to 9.8% (as inter-day relative standard deviation). The linear dynamic ranges were in the interval of 5-500μgL(-1), 0.05-5μgL(-1), 0.02-1μgL(-1) and 0.001-0.5μgL(-1) for 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol, respectively. The enrichment factors were between 432 and 785. The limits of detection were in the range of 0.0004-1.2μgL(-1). Tap water, well water and wastewater samples were also analyzed to evaluate the method capability for real sample analysis. PMID:26411480

  15. Ultra-sensitive determination of cadmium in rice and water by UV-vis spectrophotometry after single drop microextraction.

    PubMed

    Wen, Xiaodong; Deng, Qingwen; Guo, Jie; Yang, Shengchun

    2011-08-01

    In this work, a new method based on single drop microextraction (SDME) preconcentration using tetrachloromethane (CCl(4)) as extraction solvent was proposed for the spectrophotometric determination of cadmium in rice and water samples. The influence factors relevant to SDME, such as type and volume of extractant, stirring rate and time, dithizone concentration, pH, drop volume and instrumental conditions were studied systematically. Under the optimal conditions, the limit of detection (LOD) was 0.5 ng L(-1), with sensitivity enhancement factor (EF) of 128. The different maximum absorption wavelength caused by the different extraction acidity compared with some conventional works and the enhancement effect of acetone (dilution solvent) for the spectrophotometric determination were the two key factors of the high EF and sensitivity. The proposed method was applied to the determination of rice and water samples with satisfactory analytical results. The proposed method was simple, rapid, cost-efficient and sensitive. PMID:21530375

  16. Ultra-sensitive determination of cadmium in rice and water by UV-vis spectrophotometry after single drop microextraction

    NASA Astrophysics Data System (ADS)

    Wen, Xiaodong; Deng, Qingwen; Guo, Jie; Yang, Shengchun

    2011-08-01

    In this work, a new method based on single drop microextraction (SDME) preconcentration using tetrachloromethane (CCl 4) as extraction solvent was proposed for the spectrophotometric determination of cadmium in rice and water samples. The influence factors relevant to SDME, such as type and volume of extractant, stirring rate and time, dithizone concentration, pH, drop volume and instrumental conditions were studied systematically. Under the optimal conditions, the limit of detection (LOD) was 0.5 ng L -1, with sensitivity enhancement factor (EF) of 128. The different maximum absorption wavelength caused by the different extraction acidity compared with some conventional works and the enhancement effect of acetone (dilution solvent) for the spectrophotometric determination were the two key factors of the high EF and sensitivity. The proposed method was applied to the determination of rice and water samples with satisfactory analytical results. The proposed method was simple, rapid, cost-efficient and sensitive.

  17. Application of liquid-phase microextraction for the determination of sulfur compounds in crude oil and diesel.

    PubMed

    Al-Zahrani, Ibrahim; Basheer, Chanbasha; Htun, Than

    2014-02-21

    A liquid-phase microextraction (LPME) method was for the first time developed for the determination of sulfur compounds in Arabian crude oil and diesel. A wide range of sulfur compounds, which included benzothiophene, dibenzothiophene and their derivatives, was used for model compounds. The analyses were performed by a gas chromatography equipped with a sulfur chemiluminescence detector (GC-SCD). Under optimum conditions, a linearity was achieved for the extraction sulfur compounds between 0.10 and 250μgmL(-1) with the correlation of determination ranging from 0.98 to 0.99. Applying the same optimum conditions, the extraction of 77-91% of the sulfur compounds in the Arabian light, Arabian medium and Arabian heavy, and diesel was achieved. PMID:24461639

  18. Comparison of headspace solid-phase microextraction with conventional extraction for the analysis of the volatile components in Melia azedarach.

    PubMed

    Yang, Yanqin; Xiao, Yanmeng; Liu, Baofeng; Fang, Xuexun; Yang, Wei; Xu, Jingwei

    2011-10-30

    The volatile compositions of Melia azedarach were studied by headspace solid-phase microextraction (HS-SPME). The result was compared with that obtained by soxhlet extraction (SE) and ultrasonic extraction (UAE). 79 compounds were identified in this study, among which 64 compounds were first reported. The experimental parameters including fiber type (PDMS, PDMS-DVB and CAR-PDMS), desorption time, extraction temperature and time were investigated. 37 compounds were obtained by HS-SPME, including curcumene (33.25%), α-cadinol (11.16%), α-muurolene (8.72%), copaene (5.04%), β-bisabolene (3.41%), and α-selinene (2.97%). The result suggested that the HS-SPME method is a powerful analytic tool and complementary to traditional methods for the determination of the volatile compounds in Chinese herbs. PMID:22063551

  19. Volatile constituents of Murraya koenigii fresh leaves using headspace solid phase microextraction--gas chromatography-mass spectrometry.

    PubMed

    Sukkaew, Sayamol; Pripdeevech, Patcharee; Thongpoon, Chalermporn; Machan, Theeraphan; Wongchuphan, Rattana

    2014-12-01

    The volatile components of Murraya koenigii fresh leaves, collected from Surat Thani province, Thailand were studied by using headspace (HS) solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS). The four fibers employed to extract the volatiles were polydimethylsiloxane (PDMS), polydimethylsiloxane-divinylbenzene (PDMS-DVB), carboxane-polydimethylsiloxane (CAR-PDMS) and polydimethylsiloxane-divinylbenzene-carboxane (PDMS-DVB-CAR). The volatile constituents of M. koenigii fresh leaves were also extracted by hydrodistillation and analyzed by GC-MS. Fifty-one compounds were identified by these fibers. Five major compounds, γ-terpinene, β-caryophyllene, β-phellandrene, a-selinene and a-pinene, were detected in all fibers. The PDMS-DVB-CAR fiber was considered as the best for trapping key volatiles of M. koenigii fresh leaves. PMID:25632485

  20. Measurement uncertainty for the determination of amphetamines in urine by liquid-phase microextraction and gas chromatography-mass spectrometry.

    PubMed

    Franco de Oliveira, Sarah Carobini Werner de Souza Eller; Yonamine, Mauricio

    2016-08-01

    A gas chromatography-mass spectrometry method for the determination of amphetamines in urine samples by means of liquid-phase microextraction was validated, including calculation of measurement uncertainty. After extraction in the three-phase mode, acceptor phase was withdrawn from the fiber and the residue was derivatized with trifluoroacetic anhydride. The method showed to be very simple, rapid and it required a significantly low amount of organic solvent for extraction. The limits of detection were 10 and 20μg/L for amphetamine and methamphetamine, respectively. The calibration curves were linear over the specified range (20μg/L to 1400μg/L; r(2)>0.99). The method showed to be both precise and accurate and a relative combined uncertainty of 2% was calculated. In order of importance, the factors which were more determinant for the calculation of method uncertainty were: analyte concentration, sample volume, trueness and method precision. PMID:26836147