Preparation and utilization of molecularly imprinted polymer for chlorsulfuron extraction from water, soil, and wheat plant.

PubMed

Fu, Xu Wei; Wu, Yan Jiao; Qu, Jin Rong; Yang, Hong

2012-07-01

A molecularly imprinted polymer (MIP) was prepared using chlorsulfuron (CS), a herbicide as a template molecule, methacrylic acid as a functional monomer, ethylene glycol dimethacrylate (EDMA) as a cross-linker, methanol and toluene as a porogen, and 2,2-azobisisobutyronitrile as an initiator. The binding behaviors of the template chlorsulfuron and its analog on MIP were evaluated by equilibrium adsorption experiments, which showed that the MIP particles had specific affinity for the template CS. Solid-phase extraction (SPE) with the chlorsulfuron molecularly imprinted polymer as an adsorbent was investigated. The optimum loading, washing, and eluting conditions for chlorsulfuron molecularly imprinted polymer solid-phase extraction (CS-MISPE) were established. The optimized CS-MISPE procedure was developed to enrich and clean up the chlorsulfuron residue in water, soils, and wheat plants. Concentrations of chlorsulfuron in the samples were analyzed by HPLC-UVD. The average recoveries of CS spiked standard at 0.05~0.2 mg L(-1) in water were 90.2~93.3%, with the relative standard deviation (RSD) being 2.0~3.9% (n=3). The average recoveries of 1.0 mL CS spiked standard at 0.1~0.5 mg L(-1) in 10 g soil were 91.1~94.7%, with the RSD being 3.1~5.6% (n=3). The average recoveries of 1.0 mL CS spiked standard at 0.1~0.5 mg L(-1) in 5 g wheat plant were 82.3~94.3%, with the RSD being 2.9~6.8% (n=3). Overall, our study provides a sensitive and cost-effective method for accurate determination of CS residues in water, soils, and plants.

Outcomes of minimally invasive simple prostatectomy for benign prostatic hyperplasia: a systematic review and meta-analysis.

PubMed

Lucca, Ilaria; Shariat, Shahrokh F; Hofbauer, Sebastian L; Klatte, Tobias

2015-04-01

(1) To assess the outcomes of minimally invasive simple prostatectomy (MISP) for the treatment of symptomatic benign prostatic hyperplasia in men with large prostates and (2) to compare them with open simple prostatectomy (OSP). A systematic review of outcomes of MISP for benign prostatic hyperplasia with meta-analysis was conducted. The article selection process was conducted according to the PRISMA guidelines. Twenty-seven observational studies with 764 patients were analyzed. The mean prostate volume was 113.5 ml (95 % CI 106-121). The mean increase in Qmax was 14.3 ml/s (95 % CI 13.1-15.6), and the mean improvement in IPSS was 17.2 (95 % CI 15.2-19.2). Mean duration of operation was 141 min (95 % CI 124-159), and the mean intraoperative blood loss was 284 ml (95 % CI 243-325). One hundred and four patients (13.6 %) developed a surgical complication. In comparative studies, length of hospital stay (WMD -1.6 days, p = 0.02), length of catheter use (WMD -1.3 days, p = 0.04) and estimated blood loss (WMD -187 ml, p = 0.015) were significantly lower in the MISP group, while the duration of operation was longer than in OSP (WMD 37.8 min, p < 0.0001). There were no differences in improvements in Qmax, IPSS and perioperative complications between both procedures. The small study sizes, publication bias, lack of systematic complication reporting and short follow-up are limitations. MISP seems an effective and safe treatment option. It provides similar improvements in Qmax and IPSS as OSP. Despite taking longer, it results in less blood loss and shorter hospital stay. Prospective randomized studies comparing OSP, MISP and laser enucleation are needed to define the standard surgical treatment for large prostates.

Separation and determination of citrinin in corn using HPLC fluorescence detection assisted by molecularly imprinted solid phase extraction clean-up

USDA-ARS?s Scientific Manuscript database

A liquid chromatography based method to detect citrinin in corn was developed using molecularly imprinted solid phase extraction (MISPE) sample clean-up. Molecularly imprinted polymers were synthesized using 1,4-dihydroxy-2-naphthoic acid as the template and an amine functional monomer. Density func...

Digital Imagery Compression Best Practices Guide - A Motion Imagery Standards Profile (MISP) Compliant Architecture

DTIC Science & Technology

2012-06-01

MISP) COMPLIANT ARCHITECTURE WHITE SANDS MISSILE RANGE REAGAN TEST SITE YUMA PROVING GROUND DUGWAY PROVING GROUND ABERDEEN TEST CENTER...DIGITAL MOTION IMAGERY COMPRESSION BEST PRACTICES GUIDE – A MOTION IMAGERY STANDARDS PROFILE (MISP) COMPLIANT ARCHITECTURE ...delivery, and archival purposes. These practices are based on a Motion Imagery Standards Profile (MISP) compliant architecture , which has been defined

Analysis of alternariol and alternariol monomethyl ether in foodstuffs by molecularly imprinted solid-phase extraction and ultra-high-performance liquid chromatography tandem mass spectrometry.

PubMed

Rico-Yuste, A; Walravens, J; Urraca, J L; Abou-Hany, R A G; Descalzo, A B; Orellana, G; Rychlik, M; De Saeger, S; Moreno-Bondi, M C

2018-03-15

Molecularly imprinted porous polymer microspheres selective to Alternaria mycotoxins, alternariol (AOH) and alternariol monomethyl ether (AME), were synthesized and applied to the extraction of both mycotoxins in food samples. The polymer was prepared using 4-vinylpiridine (VIPY) and methacrylamide (MAM) as functional monomers, ethylene glycol dimethacrylate (EDMA) as cross-linker and 3,8,9-trihydroxy-6H-dibenzo[b,d]pyran-6-one (S2) as AOH surrogate template. A molecularly imprinted solid phase extraction (MISPE) method has been optimized for the selective isolation of the mycotoxins from aqueous samples coupled to HPLC with fluorescence (λ ex =258nm; λ em =440nm) or MS/MS analysis. The MISPE method was validated by UPLC-MS/MS for the determination of AOH and AME in tomato juice and sesame oil based on the European Commission Decision 2002/657/EC. Method performance was satisfactory with recoveries from 92.5% to 106.2% and limits of quantification within the 1.1-2.8µgkg -1 range in both samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparation of molecular imprinted microspheres based on inorganic-organic co-functional monomer for miniaturized solid-phase extraction of fluoroquinolones in milk.

PubMed

Wang, Hui; Wang, Ruiling; Han, Yehong

2014-02-15

An inorganic-organic co-functional monomer, methacrylic acid-vinyltriethoxysilan (MAA-VTES) was designed for the synthesis of molecularly imprinted microspheres (MIMs). By virtue of the aqueous suspension polymerization and dummy template (pazufloxacin), the obtained MAA-VTES based MIMs exhibited good recognition and selectivity to fluoroquinolones (FQs), and were successfully applied as selective sorbents of a miniaturized home-made solid phase extraction device for the determination of ofloxacin (OFL), lomefloxacin (LOM) and ciprofloxacin (CIP) in milk samples. Under the optimum conditions of the miniaturized molecularly imprinted solid phase extraction (mini-MISPE) coupled with liquid chromatography-ultraviolet detector (LC-UV), good linearities were obtained for three FQs in a range of 0.2-20.0μgmL(-1) and the average recoveries at three spiked levels were ranged from 87.2% to 106.1% with the relative standard deviation (RSD) less than 5.4%. The presented co-functional monomer based mini-MISPE-LC-UV protocol introduced the rigidity and flexibility of inorganic silicon materials, exhibited excellent extraction performance towards targets, and could be potentially applied to the determination of FQs in milk samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Molecularly imprinted polymer solid-phase extraction coupled to square wave voltammetry at carbon fibre microelectrodes for the determination of fenbendazole in beef liver.

PubMed

Guzmán-Vázquez de Prada, A; Loaiza, Oscar A; Serra, B; Morales, D; Martínez-Ruiz, P; Reviejo, A J; Pingarrón, J M

2007-05-01

A molecularly imprinted polymer was developed and used for solid-phase extraction (MISPE) of the antihelmintic fenbendazole in beef liver samples. Detection of the analyte was accomplished using square wave voltammetry (SWV) at a cylindrical carbon fibre microelectrode (CFME). A mixture of MeOH/HAc (9:1) was employed both as eluent in the MISPE system and as working medium for electrochemical detection of fenbendazole. The limit of detection was 1.9x10(-7) mol L-1 (57 microg L-1), which was appropriate for the determination of fenbendazole at the maximum residue level permitted by the European Commission (500 microg kg-1 in liver). Given that the SW voltammetric analysis could not be directly performed in the sample extract as a consequence of interference from some sample components, a sample clean-up with a MIP for selectively retaining fenbendazole was performed. The MIP was synthesized using a 1:8:22 template/methacrylic acid/ethylene glycol dimethacrylate ratio. A Britton-Robinson Buffer of pH 9.0 was selected for retaining fenbendazole in the MIP cartridges, and an eluent volume of 5.0 mL at a flow rate of 2.0 mL min-1 was chosen in the elution step. Cross-reactivity with the MIP was observed for other benzimidazoles. The synthesized MIP exhibited a good selectivity for benzimidazoles with respect to other veterinary drugs. The applicability of the MISPE-SWV method was tested with beef liver samples, spiked with fenbendazole at 5,000 and 500 microg kg-1. Results obtained for ten different liver samples yielded mean recoveries of (95+/-12)% and (96+/-11)% for the upper and lower concentration level, respectively.

Determination of fusaric acid in maize using molecularly imprinted SPE clean-up

USDA-ARS?s Scientific Manuscript database

A new liquid chromatography method to detect fusaric acid in maize is reported based on molecularly imprinted polymer solid phase extraction clean-up (MISPE) using mimic-templated molecularly-imprinted polymers. Picolinic acid was used as a toxin analog for imprinting polymers during a thermolytic s...

Simultaneous determination of four plant hormones in bananas by molecularly imprinted solid-phase extraction coupled with high performance liquid chromatography.

PubMed

Yan, Hongyuan; Wang, Fang; Han, Dandan; Yang, Gengliang

2012-06-21

A highly selective molecularly imprinted solid-phase extraction (MISPE) combined with liquid chromatography-ultraviolet detection was developed for the simultaneous isolation and determination of four plant hormones including indole-3-acetic acid (IAA), indole-3-propionic acid (IPA), indole-3-butyric acid (IBA) and 1-naphthaleneacetic acid (NAA) in banana samples. The new molecularly imprinted microspheres (MIMs) prepared by aqueous suspension polymerization using 3-hydroxy-2-naphthoic acid and 1-methylpiperazine as mimic templates performed with high selectivity and affinity for the four plant hormones, and applied as selective sorbents of solid-phase extraction could effectively eliminate the interferences of the banana matrix. Good linearity was obtained in a range of 0.04-4.00 μg g(-1) and the recoveries of the four plant hormones at three spiked levels ranged from 78.5 to 107.7% with the relative standard deviations (RSD) of less than 4.6%. The developed MISPE-HPLC protocol obviously improved the selectivity and eliminated the effect of template leakage on quantitative analysis, and could be applied for the determination of plant hormones in complicated biological samples.

Minimum initial service package (MISP) for sexual and reproductive health in disasters.

PubMed

Lisam, Suchitra

2014-12-01

This paper is based on a presentation given at the Evidence Aid Symposium, on 20 September 2014, at Hyderabad, India. The paper provides background about how the sexual and reproductive health (SRH) got conceived as a humanitarian health response that adopts human right approach, based on core principles driven by needs of adolescent girls and women, and having respect for their values, ethics and morals. Good practices across nations documented by Inter-Agency Working Groups (IAWGs) on Reproductive Health in Humanitarian Crisis has supported the provision of essential SRH care services to adolescent girls and women in humanitarian crisis and in disasters. Secondary desk review is used to document the lessons learnt and good practices followed and documents for SRH. These essential SRH care services are to be provided as "Minimum Initial Service Package (MISP)" for implementation at the outset of disaster. The Sphere Humanitarian Charter and Minimum Standards in Disaster Response incorporated the MISP for SRH as a minimum standard of care in disaster response with a goal to reduce mortality, morbidity and disability among populations affected by crises, particularly women and girls. Disaster prone countries are expected to roll out MISP to improve humanitarian response and emergency preparedness systems. The East Europe and Central Asia (EECA) region including India have rolled out MISP starting from 2011 (EECA) and from 2013-2014 onwards in India across cities such as Chennai, Patna, Bhubaneshwar, Kolkata, Faridabad and Calcutta. Across India, through these national and state level trainings, nearly 600 people from NGOs, institutions, and government agencies were developed as national level trainers and resource persons for MISP who could advocate for RH in emergencies, apply core techniques provided in the MISP, apply coordination skills for the implementation of MISP and develop an action plan to integrate RH and Gender Based Violence (GBV) into Disaster Management Plans of respective agencies. The way forward includes focusing on MISP distance learning module, integration of MISP in Health action plans, and integration into national disaster preparedness and contingency planning of respective agencies and departments and building capacity at various levels. © 2014 Chinese Cochrane Center, West China Hospital of Sichuan University and Wiley Publishing Asia Pty Ltd.

Molecularly imprinted polymer for selective extraction of malachite green from seawater and seafood coupled with high-performance liquid chromatographic determination.

PubMed

Lian, Ziru; Wang, Jiangtao

2012-12-01

In this paper, a highly selective sample cleanup procedure combining molecular imprinting technique (MIT) and solid-phase extraction (SPE) was developed for the isolation of malachite green in seawater and seafood samples. The molecularly imprinted polymer (MIP) was prepared using malachite green as the template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking monomer. The imprinted polymer and non-imprinted polymer were characterized by scanning electron microscope and static adsorption experiments. The MIP showed a high adsorption capacity and was used as selective sorbent for the SPE of malachite green. An off-line molecularly imprinted solid-phase extraction (MISPE) method followed by high-performance liquid chromatography with diodearray detection for the analysis of malachite green in seawater and seafood samples was also established. Finally, five samples were determined. The results showed that malachite green concentration in one seawater sample was at 1.30 μg L⁻¹ and the RSD (n=3) was 4.15%. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

Computer-assisted design and synthesis of molecularly imprinted polymers for selective extraction of acetazolamide from human plasma prior to its voltammetric determination.

PubMed

Khodadadian, Mehdi; Ahmadi, Farhad

2010-06-15

Molecularly imprinted polymers (MIPs) were computationally designed and synthesized for the selective extraction of a carbonic anhydrase inhibitor, i.e. acetazolamide (ACZ), from human plasma. Density functional theory (DFT) calculations were performed to study the intermolecular interactions in the pre-polymerization mixture and to find a suitable functional monomer in MIP preparation. The interaction energies were corrected for the basis set superposition error (BSSE) using the counterpoise (CP) correction. The polymerization solvent was simulated by means of polarizable continuum model (PCM). It was found that acrylamide (AAM) is the best candidate to prepare MIPs. To confirm the results of theoretical calculations, three MIPs were synthesized with different functional monomers and evaluated using Langmuir-Freundlich (LF) isotherm. The results indicated that the most homogeneous MIP with the highest number of binding sites is the MIP prepared by AAM. This polymer was then used as a selective adsorbent to develop a molecularly imprinted solid-phase extraction procedure followed by differential pulse voltammetry (MISPE-DPV) for clean-up and determination of ACZ in human plasma.

MISPS: Module integrated solar position sensor for concentration photovoltaics

NASA Astrophysics Data System (ADS)

Pardell, Ricard

2012-10-01

This paper describes a new device, the MISPS (Module Integrated. Solar Position Sensor) for CPV systems. Its main innovation lies in it being module integrated, so that the sensor is a constituent part of the module and uses its optics. The MISPS has been designed within the scope of the CPVRS project, but it can be used in any refractive optics CPV system.

Design and development of molecularly imprinted polymers for the selective extraction of deltamethrin in olive oil: An integrated computational-assisted approach.

PubMed

Martins, Nuno; Carreiro, Elisabete P; Locati, Abel; Ramalho, João P Prates; Cabrita, Maria João; Burke, Anthony J; Garcia, Raquel

2015-08-28

This work firstly addresses the design and development of molecularly imprinted systems selective for deltamethrin aiming to provide a suitable sorbent for solid phase (SPE) extraction that will be further used for the implementation of an analytical methodology for the trace analysis of the target pesticide in spiked olive oil samples. To achieve this goal, a preliminary evaluation of the molecular recognition and selectivity of the molecularly imprinted polymers has been performed. In order to investigate the complexity of the mechanistic basis for template selective recognition in these polymeric matrices, the use of a quantum chemical approach has been attempted providing new insights about the mechanisms underlying template recognition, and in particular the crucial role of the crosslinker agent and the solvent used. Thus, DFT calculations corroborate the results obtained by experimental molecular recognition assays enabling one to select the most suitable imprinting system for MISPE extraction technique which encompasses acrylamide as functional monomer and ethylene glycol dimethacrylate as crosslinker. Furthermore, an analytical methodology comprising a sample preparation step based on solid phase extraction has been implemented using this "tailor made" imprinting system as sorbent, for the selective isolation/pre-concentration of deltamethrin from olive oil samples. Molecularly imprinted solid phase extraction (MISPE) methodology was successfully applied for the clean-up of spiked olive oil samples, with recovery rates up to 94%. Copyright © 2015 Elsevier B.V. All rights reserved.

Mars Science Laboratory (MSL) Entry, Descent, and Landing Instrumentation (MEDLI): Complete Flight Data Set

NASA Technical Reports Server (NTRS)

Cheatwood, F. McNeil; Bose, Deepak; Karlgaard, Christopher D.; Kuhl, Christopher A.; Santos, Jose A.; Wright, Michael J.

2014-01-01

The Mars Science Laboratory (MSL) entry vehicle (EV) successfully entered the Mars atmosphere and landed the Curiosity rover safely on the surface of the planet in Gale crater on August 6, 2012. MSL carried the MSL Entry, Descent, and Landing (EDL) Instrumentation (MEDLI). MEDLI delivered the first in-depth understanding of the Mars entry environments and the response of the entry vehicle to those environments. MEDLI was comprised of three major subsystems: the Mars Entry Atmospheric Data System (MEADS), the MEDLI Integrated Sensor Plugs (MISP), and the Sensor Support Electronics (SSE). Ultimately, the entire MEDLI sensor suite consisting of both MEADS and MISP provided measurements that were used for trajectory reconstruction and engineering validation of aerodynamic, atmospheric, and thermal protection system (TPS) models in addition to Earth-based systems testing procedures. This report contains in-depth hardware descriptions, performance evaluation, and data information of the three MEDLI subsystems.

Selective trace enrichment of acidic pharmaceuticals in real water and sediment samples based on solid-phase extraction using multi-templates molecularly imprinted polymers.

PubMed

Duan, Yan-Ping; Dai, Chao-Meng; Zhang, Ya-Lei; Ling-Chen

2013-01-03

A novel multi-templates molecularly imprinted polymer (MIP), using acidic pharmaceuticals mixture (ibuprofen (IBP), naproxen (NPX), ketoprofen (KEP), diclofenac (DFC), and clofibric acid (CA)) as the template, was prepared as solid-phase extraction (SPE) material for the quantitative enrichment of acidic pharmaceuticals in environmental samples and off-line coupled with liquid chromatography-mass spectrometry (LC/MS/MS). Washing solvent was optimized in terms of kind and volume for removing the matrix constituents nonspecifically adsorbed on the MIP. When 1L of water sample spiked at 1μg/L was loaded onto the cartridge, the binding capacity of the MIP cartridge were 48.7μg/g for KEP, 60.7μg/g for NPX, 52μg/g for CA, 61.3μg/g for DFC and 60.7μg/g for IBP, respectively, which are higher than those of the commercial single template MIP in organic medium (e.g. toluene) reported in the literature. Recoveries of the five acidic pharmaceuticals extracted from 1L of real water samples such as lake water and wastewater spiked at 1μg/L were more than 95%. The recoveries of acidic pharmaceuticals extracted from 10-g sediment sample spiked at the 10ng/g level were in the range of 77.4-90.6%. To demonstrate the potential of the MIP obtained, a comparison with commercial C18 SPE cartridge was performed. Molecularly imprinted solid-phase extraction (MISPE) cartridge showed higher recoveries than commercial C18 SPE cartridge for acidic pharmaceuticals. These results showed the suitability of the MISPE method for the selective extraction of a group of structurally related compounds such as acidic pharmaceuticals. Copyright © 2012 Elsevier B.V. All rights reserved.

Duplication and concerted evolution of MiSp-encoding genes underlie the material properties of minor ampullate silks of cobweb weaving spiders.

PubMed

Vienneau-Hathaway, Jannelle M; Brassfield, Elizabeth R; Lane, Amanda Kelly; Collin, Matthew A; Correa-Garhwal, Sandra M; Clarke, Thomas H; Schwager, Evelyn E; Garb, Jessica E; Hayashi, Cheryl Y; Ayoub, Nadia A

2017-03-14

Orb-web weaving spiders and their relatives use multiple types of task-specific silks. The majority of spider silk studies have focused on the ultra-tough dragline silk synthesized in major ampullate glands, but other silk types have impressive material properties. For instance, minor ampullate silks of orb-web weaving spiders are as tough as draglines, due to their higher extensibility despite lower strength. Differences in material properties between silk types result from differences in their component proteins, particularly members of the spidroin (spider fibroin) gene family. However, the extent to which variation in material properties within a single silk type can be explained by variation in spidroin sequences is unknown. Here, we compare the minor ampullate spidroins (MiSp) of orb-weavers and cobweb weavers. Orb-web weavers use minor ampullate silk to form the auxiliary spiral of the orb-web while cobweb weavers use it to wrap prey, suggesting that selection pressures on minor ampullate spidroins (MiSp) may differ between the two groups. We report complete or nearly complete MiSp sequences from five cobweb weaving spider species and measure material properties of minor ampullate silks in a subset of these species. We also compare MiSp sequences and silk properties of our cobweb weavers to published data for orb-web weavers. We demonstrate that all our cobweb weavers possess multiple MiSp loci and that one locus is more highly expressed in at least two species. We also find that the proportion of β-spiral-forming amino acid motifs in MiSp positively correlates with minor ampullate silk extensibility across orb-web and cobweb weavers. MiSp sequences vary dramatically within and among spider species, and have likely been subject to multiple rounds of gene duplication and concerted evolution, which have contributed to the diverse material properties of minor ampullate silks. Our sequences also provide templates for recombinant silk proteins with tailored properties.

Preparation and characterization of molecularly imprinted polymer for di(2-ethylhexyl) phthalate: application to sample clean-up prior to gas chromatographic determination.

PubMed

Shaikh, Huma; Memon, Najma; Khan, Hamayun; Bhanger, M I; Nizamani, S M

2012-07-20

The molecularly imprinted polymer (MIP) selective for di(2-ethylhexyl) phthalate (DEHP) an environmental endocrine disruptor was prepared by suspension polymerization using methacrylamide as functional monomer and N,N'-methylene-bis-acrylamide as cross-linker. The imprinted polymer was employed for solid-phase extraction of DEHP from water samples of environmental importance and characterized by FT-IR and SEM. The adsorption properties of the imprinted polymer were demonstrated by equilibrium rebinding experiments, Pseudo-second-order kinetic model, Sips isotherm and Scatchard analysis. The reusability of MIP was checked for at least six repeated batch adsorption cycles and the results showed almost no deterioration in the adsorption capacity. The competitive recognition studies were performed with DEHP and structurally similar compounds; dimethyl phthalate (DMP), diethyl phthalate (DEP), and dibutyl phthalate (DBP). The imprinting factor (IF) of DEHP was found to be 12.86 which was much higher than the imprinting factors (IF) of other phthalates. A method constituted by molecularly imprinted solid-phase extraction (MISPE) with GC-FID was developed for DEHP analysis in water samples under very simple conditions. Sample loading and desorption conditions were also optimized. The MISPE method's linearity ranged from 0.035 to 3.0 μg ml⁻¹ with r² = 0.9998. Intra-assay, interassay precision and accuracy ranged from 0.0168% to 1.017%, 1.130% to 4.799% and 94.98% to 99.35%, respectively. The LOD and LOQ were found to be 0.011 and 0.035 μg ml⁻¹, respectively. Synthesized MIP was employed in MISPE for cleaning up the spiked river water samples prior to gas chromatographic analysis. The river samples were found to contain DEHP in the range of 1.4 × 10⁻³ to 0.349 μg ml⁻¹. Copyright © 2012 Elsevier B.V. All rights reserved.

Preparation of molecular imprinted polymers using bi-functional monomer and bi-crosslinker for solid-phase extraction of rutin.

PubMed

Zeng, Huan; Wang, Yuzhi; Liu, Xiaojie; Kong, Jinhuan; Nie, Chan

2012-05-15

Molecular imprinted polymers (MIPs) were prepared using rutin as the template, different reagents as the functional monomer and different reagents as the cross-linker by solution polymerization. Several parameters that would influence the performance of MIPs were investigated including the type of functional monomer (single or double) and cross-linker (single or double), and the molar ratio of the template, the functional monomer and the cross-linker. The optimum synthesis conditions of MIPs were found to be bi-monomers (acrylamide-co-2-vinyl pyridine, 3:1) and bi-crosslinker (ethylene glycol dimethacrylate-co-divinylbenzene, 3:1). The ratio of the template, the functional monomer and the cross-linker was found to be 1:6:20. MIPs synthesized under these conditions were filled into the cartridges as the adsorbents of solid-phase extraction (SPE). A competition test was conducted to authenticate the selectivity and the specificity of molecularly imprinted solid-phase extraction (MISPE) for rutin using the mixture solution of standard rutin and its structural analogs including quercetin, naringenin and kaempferol. Compared with purchased SPE including C(18), silica and PCX, MISPE showed better selectivity and enrichment property for rutin in the extracted solutions of Chinese medicinal plants than any others. The mean recoveries were 85.93% (RSD: 3.04%, n=3) for Saururus chinensis (Lour.) Bail and 88.61% (RSD: 3.36%, n=3) for Flos Sophorae, respectively, which indicated that the optimized rutin-MIPs possess the value of practical application. Copyright © 2012 Elsevier B.V. All rights reserved.

Reproductive health services for Syrian refugees in Zaatri Camp and Irbid City, Hashemite Kingdom of Jordan: an evaluation of the Minimum Initial Services Package.

PubMed

Krause, Sandra; Williams, Holly; Onyango, Monica A; Sami, Samira; Doedens, Wilma; Giga, Noreen; Stone, Erin; Tomczyk, Barbara

2015-01-01

The Minimum Initial Services Package (MISP) for reproductive health, a standard of care in humanitarian emergencies, is a coordinated set of priority activities developed to prevent excess morbidity and mortality, particularly among women and girls, which should be implemented at the onset of an emergency. The purpose of the evaluation was to determine the status of MISP implementation for Syrian refugees in Jordan as part of a global evaluation of reproductive health in crises. In March 2013, applying a formative evaluation approach 11 key informant interviews, 13 health facility assessments, and focus group discussions (14 groups; 159 participants) were conducted in two Syrian refugee sites in Jordan, Zaatri Camp, and Irbid City, respectively. Information was coded, themes were identified, and relationships between data explored. Lead health agencies addressed the MISP by securing funding and supplies and establishing reproductive health focal points, services and coordination mechanisms. However, Irbid City was less likely to be included in coordination activities and health facilities reported challenges in human resource capacity. Access to clinical management of rape survivors was limited, and both women and service provider's knowledge about availability of these services was low. Activities to reduce the transmission of HIV and to prevent excess maternal and newborn morbidity and mortality were available, although some interventions needed strengthening. Some planning for comprehensive reproductive health services, including health indicator collection, was delayed. Contraceptives were available to meet demand. Syndromic treatment of sexually transmitted infections and antiretrovirals for continuing users were not available. In general refugee women and adolescent girls perceived clinical services negatively and complained about the lack of basic necessities. MISP services and key elements to support implementation were largely in place. Pre-existing Jordanian health infrastructure, prior MISP trainings, dedicated leadership and available funding and supplies facilitated MISP implementation. The lack of a national protocol on clinical management of rape survivors hindered provision of these services, while communities' lack of information about the health benefits of the services as well as perceived cultural repercussions likely contributed to no recent service uptake from survivors. This information can inform MISP programming in this setting.

Reproductive health services for Syrian refugees in Zaatri Camp and Irbid City, Hashemite Kingdom of Jordan: an evaluation of the Minimum Initial Services Package

PubMed Central

2015-01-01

Background The Minimum Initial Services Package (MISP) for reproductive health, a standard of care in humanitarian emergencies, is a coordinated set of priority activities developed to prevent excess morbidity and mortality, particularly among women and girls, which should be implemented at the onset of an emergency. The purpose of the evaluation was to determine the status of MISP implementation for Syrian refugees in Jordan as part of a global evaluation of reproductive health in crises. Methods In March 2013, applying a formative evaluation approach 11 key informant interviews, 13 health facility assessments, and focus group discussions (14 groups; 159 participants) were conducted in two Syrian refugee sites in Jordan, Zaatri Camp, and Irbid City, respectively. Information was coded, themes were identified, and relationships between data explored. Results Lead health agencies addressed the MISP by securing funding and supplies and establishing reproductive health focal points, services and coordination mechanisms. However, Irbid City was less likely to be included in coordination activities and health facilities reported challenges in human resource capacity. Access to clinical management of rape survivors was limited, and both women and service provider’s knowledge about availability of these services was low. Activities to reduce the transmission of HIV and to prevent excess maternal and newborn morbidity and mortality were available, although some interventions needed strengthening. Some planning for comprehensive reproductive health services, including health indicator collection, was delayed. Contraceptives were available to meet demand. Syndromic treatment of sexually transmitted infections and antiretrovirals for continuing users were not available. In general refugee women and adolescent girls perceived clinical services negatively and complained about the lack of basic necessities. Conclusions MISP services and key elements to support implementation were largely in place. Pre-existing Jordanian health infrastructure, prior MISP trainings, dedicated leadership and available funding and supplies facilitated MISP implementation. The lack of a national protocol on clinical management of rape survivors hindered provision of these services, while communities’ lack of information about the health benefits of the services as well as perceived cultural repercussions likely contributed to no recent service uptake from survivors. This information can inform MISP programming in this setting. PMID:25798190

Determination of zearalenone and its metabolites in endometrial cancer by coupled separation techniques.

PubMed

Gadzała-Kopciuch, Renata; Cendrowski, Krzysztof; Cesarz, Anna; Kiełbasa, Paweł; Buszewski, Bogusław

2011-10-01

This study presents a selective method of isolation of zearalenone (ZON) and its metabolite, α-zearalenol (α-ZOL), in neoplastically changed human tissue by accelerated solvent and ultrasonic extractions using a mixture of acetonitrile/water (84/16% v/v) as the extraction solvent. Extraction effectiveness was determined through the selection of parameters (composition of the solvent mixture, temperature, pressure, number of cycles) with tissue contamination at the level of nanograms per gram. The produced acetonitrile/water extracts were purified, and analytes were enriched in columns packed with homemade molecularly imprinted polymers. Purified extracts were determined by liquid chromatography (LC) coupled with different detection systems (diode array detection--DAD and mass spectrometry--MS) involving the Ascentis RP-Amide as a stationary phase and gradient elution. The combination of UE-MISPE-LC (ultrasonic extraction--molecularly imprinted solid-phase extraction--liquid chromatography) produced high (R≈95-98%) and repeatable (RSD<3%) recovery values for ZON and α-ZOL. © The Author(s) 2011. This article is published with open access at Springerlink.com

Development of magnetic molecularly imprinted polymers with double templates for the rapid and selective determination of amphenicol antibiotics in water, blood, and egg samples.

PubMed

Wei, Shoulian; Li, Jianwen; Liu, Yong; Ma, Jinkui

2016-11-18

A magnetic mesoporous dual-template molecularly imprinted polymer (Fe 3 O 4 @mSiO 2 @DMIP) with a specific recognition capability for chloramphenicol (CAP) and florfenicol (FF) was synthesised. CAP and FF were used as dual-template molecules, α-methacrylic acid and Fe 3 O 4 @mSiO 2 @-CHCH 2 as dual functional monomers, and ethylene glycol dimethyl methacrylate as a crosslinking agent. For comparison, a magnetic mesoporous non-molecularly imprinted polymer (Fe 3 O 4 @mSiO 2 @NIP) was also prepared using the same synthesis procedure, but without the dual templates. The prepared polymers were characterised using scanning electron microscopy, Fourier-transform infrared spectroscopy and adsorption experiments. Results indicated that both the Fe 3 O 4 @mSiO 2 @DMIP and the Fe 3 O 4 @mSiO 2 @NIP were microspherical nanoparticles, and the surface of the Fe 3 O 4 @mSiO 2 @DMIP was rougher than that of the Fe 3 O 4 @mSiO 2 @NIP. In addition, the prepared Fe 3 O 4 @mSiO 2 @DMIP possessed a higher adsorption capacity and better selectivity for CAP and FF than the Fe 3 O 4 @mSiO 2 @NIP. The maximum static adsorption capacities of the Fe 3 O 4 @mSiO 2 @ DMIP for CAP and FF were 146.5 and 190.1mgg -1 , respectively, whereas those of the Fe 3 O 4 @mSiO 2 @NIP were 50.0 and 44.0mgg -1 , respectively. The obtained Fe 3 O 4 @mSiO 2 @DMIP particles were applied as a magnetic solid-phase extraction sorbent for the rapid and selective extraction of CAP, FF, and thiamphenicol (TAP) in water, chicken blood and egg samples. The method of magnetic molecularly imprinted solid-phase extraction (M-MISPE) coupled to high-performance liquid chromatography with UV detection (HPLC-UV) was conducted to detect CAP, FF, and TAP. The limits of detection for CAP, FF, and TAP were 0.16, 0.08, and 0.08μgkg -1 , respectively. The average recovery and precision values for the spiked water, chicken blood, and egg samples ranged from 88.3% to 99.1% and 2.7% to 7.9%, respectively. Given its rapidity, selectivity, and sensitivity, the developed method of M-MISPE coupled to HPLC-UV detection has good application prospects in environmental, biological, and food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Exploiting automatic on-line renewable molecularly imprinted solid-phase extraction in lab-on-valve format as front end to liquid chromatography: application to the determination of riboflavin in foodstuffs.

PubMed

Oliveira, Hugo M; Segundo, Marcela A; Lima, José L F C; Miró, Manuel; Cerdà, Victor

2010-05-01

In the present work, it is proposed, for the first time, an on-line automatic renewable molecularly imprinted solid-phase extraction (MISPE) protocol for sample preparation prior to liquid chromatographic analysis. The automatic microscale procedure was based on the bead injection (BI) concept under the lab-on-valve (LOV) format, using a multisyringe burette as propulsion unit for handling solutions and suspensions. A high precision on handling the suspensions containing irregularly shaped molecularly imprinted polymer (MIP) particles was attained, enabling the use of commercial MIP as renewable sorbent. The features of the proposed BI-LOV manifold also allowed a strict control of the different steps within the extraction protocol, which are essential for promoting selective interactions in the cavities of the MIP. By using this on-line method, it was possible to extract and quantify riboflavin from different foodstuff samples in the range between 0.450 and 5.00 mg L(-1) after processing 1,000 microL of sample (infant milk, pig liver extract, and energy drink) without any prior treatment. For milk samples, LOD and LOQ values were 0.05 and 0.17 mg L(-1), respectively. The method was successfully applied to the analysis of two certified reference materials (NIST 1846 and BCR 487) with high precision (RSD < 5.5%). Considering the downscale and simplification of the sample preparation protocol and the simultaneous performance of extraction and chromatographic assays, a cost-effective and enhanced throughput (six determinations per hour) methodology for determination of riboflavin in foodstuff samples is deployed here.

Computational and experimental investigation of molecular imprinted polymers for selective extraction of dimethoate and its metabolite omethoate from olive oil.

PubMed

Bakas, Idriss; Oujji, Najwa Ben; Moczko, Ewa; Istamboulie, Georges; Piletsky, Sergey; Piletska, Elena; Ait-Addi, Elhabib; Ait-Ichou, Ihya; Noguer, Thierry; Rouillon, Régis

2013-01-25

This work presents the development of molecularly imprinted polymers (MIPs) for the selective extraction of dimethoate from olive oil. Computational simulations allowed selecting itaconic acid as the monomer showing the highest affinity towards dimethoate. Experimental validation confirmed modelling predictions and showed that the polymer based on IA as functional monomer and omethoate as template molecule displays the highest selectivity for the structurally similar pesticides dimethoate, omethoate and monocrotophos. Molecularly imprinted solid phase extraction (MISPE) method was developed and applied to the clean-up of olive oil extracts. It was found that the most suitable solvents for loading, washing and elution step were respectively hexane, hexane-dichloromethane (85:15%) and methanol. The developed MIPSE was successfully applied to extraction of dimethoate from olive oil, with recovery rates up to 94%. The limits of detection and quantification of the described method were respectively 0.012 and 0.05 μg g(-1). Copyright © 2012 Elsevier B.V. All rights reserved.

Automated Protein Biomarker Analysis: on-line extraction of clinical samples by Molecularly Imprinted Polymers

NASA Astrophysics Data System (ADS)

Rossetti, Cecilia; Świtnicka-Plak, Magdalena A.; Grønhaug Halvorsen, Trine; Cormack, Peter A. G.; Sellergren, Börje; Reubsaet, Léon

2017-03-01

Robust biomarker quantification is essential for the accurate diagnosis of diseases and is of great value in cancer management. In this paper, an innovative diagnostic platform is presented which provides automated molecularly imprinted solid-phase extraction (MISPE) followed by liquid chromatography-mass spectrometry (LC-MS) for biomarker determination using ProGastrin Releasing Peptide (ProGRP), a highly sensitive biomarker for Small Cell Lung Cancer, as a model. Molecularly imprinted polymer microspheres were synthesized by precipitation polymerization and analytical optimization of the most promising material led to the development of an automated quantification method for ProGRP. The method enabled analysis of patient serum samples with elevated ProGRP levels. Particularly low sample volumes were permitted using the automated extraction within a method which was time-efficient, thereby demonstrating the potential of such a strategy in a clinical setting.

Molecularly imprinted polymer for determination of lumefantrine in human plasma through chemometric-assisted solid-phase extraction and liquid chromatography.

PubMed

da Silva, Pedro Henrique Reis; Diniz, Melina Luiza Vieira; Pianetti, Gerson Antônio; da Costa César, Isabela; Ribeiro E Silva, Maria Elisa Scarpelli; de Souza Freitas, Roberto Fernando; de Sousa, Ricardo Geraldo; Fernandes, Christian

2018-07-01

Lumefantrine is the first-choice treatment of Falciparum uncomplicated malaria. Recent findings of resistance to lumefantrine has brought attention for the importance of therapeutic monitoring, since exposure to subtherapeutic doses of antimalarials after administration is a major cause of selection of resistant parasites. Therefore, this study focused on the development of innovative, selective, less expensive and stable molecularly imprinted polymers (MIPs) for solid-phase extraction (SPE) of lumefantrine from human plasma to be used in drug monitoring. Polymers were synthesized by precipitation polymerization and chemometric tools (Box-Behnken design and surface response methodology) were employed for rational optimization of synthetic parameters. Optimum conditions were achieved with 2-vinylpyridine as monomer, ethylene glycol dimethacrylate as crosslinker and toluene as porogen, at molar ratio of 1:6:30 of template/monomer/crosslinker and azo-bisisobutyronitrile as initiator at 65 °C. The MIP obtained was characterized and exhibited high thermal stability, adequate surface morphology and porosity characteristics and high binding properties, with high affinity (adsorption capacity of 977.83 μg g -1 ) and selectivity (imprinting factor of 2.44; and selectivity factor of 1.48 and selectivity constant of 1.44 compared with halofantrine). Doehlert matrix and fractional designs were satisfactorily used for development and optimization of a MISPE-HPLC-UV method for determination of lumefantrine. The method fulfilled all validation parameters, with recoveries ranging from 83.68% to 85.42%, and was applied for quantitation of the drug in plasma from two healthy volunteers, with results of 1407.89 and 1271.35 ng mL -1 , respectively. Therefore, the MISPE-HPLC-UV method optimized through chemometrics provided a rapid, highly selective, less expensive and reproducible approach for lumefantrine drug monitoring. Copyright © 2018 Elsevier B.V. All rights reserved.

Perioperative Outcomes of Robotic and Laparoscopic Simple Prostatectomy: A European-American Multi-institutional Analysis.

PubMed

Autorino, Riccardo; Zargar, Homayoun; Mariano, Mirandolino B; Sanchez-Salas, Rafael; Sotelo, René J; Chlosta, Piotr L; Castillo, Octavio; Matei, Deliu V; Celia, Antonio; Koc, Gokhan; Vora, Anup; Aron, Monish; Parsons, J Kellogg; Pini, Giovannalberto; Jensen, James C; Sutherland, Douglas; Cathelineau, Xavier; Nuñez Bragayrac, Luciano A; Varkarakis, Ioannis M; Amparore, Daniele; Ferro, Matteo; Gallo, Gaetano; Volpe, Alessandro; Vuruskan, Hakan; Bandi, Gaurav; Hwang, Jonathan; Nething, Josh; Muruve, Nic; Chopra, Sameer; Patel, Nishant D; Derweesh, Ithaar; Champ Weeks, David; Spier, Ryan; Kowalczyk, Keith; Lynch, John; Harbin, Andrew; Verghese, Mohan; Samavedi, Srinivas; Molina, Wilson R; Dias, Emanuel; Ahallal, Youness; Laydner, Humberto; Cherullo, Edward; De Cobelli, Ottavio; Thiel, David D; Lagerkvist, Mikael; Haber, Georges-Pascal; Kaouk, Jihad; Kim, Fernando J; Lima, Estevao; Patel, Vipul; White, Wesley; Mottrie, Alexander; Porpiglia, Francesco

2015-07-01

Laparoscopic and robotic simple prostatectomy (SP) have been introduced with the aim of reducing the morbidity of the standard open technique. To report a large multi-institutional series of minimally invasive SP (MISP). Consecutive cases of MISP done for the treatment of bladder outlet obstruction (BOO) due to benign prostatic enlargement (BPE) between 2000 and 2014 at 23 participating institutions in the Americas and Europe were included in this retrospective analysis. Laparoscopic or robotic SP. Demographic data and main perioperative outcomes were gathered and analyzed. A multivariable analysis was conducted to identify factors associated with a favorable trifecta outcome, arbitrarily defined as a combination of the following postoperative events: International Prostate Symptom Score <8, maximum flow rate >15ml/s, and no perioperative complications. Overall, 1330 consecutive cases were analyzed, including 487 robotic (36.6%) and 843 laparoscopic (63.4%) SP cases. Median overall prostate volume was 100ml (range: 89-128). Median estimated blood loss was 200ml (range: 150-300). An intraoperative transfusion was required in 3.5% of cases, an intraoperative complication was recorded in 2.2% of cases, and the conversion rate was 3%. Median length of stay was 4 d (range: 3-5). On pathology, prostate cancer was found in 4% of cases. Overall postoperative complication rate was 10.6%, mostly of low grade. At a median follow-up of 12 mo, a significant improvement was observed for subjective and objective indicators of BOO. Trifecta outcome was not significantly influenced by the type of procedure (robotic vs laparoscopic; p=0.136; odds ratio [OR]: 1.6; 95% confidence interval [CI], 0.8-2.9), whereas operative time (p=0.01; OR: 0.9; 95% CI, 0.9-1.0) and estimated blood loss (p=0.03; OR: 0.9; 95% CI, 0.9-1.0) were the only two significant factors. Retrospective study design, lack of a control arm, and limited follow-up represent major limitations of the present analysis. This study provides the largest outcome analysis reported for MISP for BOO/BPE. These findings confirm that SP can be safely and effectively performed in a minimally invasive fashion in a variety of healthcare settings in which specific surgical expertise and technology is available. MISP can be considered a viable surgical treatment in cases of large prostatic adenomas. The use of robotic technology for this indication can be considered in centers that have a robotic program in place for other urologic indications. Analysis of a large data set from multiple institutions shows that surgical removal of symptomatic large prostatic adenomas can be carried out with good outcomes by using robot-assisted laparoscopy. Copyright © 2014 European Association of Urology. Published by Elsevier B.V. All rights reserved.

Three-dimensional ionic liquid functionalized magnetic graphene oxide nanocomposite for the magnetic dispersive solid phase extraction of 16 polycyclic aromatic hydrocarbons in vegetable oils.

PubMed

Zhang, Yun; Zhou, Hua; Zhang, Zhe-Hua; Wu, Xiang-Lun; Chen, Wei-Guo; Zhu, Yan; Fang, Chun-Fu; Zhao, Yong-Gang

2017-03-17

In this paper, a novel three-dimensional ionic liquid functionalized magnetic graphene oxide nanocomposite (3D-IL@mGO) was prepared, and used as an effective adsorbent for the magnetic dispersive solid phase extraction (MSPE) of 16 polycyclic aromatic hydrocarbons (PAHs) in vegetable oil prior to gas chromatography-mass spectrometry (GC-MS). The properties of 3D-IL@mGO were characterized by scanning electron micrographs (SEM), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometer (VSM). The 3D-IL@mGO, functionalized by ionic liquid, exhibited high adsorption toward PAHs. Compared to molecularly imprinted solid phase extraction (MISPE), the MSPE method based on 3D-IL@mGO had less solvent consumption and low cost, and was more efficent to light PAHs in quantitative analysis. Furthermore, the rapid and accurate GC-MS method coupled with 3D-IL@mGO MSPE procedure was successfully applied for the analysis of 16 PAHs in eleven vegetable oil samples from supermarket in Zhejiang Province. The results showed that the concentrations of BaP in 3 out of 11 samples were higher than the legal limit (2.0μg/kg, Commission Regulation 835/2011a), the sum of 8 heavy PAHs (BaA, CHR, BbF, BkF, BaP, IcP, DaA, BgP) in 11 samples was between 3.03μg/kg and 229.5μg/kg. Validation results on linearity, specificity, accuracy, precision and stability, as well as on application to the analysis of PAHs in oil samples demonstrated the applicability to food safety risk monitoring in China. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of a Central Avascular Triangle within the Obturator Foramen: A Radioanatomic Study

PubMed Central

Nyangoh Timoh, Krystel; Bader, Georges; Fauconnier, Arnaud; Barrau, Vincent; Delmas, Vincent; Touboul, Cyril

2015-01-01

Purpose To map the vascular anatomy of the obturator foramen using fixed anatomic landmarks. Method Twenty obturator regions were dissected in 10 fresh female cadavers after vascular blue dye injection in five cadavers (50%). Furthermore, 104 obturator regions were reconstructed by angiotomodensitometry from 52 women under investigation for suspected arterial disease. The anatomy of the obturator region was mapped by measuring the distance of vascular structures from the middle of the two branches of the ischiopubic bone, which were used as fixed landmarks. Results The bifurcation of the obturator artery was at a mean (SD) distance of 30.0 mm (4.5) from the middle of the ischiopubic branch (MISP). The anterior branch of the obturator vessels was 15.2 mm (10.1) from the MISP. The posterior branch of the obturator vessels was 5.5 mm (4.0) and 23.6 mm (8.7) from the middle of the outer edge of the obturator foramen (MOE) and the MISP, respectively. Using 5° and 95° percentiles of these measurements we defined a central avascular triangle. Conclusions Our data show that, beyond inter-individual variations, a central triangular avascular area can be identified in the obturator foramen between the posterior and anterior obturator artery using fixed landmarks. PMID:26624993

Molecularly imprinted polymers as the extracted sorbents of clenbuterol ahead of liquid chromatographic determination*

PubMed Central

Lay, Sovichea; Yu, Hai-ning; Hu, Bao-xiang; Shen, Sheng-rong

2016-01-01

A pre-treatment methodology for clenbuterol hydrochloride (CLEN) isolation and enrichment in a complex matrix environment was developed through exploiting molecularly imprinted polymers (MIPs). CLEN-imprinted polymers were synthesized by the combined use of ally-β-cyclodextrin (ally-β-CD) and methacrylic acid (MAA), allyl-β-CD and acrylonitrile (AN), and allyl-β-CD and methyl methacrylate (MMA) as the binary functional monomers. MAA-linked allyl-β-CD MIPs (M-MAA) were characterized by Fourier transform-infrared (FT-IR) spectroscopy and a scanning electron microscope (SEM). Based upon the results, M-MAA polymers generally proved to be an excellent selective extraction compared to its references: AN-linked allyl-β-CD MIPs (M-AN) and MMA-linked allyl-β-CD MIPs (M-MMA). M-MAA polymers were eventually chosen to run through a molecularly imprinted solid-phase extraction (MISPE) micro-column to enrich CLEN residues spiked in pig livers. A high recovery was achieved, ranging from 91.03% to 96.76% with relative standard deviation (RSD) ≤4.45%. PMID:27256680

Molecularly imprinted solid-phase extraction coupled to liquid chromatography for determination of Sudan dyes in preserved beancurds.

PubMed

Yan, Hongyuan; Qiao, Jindong; Pei, Yuning; Long, Tao; Ding, Wen; Xie, Kun

2012-05-01

New molecularly imprinted microspheres synthesized by suspension polymerisation using phenylamine and naphthol as mimic template were successfully applied as selective sorbents for the solid-phase extraction used for the simultaneous determination of four Sudan dyes from preserved beancurd products. The obtained imprinted microspheres showed good recognition and selectivity to the four Sudan dyes in aqueous solution and the affinity could be easily controlled by adjusting the property of the solution. Under the selected experimental condition, the recoveries of the Sudan dyes in preserved beancurds at three spiked levels were ranged between 90.2-104.5% with the relative standard deviation of less than 6.8%. The limit of detection (LOD) and limit of quantification (LOQ) based on a signal-to-noise of 3 and 10 were in the range of 0.005-0.009μgg(-1) and 0.015-0.030μgg(-1), respectively. Comparing with alumina and C18-based extraction, the selectivity and repeatability of molecularly imprinted solid-phase extraction (MISPE) were obviously improved. This method could be potentially applied for the determination of Sudan dyes in complicated food samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

Molecularly imprinted polymer/cryogel composites for solid-phase extraction of bisphenol A from river water and wine.

PubMed

Baggiani, Claudio; Baravalle, Patrizia; Giovannoli, Cristina; Anfossi, Laura; Giraudi, Gianfranco

2010-05-01

Superporous monolithic hydrogels (cryogel monoliths) are elastic, sponge-like materials that can be prepared in an aqueous medium through a cryotropic gelation technique. These monoliths show interesting properties for the development of high-throughput solid-phase extraction supports to treat large volumes of aqueous samples. In this work, a cryogel-supported molecularly imprinted solid-phase extraction approach for the endocrine disruptor bisphenol A (BPA) from river water and wine samples is presented. An imprinted polymer with molecular recognition properties for BPA was prepared in acetonitrile by thermal polymerization of a mixture of 4,4'-dihydroxy-2,2-diphenyl-1,1,1,3,3,3-trifluoropropane as a mimic template of BPA, 4-vinylpyridine and trimethylolpropane trimethacrylate in a molar ratio of 1 + 6 + 6. Fine imprinted particles (<10 microm) were embedded in a poly-acrylamide-co-N,N'-methylenbisacrylamide cryogel obtained by ammonium persulfate-induced cryopolymerization at -18 degrees C. The resulting monolithic gel was evaluated for its use as a sorbent support in an off-line solid-phase extraction approach to recover BPA from dilute aqueous samples with minimum pre-loading work-up. The optimized extraction protocol resulted in a reliable MISPE method suitable to selectively extract and preconcentrate BPA from river water and red wine samples, demonstrating the practical feasibility of cryogel-trapped imprinted polymers as solid-phase extraction materials.

Molecular imprinting solid phase extraction for selective detection of methidathion in olive oil.

PubMed

Bakas, Idriss; Oujji, Najwa Ben; Moczko, Ewa; Istamboulie, Georges; Piletsky, Sergey; Piletska, Elena; Ait-Ichou, Ihya; Ait-Addi, Elhabib; Noguer, Thierry; Rouillon, Régis

2012-07-13

A specific adsorbent for extraction of methidathion from olive oil was developed. The design of the molecularly imprinted polymer (MIP) was based on the results of the computational screening of the library of polymerisable functional monomers. MIP was prepared by thermal polymerisation using N,N'-methylene bisacrylamide (MBAA) as a functional monomer and ethylene glycol dimethacrylate (EGDMA) as a cross-linker. The polymers based on the itaconic acid (IA), methacrylic acid (MAA) and 2-(trifluoromethyl)acryl acid (TFMAA) functional monomers and one control polymer which was made without functional monomers with cross-linker EGDMA were also synthesised and tested. The performance of each polymer was compared using corresponding imprinting factor. As it was predicted by molecular modelling the best results were obtained for the MIP prepared with MBAA. The obtained MIP was optimised in solid-phase extraction coupled with high performance liquid chromatography (MISPE-HPLC-UV) and tested for the rapid screening of methidathion in olive oil. The proposed method allowed the efficient extraction of methidathion for concentrations ranging from 0.1 to 9 mg L(-1) (r(2)=0.996). The limits of detection (LOD) and quantification (LOQ) in olive oil were 0.02 mg L(-1) and 0.1 mg L(-1), respectively. MIPs extraction was much more effective than traditional C18 reverse-phase solid phase extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

Development of magnetic molecularly imprinted polymers for selective extraction: determination of citrinin in rice samples by liquid chromatography with UV diode array detection.

PubMed

Urraca, Javier L; Huertas-Pérez, José F; Cazorla, Guillermo Aragoneses; Gracia-Mora, Jesus; García-Campaña, Ana M; Moreno-Bondi, María Cruz

2016-04-01

In this work, we report the synthesis of novel magnetic molecularly imprinted polymers (m-MIPs) and their application to the selective extraction of the mycotoxin citrinin (CIT) from food samples. The polymers were prepared by surface imprinting of Fe3O4 nanoparticles, using 2-naphtholic acid (2-NA) as template molecule, N-3,5-bis(trifluoromethyl)phenyl-N'-4-vinylphenyl urea and methacrylamide as functional monomers and ethyleneglycol dimethacrylate as cross-linker. The resulting material was characterized by transmission electron microscopy (TEM), and X-ray diffraction (XRD) and Fourier transform infrared spectroscopies (FT-IR). The polymers were used to develop a solid-phase extraction method (m-MISPE) for the selective recovery of CIT from rice extracts prior to its determination by HPLC with UV diode array detection. The method involves ultrasound-assisted extraction of the mycotoxin from rice samples with (7:3, v/v) methanol/water, followed by sample cleanup and preconcentration with m-MIP. The extraction (washing and elution) conditions were optimized and their optimal values found to provide CIT recoveries of 94-98 % with relative standard deviations (RSD) less than 3.4 % (n = 3) for preconcentrated sample extracts (5 mL) fortified with the analyte at concentrations over the range 25-100 μg kg(-1). Based on the results, the application of the m-MIPs facilitates the accurate and efficient determination of CIT in rice extracts.

Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of dextromethorphan in human plasma samples.

PubMed

Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-Adergani, Behrouz

2011-04-01

In this paper, a novel method is described for automated determination of dextromethorphan in biological fluids using molecularly imprinted solid-phase extraction (MISPE) as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and dextromethorphan as template molecule. These imprinted polymers were used as solid-phase extraction sorbent for the extraction of dextromethorphan from human plasma samples. Various parameters affecting the extraction efficiency of the MIP cartridges were evaluated. The high selectivity of the sorbent coupled to the high performance liquid chromatographic system permitted a simple and rapid analysis of this drug in plasma samples with limits of detection (LOD) and quantification (LOQ) of 0.12 ng/mL and 0.35 ng/mL, respectively. The MIP selectivity was evaluated by analyzing of the dextromethorphan in presence of several substances with similar molecular structures and properties. Results from the HPLC analyses showed that the recoveries of dextromethorphan using MIP cartridges from human plasma samples in the range of 1-50 ng/mL were higher than 87%. Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of Ten Macrolide Drugs in Environmental Water Using Molecularly Imprinted Solid-Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Song, Xuqin; Zhou, Tong; Li, Jiufeng; Zhang, Meiyu; Xie, Jingmeng; He, Limin

2018-05-14

With the extensive application of antibiotics in livestock, their contamination of the aquatic environment has received more attention. Molecularly imprinted polymer (MIP), as an eco-friendly and durable solid-phase extraction material, has shown great potential for the separation and enrichment of antibiotics in water. This study aims at developing a practical and economical method based on molecularly imprinted solid phase extraction (MISPE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for simultaneously detecting ten macrolide drugs in different sources of water samples. The MIP was synthesized by bulk polymerization using tylosin as the template and methacrylic acid as the functional monomer. The MIP exhibited a favorable load-bearing capacity for water (>90 mL), which is more than triple that of non-molecularly imprinted polymers (NIP). The mean recoveries of macrolides at four spiked concentration levels (limit of quantification, 40, 100, and 400 ng/L) were 62.6⁻100.9%, with intra-day and inter-day relative standard deviations below 12.6%. The limit of detection and limit of quantification were 1.0⁻15.0 ng/L and 3.0⁻40.0 ng/L, respectively. Finally, the proposed method was successfully applied to the analysis of real water samples.

Molecularly imprinted polymer coupled with dispersive liquid-liquid microextraction and injector port silylation: a novel approach for the determination of 3-phenoxybenzoic acid in complex biological samples using gas chromatography-tandem mass spectrometry.

PubMed

Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Jain, Rajeev; Dhuriya, Yogesh Kumar; Saxena, Prem Narain; Khanna, Vinay Kumar

2014-01-15

A novel analytical approach based on molecularly imprinted solid phase extraction (MISPE) coupled with dispersive liquid-liquid microextraction (DLLME), and injector port silylation (IPS) has been developed for the selective preconcentration, derivatization and analysis of 3-phenoxybenzoic acid (3-PBA) using gas chromatography-tandem mass spectrometry (GC-MS/MS) in complex biological samples such as rat blood and liver. Factors affecting the synthesis of MIP were evaluated and the best monomer and cross-linker were selected based on binding affinity studies. Various parameters of MISPE, DLLME and IPS were optimized for the selective preconcentration and derivatization of 3-PBA. The developed method offers a good linearity over the calibration range of 0.02-2.5ngmg(-1) and 7.5-2000ngmL(-1) for liver and blood respectively. Under optimized conditions, the recovery of 3-PBA in liver and blood samples were found to be in the range of 83-91%. The detection limit was found to be 0.0045ngmg(-1) and 1.82ngmL(-1) in liver and blood respectively. SRM transition of 271→227 and 271→197 has been selected as quantifier and qualifier transition for 3-PBA derivative. Intra and inter-day precision for five replicates in a day and for five, successive days was found to be less than 8%. The method developed was successfully applied to real samples, i.e. rat blood and tissue for quantitative evaluation of 3-PBA. The analytical approach developed is rapid, economic, simple, eco-friendly and possess immense utility for the analysis of analytes with polar functional groups in complex biological samples by GC-MS/MS. Copyright © 2013 Elsevier B.V. All rights reserved.

Molecularly imprinted solid-phase extraction for the selective determination of bromhexine in human serum and urine with high performance liquid chromatography.

PubMed

Javanbakht, Mehran; Namjumanesh, Mohammad Hadi; Akbari-Adergani, Behrouz

2009-11-15

In this work, a novel method is described for the determination of bromhexine in biological fluids using molecularly imprinted solid-phase extraction as the sample cleanup technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and bromhexine as the template molecule. The novel imprinted polymer was used as a solid-phase extraction sorbent for the extraction of bromhexine from human serum and urine. Various parameters affecting the extraction efficiency of the polymer have been evaluated. The optimal conditions for molecularly imprinted solid-phase extraction (MISPE) consisted of conditioning 1 mL methanol and 1 mL of deionized water at neutral pH, loading of 5 mL of the water sample (25 microg L(-1)) at pH 6.0, washing using 2 mL acetonitrile/acetone (1/4, v/v) and elution with 3x 1 mL methanol/acetic acid (10/1, v/v). The MIP selectivity was evaluated by checking several substances with similar molecular structures to that of bromhexine. Results from the HPLC analyses showed that the calibration curve of bromhexine using MIP from human serum and urine is linear in the ranges of 0.5-100 and 1.5-100 microg L(-1) with good precisions (3.3% and 2.8% for 5.0 microg L(-1)), respectively. The recoveries for serum and urine samples were higher than 92%.

The Minnesota Indian Scholarship Program (MISP), 1955-1979.

ERIC Educational Resources Information Center

1979

The Minnesota Indian Scholarship Program has grown tremendously since 1955 when three Indian students were given financial aid to attend college. This report provides a narrative and statistical history of the program and its activities with the state legislature, high school counselors, post secondary financial aids officers, tribal and…

Molecular imprinting-based separation methods for selective analysis of fluoroquinolones in soils.

PubMed

Turiel, Esther; Martín-Esteban, Antonio; Tadeo, José Luis

2007-11-23

Molecularly imprinted polymers (MIPs) for fluoroquinolone antibiotics (FQs) have been synthesised in one single preparative step by precipitation polymerisation using ciprofloxacin (CIP) as template. Combinations of methacrylic acid (MAA) or 4-vinylpyridine (VP) as functional monomers, ethylene glycol dimethacrylate as crosslinker and dichloromethane, methanol, acetonitrile or toluene as porogens were tested. The experiments carried out by molecularly imprinted solid-phase extraction (MISPE) in cartridges did not allow to detect any imprint effect in the VP-based polymers whereas it was clearly observed in the MAA-based polymers. Among them, the MIP prepared in methanol using MAA as monomer showed the best performance and was chosen for further experiments. The ability of the selected MIP for the selective recognition of other widely used FQs (enoxacin, norfloxacin, danofloxacin and enrofloxacin) and quinolones (Qs) (cinoxacin, flumequine, nalidixic acid and oxolinic acid) was evaluated. The obtained results revealed the high selectivity of the obtained polymer, which was able to distinguish between FQs, that were recognised and retained onto the MIP cartridge, and Qs, which were washed out during loading and washing steps. The MIP was then packed into a stainless steel column (50mmx4.6mm i.d.) and evaluated as chromatography column for screening of FQs in soil samples. The mobile phase composition, flow rate, and the elution profile were then optimised in order to improve peak shape without sacrifying imprinting factor. Finally, under optimised conditions, soil samples spiked with CIP or with a mixture of fluoroquinolones in concentration of 0.5microgg(-1) were successfully analysed by the developed MIP-based procedures.

Evaluation of the Massage in Schools Programme in One Primary School

ERIC Educational Resources Information Center

Marsh, Lesley J.

2011-01-01

This article discusses the potential benefits of the Massage in Schools Programme (MISP), a programme originating in Scandinavia, which has been introduced into schools in the United Kingdom (UK) since 2001. Meeting four out of five outcomes of the Every Child Matters agenda, the review of the literature aims to separate anecdotal and media…

Synthesis and application of selective adsorbent for pirimicarb pesticides in aqueous media using allyl-β-cyclodextrin based binary functional monomers.

PubMed

He, Chengzijing; Lay, Sovichea; Yu, Haining; Shen, Shengrong

2018-04-01

Binary functional monomers, allyl-β-cyclodextrin (allyl-β-CD) and methacrylic acid (MAA) or allyl-β-CD and acrylonitrile (AN), were exploited in a fabrication of molecularly imprinted polymers (MIPs) for selective recognition and large enrichment of pirimicarb from aqueous media. Special attention was paid to the computational simulation of the imprinting molecular and functional monomers. The morphological characteristics of MIPs made of allyl-β-CD and MAA (M-MAA) were characterised by scanning electron microscopy. The effect of binding capacity of MAA-linked allyl-β-CD MIPs (M-MAA) demonstrated higher efficiency than that of AN-linked allyl-β-CD MIPs (M-AN) when tested in binding specificity. Finally, M-MAA was chosen to run through molecularly imprinted solid-phase extraction (MISPE) to analyse the spiked fresh leafy vegetables of pirimicarb. The present proposed technique is a promising tool for the preparation of the receptors which could recognise pirimicarb pesticide in aqueous media. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

The 2018 Inter-agency field manual on reproductive health in humanitarian settings: revising the global standards.

PubMed

Foster, Angel M; Evans, Dabney P; Garcia, Melissa; Knaster, Sarah; Krause, Sandra; McGinn, Therese; Rich, Sarah; Shah, Meera; Tappis, Hannah; Wheeler, Erin

2017-11-01

Since the 1990s, the Inter-agency field manual on reproductive health in humanitarian settings (IAFM) has provided authoritative guidance on reproductive health service provision during different phases of complex humanitarian emergencies. In 2018, the Inter-Agency Working Group on Reproductive Health in Crises will release a new edition of this global resource. In this article, we describe the collaborative and inter-sectoral revision process and highlight major changes in the 2018 IAFM. Key revisions to the manual include repositioning unintended pregnancy prevention within and explicitly incorporating safe abortion care into the Minimum Initial Service Package (MISP) chapter, which outlines a set of priority activities to be implemented at the outset of a humanitarian crisis; stronger guidance on the transition from the MISP to comprehensive sexual and reproductive health services; and the addition of a logistics chapter. In addition, the IAFM now places greater and more consistent emphasis on human rights principles and obligations, gender-based violence, and the linkages between maternal and newborn health, and incorporates a diverse range of field examples. We conclude this article with an outline of plans for releasing the 2018 IAFM and facilitating uptake by those working in refugee, crisis, conflict, and emergency settings.

Matrix molecularly imprinted mesoporous sol-gel sorbent for efficient solid-phase extraction of chloramphenicol from milk.

PubMed

Samanidou, Victoria; Kehagia, Maria; Kabir, Abuzar; Furton, Kenneth G

2016-03-31

Highly selective and efficient chloramphenicol imprinted sol-gel silica based inorganic polymeric sorbent (sol-gel MIP) was synthesized via matrix imprinting approach for the extraction of chloramphenicol in milk. Chloramphenicol was used as the template molecule, 3-aminopropyltriethoxysilane (3-APTES) and triethoxyphenylsilane (TEPS) as the functional precursors, tetramethyl orthosilicate (TMOS) as the cross-linker, isopropanol as the solvent/porogen, and HCl as the sol-gel catalyst. Non-imprinted sol-gel polymer (sol-gel NIP) was synthesized under identical conditions in absence of template molecules for comparison purpose. Both synthesized materials were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and nitrogen adsorption porosimetry, which unambiguously confirmed their significant structural and morphological differences. The synthesized MIP and NIP materials were evaluated as sorbents for molecularly imprinted solid phase extraction (MISPE) of chloramphenicol in milk. The effect of critical extraction parameters (flow rate, elution solvent, sample and eluent volume, selectivity coefficient, retention capacity) was studied in terms of retention and desorption of chloramphenicol. Competition and cross reactivity tests have proved that sol-gel MIP sorbent possesses significantly higher specific retention and enrichment capacity for chloramphenicol compared to its non-imprinted analogue. The maximum imprinting factor (IF) was found as 9.7, whereas the highest adsorption capacity of chloramphenicol by sol-gel MIP was 23 mg/g. The sol-gel MIP was found to be adequately selective towards chloramphenicol to provide the necessary minimum required performance limit (MRPL) of 0.3 μg/kg set forth by European Commission after analysis by LC-MS even without requiring time consuming solvent evaporation and sample reconstitution step, often considered as an integral part in solid phase extraction work-flow. Intra and inter-assay RSD values were less than 13% and accuracy expressed as relative recovery ranged from 85 to 106%. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and application of molecularly imprinted nanoparticles combined ultrasonic assisted for highly selective solid phase extraction trace amount of celecoxib from human plasma samples using design expert (DXB) software.

PubMed

Arabi, Maryam; Ghaedi, Mehrorang; Ostovan, Abbas; Tashkhourian, Javad; Asadallahzadeh, Hamideh

2016-11-01

In this work molecular imprinted nanoparticles (MINPs) was synthesized and applied for ultrasonic assisted solid phase extraction of celecoxib (CEL) from human plasma sample following its combination by HPLC-UV. The MINPs were prepared in a non-covalent approach using methacrylic acid as monomer, CEL as template, ethylene glycol dimethacrylate as cross-linker, and 2,2-azobisisobutyronitrile (AIBN) as the initiator of polymerization. pH, volume of rinsing and eluent solvent and amount of sorbent influence on response were investigated using factorial experimental design, while optimum point was achieved and set as 250mg sorbent, pH 7.0, 1.5mL washing solvent and 2mL eluent by analysis of results according to design expert (DX) software. At above specified conditions, CEL in human plasma with complicated matrices with acceptable high recoveries (96%) and RSD% lower than 10% was quantified and estimated. The proposed MISPE-HPLC-UV method has linear responses among peak area and concentrations of CEL in the range of 0.2-2000μgL(-1), with regression coefficient of 0.98. The limit of detection (LOD) and quantification (LOQ) based on three and ten times of the noise of HPLC peaks correspond to blank solution were 0.08 and 0.18μgL(-1), respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of (monomer - crosslinker – initiator) composition during non imprinted polymers synthesis for catechin retention

NASA Astrophysics Data System (ADS)

Triadhi, U.; Zulfikar, M. A.; Setiyanto, H.; Amran, M. B.

2018-05-01

MISPE (molecularly imprinted Solid Phase Extraction) is a separation technique using a solid adsorbent as a principle of MI (molecularly imprinted). Methacrylic acid (MAA) was used as a monomer, ethylene glycol dimethacrylate (EGDMA) as a crosslinker, benzoyl peroxide (BPO) as an initiator and acetonitrile (ACN) as a porogen. Catechin will be used as the template. Thermal and microwave methods were employed in the synthesis method. When analyzed using FTIR spectra, it was found that there were no significant differences between NIP (non-imprinted polymer) resulting from thermal method and that resulting from microwave method. Preparation of polymers by microwave method required 4 mins at 60-65 °C, significantly less than thermal method, that took 60 minutes at the same temperature. The variations of mole ratios of the monomer, the crosslinker, and the initiator were also performed. Based on the FTIR spectra, intensity of some peaks were changed due to the decreases of concentration. The optimum composition for NIP synthesis was MAA: EGDMA: BPO ratio of 5:30:0.5 (in mmole). The TGA curve showed that the NIP sythesized using microwave method experienced mass loss of around 98.50% at 604.8 °C.

Preparation and characterization of a molecularly imprinted polymer by grafting on silica supports: a selective sorbent for patulin toxin.

PubMed

Zhao, Dayun; Jia, Jingfu; Yu, Xuelei; Sun, Xiangjun

2011-10-01

A new molecularly imprinted polymer (MIP) has been prepared on silica beads using the radical "grafting from" polymerization method for selective extraction of minor contaminant mycotoxin of patulin (PTL). After the introduction of amino groups onto the silica surface with 3-aminopropyltriethoxysilane, azo initiator onto the silica surface was achieved by the reaction of surface amino groups with 4,4'-azobis(4-cyanopentanoic acid). The scale-up synthesis of MIP was then carried out in the presence of 6-hydroxynicotinic acid as template substitute, functional, and cross-linking monomers. The prepared sorbent was characterized using FT-IR spectroscopy, scanning electron microscopy, elemental analysis, and the adsorption-desorption selectivity, and the capacity characteristic of the polymer was investigated by a conventional batch adsorption test and Scatchard plot analysis. The results indicated that coated polymers had specific adsorption to PTL as compared with its co-occurring 5-hydroxymethyl-2-furaldehyde (hydroxymethylfurfural (HMF)), at the same bulk concentration for solution of PTL and HMF, the maximum absorbance in the solid-phase extraction (SPE) method to PTL were 93.97% or 0.654 μg/mg while to HMF they were 76.89% or 0.496 μg/mg. Scatchard analysis revealed that two classes of binding sites were formed in PTL-MIP with dissociation constants of 3.2 × 10(-2) and 5.0 × 10(-3) mg/mL and the affinity binding sites of 8.029 and 1.364 mg/g, respectively. The recoveries of PTL were more than 90% for the developed MISPE and around 75% for the traditional liquid-liquid extraction in spiked apple juice samples. It was concluded that the method is suitable for the scale-up synthesis of PTL-MIP grafted on silica, and the polymer can be effectively applied as SPE coupled with high-performance liquid chromatography (HPLC) for the determination of PTL in apple juice or other related products. © Springer-Verlag 2011

Isfahan MISP Dataset.

PubMed

Kashefpur, Masoud; Kafieh, Rahele; Jorjandi, Sahar; Golmohammadi, Hadis; Khodabande, Zahra; Abbasi, Mohammadreza; Teifuri, Nilufar; Fakharzadeh, Ali Akbar; Kashefpoor, Maryam; Rabbani, Hossein

2017-01-01

An online depository was introduced to share clinical ground truth with the public and provide open access for researchers to evaluate their computer-aided algorithms. PHP was used for web programming and MySQL for database managing. The website was entitled "biosigdata.com." It was a fast, secure, and easy-to-use online database for medical signals and images. Freely registered users could download the datasets and could also share their own supplementary materials while maintaining their privacies (citation and fee). Commenting was also available for all datasets, and automatic sitemap and semi-automatic SEO indexing have been set for the site. A comprehensive list of available websites for medical datasets is also presented as a Supplementary (http://journalonweb.com/tempaccess/4800.584.JMSS_55_16I3253.pdf).

Isfahan MISP Dataset

PubMed Central

Kashefpur, Masoud; Kafieh, Rahele; Jorjandi, Sahar; Golmohammadi, Hadis; Khodabande, Zahra; Abbasi, Mohammadreza; Teifuri, Nilufar; Fakharzadeh, Ali Akbar; Kashefpoor, Maryam; Rabbani, Hossein

2017-01-01

An online depository was introduced to share clinical ground truth with the public and provide open access for researchers to evaluate their computer-aided algorithms. PHP was used for web programming and MySQL for database managing. The website was entitled “biosigdata.com.” It was a fast, secure, and easy-to-use online database for medical signals and images. Freely registered users could download the datasets and could also share their own supplementary materials while maintaining their privacies (citation and fee). Commenting was also available for all datasets, and automatic sitemap and semi-automatic SEO indexing have been set for the site. A comprehensive list of available websites for medical datasets is also presented as a Supplementary (http://journalonweb.com/tempaccess/4800.584.JMSS_55_16I3253.pdf). PMID:28487832

Investigation of the continuous flow of the sample solution on the performance of electromembrane extraction: Comparison with conventional procedure.

PubMed

Nojavan, Saeed; Sirani, Mahsa; Asadi, Sakine

2017-10-01

In this study, electromembrane extraction from a flowing sample solution, termed as continuous-flow electromembrane extraction, was developed and compared with conventional procedures for the determination of four basic drugs in real samples. Experimental parameters affecting the extraction efficiency were further studied and optimized. Under optimum conditions, linearity of continuous-flow procedure was within 8.0-500 ng/mL, while it was wider for conventional procedures (2.0-500 ng/mL). Moreover, repeatability (percentage relative standard deviation) was found to range between 5.6 and 10.4% (n = 3) for the continuous-flow procedure, with a better repeatability than that of conventional procedures (2.3-5.5% (n = 3)). Also, for the continuous-flow procedure, the estimated detection limit (signal-to-noise ratio = 3) was less than 2.4 ng/mL and extraction recoveries were within 8-10%, while the corresponding figures for conventional procedures were less than 0.6 ng/mL and 42-60%, respectively. Thus, the results showed that both continuous flow and conventional procedures were applicable for the extraction of model compounds. However, the conventional procedure was more convenient to use, and thus it was applied to determine sample drugs in real urine and wastewater samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a modified cortisol extraction procedure for intermediately sized fish not amenable to whole-body or plasma extraction methods.

PubMed

Guest, Taylor W; Blaylock, Reginald B; Evans, Andrew N

2016-02-01

The corticosteroid hormone cortisol is the central mediator of the teleost stress response. Therefore, the accurate quantification of cortisol in teleost fishes is a vital tool for addressing fundamental questions about an animal's physiological response to environmental stressors. Conventional steroid extraction methods using plasma or whole-body homogenates, however, are inefficient within an intermediate size range of fish that are too small for phlebotomy and too large for whole-body steroid extractions. To assess the potential effects of hatchery-induced stress on survival of fingerling hatchery-reared Spotted Seatrout (Cynoscion nebulosus), we developed a novel extraction procedure for measuring cortisol in intermediately sized fish (50-100 mm in length) that are not amenable to standard cortisol extraction methods. By excising a standardized portion of the caudal peduncle, this tissue extraction procedure allows for a small portion of a larger fish to be sampled for cortisol, while minimizing the potential interference from lipids that may be extracted using whole-body homogenization procedures. Assay precision was comparable to published plasma and whole-body extraction procedures, and cortisol quantification over a wide range of sample dilutions displayed parallelism versus assay standards. Intra-assay %CV was 8.54%, and average recovery of spiked samples was 102%. Also, tissue cortisol levels quantified using this method increase 30 min after handling stress and are significantly correlated with blood values. We conclude that this modified cortisol extraction procedure provides an excellent alternative to plasma and whole-body extraction procedures for intermediately sized fish, and will facilitate the efficient assessment of cortisol in a variety of situations ranging from basic laboratory research to industrial and field-based environmental health applications.

Comparison of extraction induced by emulsion breaking, ultrasonic extraction and wet digestion procedures for determination of metals in edible oil samples in Turkey using ICP-OES.

PubMed

Bakircioglu, Dilek; Kurtulus, Yasemin Bakircioglu; Yurtsever, Selcuk

2013-06-01

The content of elements (Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn) in edible oils (sunflower, hazelnut, canola, corn and olive oils) from Turkey was determined using inductively coupled plasma optical emission spectrometry (ICP-OES) after ultrasonic extraction, wet digestion, and extraction induced by emulsion breaking procedures (EIEB). In order to evaluate the best sample preparation procedure, EIEB procedure was compared by ultrasonic extraction and wet digestion procedures. The results in the samples (minimum-maximum in mgkg(-1)) were : 0.022-0.058, Cr 0.126-7.106, Cu 0.570-4.504, Fe 8.004-12.588, Mn 0.035-0.054, Ni 0.908-2.182, Pb 0.099-0.134 and Zn 2.206-8.982. The EIEB procedure was found to be fast, reliable, simple, and excellent in comparison with the other studied procedures. The recovery test was performed by spiking the samples with known amounts of the metals in the form of organometallic standards and applying the EIEB procedure. The recoveries were in the range of 96-109%. Copyright © 2012 Elsevier Ltd. All rights reserved.

Analysis of free and bound chlorophenoxy acids in cereals.

PubMed

Lokke, H

1975-06-01

Extraction of the chlorophenoxy acids 2,4-D and dichlorprop in cereals has been examined by analyzing barley from spraying experiments. A procedure has been set up by combination of acid hydrolysis and enzymatic degradation followed by extraction and clean up on either silica gel or basic aluminum oxide. The final determination is based on reaction with diazomethane and subsequently GLC with ECD. This procedure was compared with two different extraction procedures previously described in the literature. The one comparative procedure uses a mixture of 50% diethyl ether/hexane in presence of sulphuric acid and resulted in residues up to ten times lower than found after the combined acid hydrolysis/enzymatic degradation procedure. In the second comparison a direct extraction was made with a mixture of 65% (v/v) acetonitrile in water. No differences were found between this and the combined acid hydrolysis/enzymatic degradation procedure.

Extraction of DNA from forensic-type sexual assault specimens using simple, rapid sonication procedures.

PubMed

Crouse, C A; Ban, J D; D'Alessio, J K

1993-10-01

Sonication procedures for the extraction of DNA from forensic-type semen specimens have been developed, which, when compared to currently utilized sperm DNA extraction techniques, are simple, rapid and result in comparable DNA yields. Sperm DNA extraction by sonication was performed on whole semen, seminal stains, buccal swabs and post-coital specimens. Ultrasound disruption of sperm cells and their ultimate release of cellular DNA has been conducted in the presence of sperm wash buffers followed by organic extraction or Chelex 100 with little or no compromise to DNA quality, quantity or amplifiability. Two advantages of sonication over currently used forensic techniques to extract sperm DNA include 1) sperm DNA extraction that occurs within five minutes of sonication compared with an hour or greater for water bath incubations in classic enzyme digestion DNA extractions and 2) one less preparatory step with the Chelex/sonication protocol and three less steps with the sonication/organic protocol compared with other procedures thus eliminating potential sample-to-sample cross-contamination. Sperm DNA extracted by optimum sonication procedures was used for forensic HLA DQ alpha typing and restriction fragment length polymorphisms analysis without any adverse effects on typing results.

Use of different sample temperatures in a single extraction procedure for the screening of the aroma profile of plant matrices by headspace solid-phase microextraction.

PubMed

Martendal, Edmar; de Souza Silveira, Cristine Durante; Nardini, Giuliana Stael; Carasek, Eduardo

2011-06-17

This study proposes a new approach to the optimization of the extraction of the volatile fraction of plant matrices using the headspace solid-phase microextraction (HS-SPME) technique. The optimization focused on the extraction time and temperature using a CAR/DVB/PDMS 50/30 μm SPME fiber and 100mg of a mixture of plants as the sample in a 15-mL vial. The extraction time (10-60 min) and temperature (5-60 °C) were optimized by means of a central composite design. The chromatogram was divided into four groups of peaks based on the elution temperature to provide a better understanding of the influence of the extraction parameters on the extraction efficiency considering compounds with different volatilities/polarities. In view of the different optimum extraction time and temperature conditions obtained for each group, a new approach based on the use of two extraction temperatures in the same procedure is proposed. The optimum conditions were achieved by extracting for 30 min with a sample temperature of 60 °C followed by a further 15 min at 5 °C. The proposed method was compared with the optimized conventional method based on a single extraction temperature (45 min of extraction at 50 °C) by submitting five samples to both procedures. The proposed method led to better results in all cases, considering as the response both peak area and the number of identified peaks. The newly proposed optimization approach provided an excellent alternative procedure to extract analytes with quite different volatilities in the same procedure. Copyright © 2011 Elsevier B.V. All rights reserved.

Risks of postextraction bleeding after receiving direct oral anticoagulants or warfarin: a retrospective cohort study

PubMed Central

Yagyuu, Takahiro; Kawakami, Mao; Ueyama, Yoshihiro; Imada, Mitsuhiko; Kurihara, Miyako; Matsusue, Yumiko; Imai, Yuichiro; Yamamoto, Kazuhiko; Kirita, Tadaaki

2017-01-01

Objective The effect of direct oral anticoagulants (DOACs) on the risk of bleeding after tooth extraction remains unclear. This study aimed to evaluate the incidence of postextraction bleeding among patients who received DOAC and vitamin K antagonists (VKAs), such as warfarin. Design This study was a retrospective cohort analysis. Incidence rates and propensity score-matched regression models were used to compare the risks of bleeding after tooth extractions involving DOACs and VKAs. Setting The study took place in a single university hospital in Japan. Participants Between April 2013 and April 2015, 543 patients underwent a total of 1196 simple tooth extractions. Primary outcome measure The primary outcome measure was the occurrence of postextraction bleeding, which was defined as bleeding that could not be stopped by biting down on gauze and required medical treatment between 30 min and 7 days after the extraction. Results A total of 1196 tooth extractions (634 procedures) in 541 patients fulfilled the study criteria, with 72 extractions (41 procedures) involving DOACs, 100 extractions (50 procedures) involving VKAs and 1024 extractions (543 procedures) involving no anticoagulants. The incidences of postextraction bleeding per tooth for the DOAC, VKA and no anticoagulant extractions were 10.4%, 12.0% and 0.9%, respectively. The incidences of postextraction bleeding per procedure for DOACs, VKAs and no anticoagulants were 9.7%, 10.0% and 1.1%, respectively. In comparison to the VKA extractions, the DOAC extractions did not significantly increase the risk of postextraction bleeding (OR 0.69, 95% CIs 0.24 to 1.97; p=0.49). Conclusions The risk of postextraction bleeding was similar for DOAC and VKA extractions. PMID:28827248

Aviation accident forensic assessment : comprehensive single-extraction urine screening procedure : final report.

DOT National Transportation Integrated Search

1996-05-01

This paper describes a new single extraction screening procedure that was developed to identify as many drugs as possible in urine, with minimal effort and cost. Urine specimens are hydrolyzed and the specimen is then extracted using commercially pur...

The effect of different solvents and number of extraction steps on the polyphenol content and antioxidant capacity of basil leaves (Ocimum basilicum L.) extracts.

PubMed

Złotek, Urszula; Mikulska, Sylwia; Nagajek, Małgorzata; Świeca, Michał

2016-09-01

The objectives of this study were to determine best conditions for the extraction of phenolic compounds from fresh, frozen and lyophilized basil leaves. The acetone mixtures with the highest addition of acetic acid extracted most of the phenolic compounds when fresh and freeze-dried material have been used. The three times procedure was more effective than once shaking procedure in most of the extracts obtained from fresh basil leaves - unlike the extracts derived from frozen material. Surprisingly, there were not any significant differences in the content of phenolics between the two used procedures in the case of lyophilized basil leaves used for extraction. Additionally, the positive correlation between the phenolic compounds content and antioxidant activity of the studied extracts has been noted. It is concluded that the acetone mixtures were more effective than the methanol ones for polyphenol extraction. The number of extraction steps in most of the cases was also a statistically significant factor affecting the yield of phenolic extraction as well as antioxidant potential of basil leaf extracts.

Development and characterization of a green procedure for apigenin extraction from Scutellaria barbata D. Don.

PubMed

Yang, Yu-Chiao; Wei, Ming-Chi

2018-06-30

This study compared the use of ultrasound-assisted supercritical CO 2 (USC-CO 2 ) extraction to obtain apigenin-rich extracts from Scutellaria barbata D. Don with that of conventional supercritical CO 2 (SC-CO 2 ) extraction and heat-reflux extraction (HRE), conducted in parallel. This green procedure yielded 20.1% and 31.6% more apigenin than conventional SC-CO 2 extraction and HRE, respectively. Moreover, the extraction time required by the USC-CO 2 procedure, which used milder conditions, was approximately 1.9 times and 2.4 times shorter than that required by conventional SC-CO 2 extraction and HRE, respectively. Furthermore, the theoretical solubility of apigenin in the supercritical fluid system was obtained from the USC-CO 2 dynamic extraction curves and was in good agreement with the calculated values for the three empirical density-based models. The second-order kinetics model was further applied to evaluate the kinetics of USC-CO 2 extraction. The results demonstrated that the selected model allowed the evaluation of the extraction rate and extent of USC-CO 2 extraction. Copyright © 2017 Elsevier Ltd. All rights reserved.

Mobility of arsenic and its compounds in soil and soil solution: the effect of soil pretreatment and extraction methods.

PubMed

Száková, J; Tlustos, P; Goessler, W; Frková, Z; Najmanová, J

2009-12-30

The effect of soil extraction procedures and/or sample pretreatment (drying, freezing of the soil sample) on the extractability of arsenic and its compounds was tested. In the first part, five extraction procedures were compared with following order of extractable arsenic portions: 2M HNO(3)>0.43 M CH(3)COOH>or=0.05 M EDTA>or=Mehlich III (0.2M CH(3)COOH+0.25 M NH(4)NO(3)+0.013 M HNO(3)+0.015 M NH(4)F+0.001 M EDTA) extraction>water). Additionally, two methods of soil solution sampling were compared, centrifugation of saturated soil and the use of suction cups. The results showed that different sample pretreatments including soil solution sampling could lead to different absolute values of mobile arsenic content in soils. However, the interpretation of the data can lead to similar conclusions as apparent from the comparison of the soil solution sampling methods (r=0.79). For determination of arsenic compounds mild extraction procedures (0.05 M (NH(4))(2)SO(4), 0.01 M CaCl(2), and water) and soil solution sampling using suction cups were compared. Regarding the real soil conditions the extraction of fresh samples and/or in situ collection of soil solution are preferred among the sample pretreatments and/or soil extraction procedures. However, chemical stabilization of the solutions should be allowed and included in the analytical procedures for determination of individual arsenic compounds.

Rapid non-enzymatic extraction method for isolating PCR-quality camelpox virus DNA from skin.

PubMed

Yousif, A Ausama; Al-Naeem, A Abdelmohsen; Al-Ali, M Ahmad

2010-10-01

Molecular diagnostic investigations of orthopoxvirus (OPV) infections are performed using a variety of clinical samples including skin lesions, tissues from internal organs, blood and secretions. Skin samples are particularly convenient for rapid diagnosis and molecular epidemiological investigations of camelpox virus (CMLV). Classical extraction procedures and commercial spin-column-based kits are time consuming, relatively expensive, and require multiple extraction and purification steps in addition to proteinase K digestion. A rapid non-enzymatic procedure for extracting CMLV DNA from dried scabs or pox lesions was developed to overcome some of the limitations of the available DNA extraction techniques. The procedure requires as little as 10mg of tissue and produces highly purified DNA [OD(260)/OD(280) ratios between 1.47 and 1.79] with concentrations ranging from 6.5 to 16 microg/ml. The extracted CMLV DNA was proven suitable for virus-specific qualitative and, semi-quantitative PCR applications. Compared to spin-column and conventional viral DNA extraction techniques, the two-step extraction procedure saves money and time, and retains the potential for automation without compromising CMLV PCR sensitivity. Copyright (c) 2010 Elsevier B.V. All rights reserved.

[Orthogonal experiment using SFE-CO2 in extraction of essential oil from fresh Houttuynia cordata and analysis of essential oil by GC-MS].

PubMed

Meng, Jiang; Dong, Xiao-ping; Zhou, Yi-sheng; Jiang, Zhi-hong; Leung, Kelvin Sze-Yin; Zhao, Zhong-zhen

2007-02-01

To optimize the extraction procedure of essential oil from H. cordata using the SFE-CO2 and analyze the chemical composition of the essential oil. The extraction procedure of essential oil from fresh H. cordata was optimized with the orthogonal experiment. Essential oil of fresh H. cordata was analysed by GC-MS. The optimize preparative procedure was as follow: essential oil of H. cordata was extracted at a temperature of 35 degrees C, pressure of 15,000 kPa for 20 min. 38 chemical components were identified and the relative contents were quantified. The optimum preparative procedure is reliable and can guarantee the quality of essential oil.

Use of feature extraction techniques for the texture and context information in ERTS imagery: Spectral and textural processing of ERTS imagery. [classification of Kansas land use

NASA Technical Reports Server (NTRS)

Haralick, R. H. (Principal Investigator); Bosley, R. J.

1974-01-01

The author has identified the following significant results. A procedure was developed to extract cross-band textural features from ERTS MSS imagery. Evolving from a single image texture extraction procedure which uses spatial dependence matrices to measure relative co-occurrence of nearest neighbor grey tones, the cross-band texture procedure uses the distribution of neighboring grey tone N-tuple differences to measure the spatial interrelationships, or co-occurrences, of the grey tone N-tuples present in a texture pattern. In both procedures, texture is characterized in such a way as to be invariant under linear grey tone transformations. However, the cross-band procedure complements the single image procedure by extracting texture information and spectral information contained in ERTS multi-images. Classification experiments show that when used alone, without spectral processing, the cross-band texture procedure extracts more information than the single image texture analysis. Results show an improvement in average correct classification from 86.2% to 88.8% for ERTS image no. 1021-16333 with the cross-band texture procedure. However, when used together with spectral features, the single image texture plus spectral features perform better than the cross-band texture plus spectral features, with an average correct classification of 93.8% and 91.6%, respectively.

Comparative Evaluation of Different Cell Lysis and Extraction Methods for Studying Benzo(a)pyrene Metabolism in HT-29 Colon Cancer Cell Cultures

PubMed Central

Myers, Jeremy N.; Rekhadevi, Perumalla V.; Ramesh, Aramandla

2011-01-01

Lysis and extraction of cells are essential sample processing steps for investigations pertaining to metabolism of xenobiotics in cell culture studies. Of particular importance to these procedures are maintaining high lysis efficiency and analyte integrity as they influence the qualitative and quantitative distribution of drug and toxicant metabolites in the intra- and extracellular milieus. In this study we have compared the efficiency of different procedures viz. homogenization, sonication, bead beating, and molecular grinding resin treatment for disruption of HT-29 colon cells exposed to benzo(a)pyrene (BaP), a polycyclic aromatic hydrocarbon (PAH) compound and a suspected colon carcinogen. Also, we have evaluated the efficiency of various procedures for extracting BaP parent compound/metabolites from colon cells and culture media prior to High Performance Liquid Chromatography (HPLC) analyses. The extraction procedures include solid phase extraction, solid-supported liquid- liquid extraction, liquid-liquid extraction, and homogeneous liquid- liquid extraction. Our findings showed that bead-beating in combination with detergent treatment of cell pellet coupled with liquid-liquid extraction yielded greater concentrations of BaP metabolites compared to the other methods employed. Our method optimization strategy revealed that disruption of HT-29 colon cells by a combination of mechanical and chemical lysis followed by liquid-liquid extraction is efficient and robust enough for analyzing BaP metabolites from cell culture studies. PMID:21865728

A Procedure for the supercritical fluid extraction of coal samples, with subsequent analysis of extracted hydrocarbons

USGS Publications Warehouse

Kolak, Jonathan J.

2006-01-01

Introduction: This report provides a detailed, step-by-step procedure for conducting extractions with supercritical carbon dioxide (CO2) using the ISCO SFX220 supercritical fluid extraction system. Protocols for the subsequent separation and analysis of extracted hydrocarbons are also included in this report. These procedures were developed under the auspices of the project 'Assessment of Geologic Reservoirs for Carbon Dioxide Sequestration' (see http://pubs.usgs.gov/fs/fs026-03/fs026-03.pdf) to investigate possible environmental ramifications associated with CO2 storage (sequestration) in geologic reservoirs, such as deep (~1 km below land surface) coal beds. Supercritical CO2 has been used previously to extract contaminants from geologic matrices. Pressure-temperature conditions within deep coal beds may render CO2 supercritical. In this context, the ability of supercritical CO2 to extract contaminants from geologic materials may serve to mobilize noxious compounds from coal, possibly complicating storage efforts. There currently exists little information on the physicochemical interactions between supercritical CO2 and coal in this setting. The procedures described herein were developed to improve the understanding of these interactions and provide insight into the fate of CO2 and contaminants during simulated CO2 injections.

[Learning curve of vacuum extraction in residency: a preliminary study].

PubMed

Velemir, L; Vendittelli, F; Bonnefoy, C; Accoceberry, M; Savary, D; Gallot, D

2009-09-01

The aim of this study was to assess the lurning curve of young residents for vacuum extraction. All vacuum extractions performed in our department by five residents (< or =5th semester) during a study period of nine months were systematically supervised by a senior who fulfilled an assessment questionnaire from which was calculated a score reflecting the quality of the extraction. Fifty-four vacuum extractions were assessed with a mean of 10.8+/-2.9 (range, 10-13) procedures by resident. We compared the group including the six first procedures performed by each resident (group 1, n = 30) with the group including the following procedures (group 2, n = 24). We observed in the group 2 compared to the group 1, a significant improvement of the scores mean (12.3+/-5.4 vs 8.4+/-6.2, p = 0.016) and a significant reduction of the need for manual assistance by the senior (12.5% vs 40%, p = 0.034). We report a method for the learning and assessment of vacuum extraction feasible at "the bed" of the patient. This approach allows to observe a significant progression of the resident for the technique of vacuum extraction on a dozen of procedures.

Soxhlet Extraction of Caffeine from Beverage Plants

NASA Astrophysics Data System (ADS)

Adam, D. J.; Mainwaring, J.; Quigley, Michael N.

1996-12-01

A simple procedure is described for the extraction of caffeine from coffee beans or granules, tea leaves, mat leaves, etc. Since dichloromethane and several other hazardous substances are used, the procedure is best performed in a fume hood. Following extraction, melting point determination of the crystalline precipitate establishes its positive identity. Includes 33 references.

Metal fractionation in olive oil and urban sewage sludges using the three-stage BCR sequential extraction method and microwave single extractions.

PubMed

Pérez Cid, B; Fernández Alborés, A; Fernández Gómez, E; Faliqé López, E

2001-08-01

The conventional three-stage BCR sequential extraction method was employed for the fractionation of heavy metals in sewage sludge samples from an urban wastewater treatment plant and from an olive oil factory. The results obtained for Cu, Cr, Ni, Pb and Zn in these samples were compared with those attained by a simplified extraction procedure based on microwave single extractions and using the same reagents as employed in each individual BCR fraction. The microwave operating conditions in the single extractions (heating time and power) were optimized for all the metals studied in order to achieve an extraction efficiency similar to that of the conventional BCR procedure. The measurement of metals in the extracts was carried out by flame atomic absorption spectrometry. The results obtained in the first and third fractions by the proposed procedure were, for all metals, in good agreement with those obtained using the BCR sequential method. Although in the reducible fraction the extraction efficiency of the accelerated procedure was inferior to that of the conventional method, the overall metals leached by both microwave single and sequential extractions were basically the same (recoveries between 90.09 and 103.7%), except for Zn in urban sewage sludges where an extraction efficiency of 87% was achieved. Chemometric analysis showed a good correlation between the results given by the two extraction methodologies compared. The application of the proposed approach to a certified reference material (CRM-601) also provided satisfactory results in the first and third fractions, as it was observed for the sludge samples analysed.

Predicting the difficulty of a lead extraction procedure: the LED index.

PubMed

Bontempi, Luca; Vassanelli, Francesca; Cerini, Manuel; D'Aloia, Antonio; Vizzardi, Enrico; Gargaro, Alessio; Chiusso, Francesco; Mamedouv, Rashad; Lipari, Alessandro; Curnis, Antonio

2014-08-01

According to recent surveys, many sites performing permanent lead extractions do not meet the minimum prerequisites concerning personnel training, procedures' volume, or facility requirements. The current Heart Rhythm Society consensus on lead extractions suggests that patients should be referred to more experienced sites when a better outcome could be achieved. The purpose of this study was to develop a score aimed at predicting the difficulty of a lead extraction procedure through the analysis of a high-volume center database. This score could help to discriminate patients who should be sent to a referral site. A total of 889 permanent leads were extracted from 469 patients. All procedures were performed from January 2009 to May 2012 by two expert electrophysiologists, at the University Hospital of Brescia. Factors influencing the difficulty of a procedure were assessed using a univariate and a multivariate logistic regression model. The fluoroscopy time of the procedure was taken as an index of difficulty. A Lead Extraction Difficulty (LED) score was defined, considering the strongest predictors. Overall, 873 of 889 (98.2%) leads were completely removed. Major complications were reported in one patient (0.2%) who manifested cardiac tamponade. Minor complications occurred in six (1.3%) patients. No deaths occurred. Median fluoroscopic time was 8.7 min (3.3-17.3). A procedure was classified as difficult when fluoroscopy time was more than 31.2 min [90th percentile (PCTL)].At a univariate analysis, the number of extracted leads and years from implant were significantly associated with an increased risk of fluoroscopy time above 90th PCTL [odds ratio (OR) 1.51, 95% confidence interval (CI) 1.08-2.11, P = 0.01; and OR 1.19, 95% CI 1.12-1.25, P < 0.001, respectively). After adjusting for patient age and sex, and combining with other covariates potentially influencing the extraction procedure, a multivariate analysis confirmed a 71% increased risk of fluoroscopy time above 90th PCTL for each additional lead extracted (OR 1.71, 95% CI 1.06-2.77, P = 0.028) and a 23% increased risk for each year of lead age (OR 1.23, 95% CI 1.15-1.31, P < 0.001). Further nonindependent factors increasing the risk were the presence of active fixation leads and dual-coil implantable cardiac defibrillator leads. Conversely, vegetations significantly favored lead extraction.The LED score was defined as: number of extracted leads within a procedure + lead age (years from implant) + 1 if dual-coil - 1 if vegetation. The LED score independently predicted complex procedure (with fluoroscopic time >90th PCTL) both at univariate and multivariate analysis. A receiver-operating characteristic analysis showed an area under the curve of 0.81. A LED score greater than 10 could predict fluoroscopy time above 90th PCTL with a sensitivity of 78.3% and a specificity of 76.7%. The LED score is easy to compute and potentially predicts fluoroscopy time above 90th PCTL with a relatively high accuracy.

Study on the extraction, purification and quantification of jasmonic acid, abscisic acid and indole-3-acetic acid in plants.

PubMed

Zhang, Feng Juan; Jin, You Ju; Xu, Xing You; Lu, Rong Chun; Chen, Hua Jun

2008-01-01

Jasmonic acid (JA), abscisic acid (ABA) and indole-3-acetic acid (IAA) are important plant hormones. Plant hormones are difficult to analyse because they occur in small concentrations and other substances in the plant interfere with their detection. To develop a new, inexpensive procedure for the rapid extraction and purification of IAA, ABA and JA from various plant species. Samples were prepared by extraction of plant tissues with methanol and ethyl acetate. Then the extracts were further purified and enriched with C(18) cartridges. The final extracts were derivatised with diazomethane and then measured by GC-MS. The results of the new methodology were compared with those of the Creelman and Mullet procedure. Sequential elution of the assimilates from the C(18 )cartridges revealed that IAA and ABA eluted in 40% methanol, while JA subsequently eluted in 60% methanol. The new plant hormone extraction and purification procedure produced results that were comparable to those obtained with the Creelman and Mullet's procedure. This new procedure requires only 0.5 g leaf samples to quantify these compounds with high reliability and can simultaneously determine the concentrations of the three plant hormones. A simple, inexpensive method was developed for determining endogenous IAA, ABA and JA concentrations in plant tissue.

Changes in Corneal Deformation Parameters after Lenticule Creation and Extraction during Small Incision Lenticule Extraction (SMILE) Procedure

PubMed Central

Shen, Yang; Zhao, Jing; Yao, Peijun; Miao, Huamao; Niu, Lingling

2014-01-01

Purpose To investigate the effects of lenticule creation and subsequent corneal lenticule extraction on corneal deformation parameters during small incision lenticule extraction (SMILE) procedure. Materials and Methods In this prospective study, 18 eyes of 10 patients (27.90±7.11 years, −5.64±2.45 diopters) scheduled for SMILE procedure were enrolled. Changes in the corneal deformation parameters, including deformation amplitude (DA), applanation time(AT1 and AT2), applanation length(AL1 and AL2), corneal velocity(CV1 and CV2), peak distance(P.Dist.), radius and intraocular pressure values were measured preoperatively, immediately after lenticule creation and subsequent to corneal lenticule extraction in all eyes with the Corvis Scheimpflug Technology (Corvis ST, OCULUS, Wetzlar, Germany). Repeated measures analysis of variance (ANOVA) with bonferroni-adjusted post hoc comparisons was performed to investigate changes following each step of the procedure. Results All surgical procedures were uneventful. A significant difference was detected among the three time points (pre-operation, post-lenticule creation and post lenticule extraction) for AT1 (P<0.001), AT2 (P = 0.001), DA(P<0.001), and IOP(P = 0.002). Bonferroni-adjusted post hoc comparisons indicated that there was no significant change in AT1, AT2, DA, or IOP after lenticule creation (post hoc P>0.05), but there was a significant change in these parameters following subsequent corneal lenticule extraction (post hoc P<0.01), when compared to values obtained pre-operatively. The scheimpflug camera of the Corvis ST demonstrated the intralamellar small gas bubbles formed from the vaporisation of tissue after lenticule creation and a gray zone was observed between the cap and the residual stromal bed after lenticule extraction. Conclusions There is a significant change in corneal deformation parameters following SMILE procedure. The changes may be caused predominantly by stromal lenticule extraction, while lenticule creation with femtosecond laser may not have an obvious effect on corneal deformation properties. PMID:25121508

Changes in corneal deformation parameters after lenticule creation and extraction during small incision lenticule extraction (SMILE) procedure.

PubMed

Shen, Yang; Zhao, Jing; Yao, Peijun; Miao, Huamao; Niu, Lingling; Wang, Xiaoying; Zhou, Xingtao

2014-01-01

To investigate the effects of lenticule creation and subsequent corneal lenticule extraction on corneal deformation parameters during small incision lenticule extraction (SMILE) procedure. In this prospective study, 18 eyes of 10 patients (27.90 ± 7.11 years, -5.64 ± 2.45 diopters) scheduled for SMILE procedure were enrolled. Changes in the corneal deformation parameters, including deformation amplitude (DA), applanation time(AT1 and AT2), applanation length(AL1 and AL2), corneal velocity(CV1 and CV2), peak distance(P.Dist.), radius and intraocular pressure values were measured preoperatively, immediately after lenticule creation and subsequent to corneal lenticule extraction in all eyes with the Corvis Scheimpflug Technology (Corvis ST, OCULUS, Wetzlar, Germany). Repeated measures analysis of variance (ANOVA) with bonferroni-adjusted post hoc comparisons was performed to investigate changes following each step of the procedure. All surgical procedures were uneventful. A significant difference was detected among the three time points (pre-operation, post-lenticule creation and post lenticule extraction) for AT1 (P<0.001), AT2 (P = 0.001), DA(P<0.001), and IOP(P = 0.002). Bonferroni-adjusted post hoc comparisons indicated that there was no significant change in AT1, AT2, DA, or IOP after lenticule creation (post hoc P>0.05), but there was a significant change in these parameters following subsequent corneal lenticule extraction (post hoc P<0.01), when compared to values obtained pre-operatively. The scheimpflug camera of the Corvis ST demonstrated the intralamellar small gas bubbles formed from the vaporisation of tissue after lenticule creation and a gray zone was observed between the cap and the residual stromal bed after lenticule extraction. There is a significant change in corneal deformation parameters following SMILE procedure. The changes may be caused predominantly by stromal lenticule extraction, while lenticule creation with femtosecond laser may not have an obvious effect on corneal deformation properties.

Extracting Undimensional Chains from Multidimensional Datasets: A Graph Theory Approach.

ERIC Educational Resources Information Center

Yamomoto, Yoneo; Wise, Steven L.

An order-analysis procedure, which uses graph theory to extract efficiently nonredundant, unidimensional chains of items from multidimensional data sets and chain consistency as a criterion for chain membership is outlined in this paper. The procedure is intended as an alternative to the Reynolds (1976) procedure which is described as being…

Sample preparation for the analysis of isoflavones from soybeans and soy foods.

PubMed

Rostagno, M A; Villares, A; Guillamón, E; García-Lafuente, A; Martínez, J A

2009-01-02

This manuscript provides a review of the actual state and the most recent advances as well as current trends and future prospects in sample preparation and analysis for the quantification of isoflavones from soybeans and soy foods. Individual steps of the procedures used in sample preparation, including sample conservation, extraction techniques and methods, and post-extraction treatment procedures are discussed. The most commonly used methods for extraction of isoflavones with both conventional and "modern" techniques are examined in detail. These modern techniques include ultrasound-assisted extraction, pressurized liquid extraction, supercritical fluid extraction and microwave-assisted extraction. Other aspects such as stability during extraction and analysis by high performance liquid chromatography are also covered.

Transparent DNA/RNA Co-extraction Workflow Protocol Suitable for Inhibitor-Rich Environmental Samples That Focuses on Complete DNA Removal for Transcriptomic Analyses

PubMed Central

Lim, Natalie Y. N.; Roco, Constance A.; Frostegård, Åsa

2016-01-01

Adequate comparisons of DNA and cDNA libraries from complex environments require methods for co-extraction of DNA and RNA due to the inherent heterogeneity of such samples, or risk bias caused by variations in lysis and extraction efficiencies. Still, there are few methods and kits allowing simultaneous extraction of DNA and RNA from the same sample, and the existing ones generally require optimization. The proprietary nature of kit components, however, makes modifications of individual steps in the manufacturer’s recommended procedure difficult. Surprisingly, enzymatic treatments are often performed before purification procedures are complete, which we have identified here as a major problem when seeking efficient genomic DNA removal from RNA extracts. Here, we tested several DNA/RNA co-extraction commercial kits on inhibitor-rich soils, and compared them to a commonly used phenol-chloroform co-extraction method. Since none of the kits/methods co-extracted high-quality nucleic acid material, we optimized the extraction workflow by introducing small but important improvements. In particular, we illustrate the need for extensive purification prior to all enzymatic procedures, with special focus on the DNase digestion step in RNA extraction. These adjustments led to the removal of enzymatic inhibition in RNA extracts and made it possible to reduce genomic DNA to below detectable levels as determined by quantitative PCR. Notably, we confirmed that DNase digestion may not be uniform in replicate extraction reactions, thus the analysis of “representative samples” is insufficient. The modular nature of our workflow protocol allows optimization of individual steps. It also increases focus on additional purification procedures prior to enzymatic processes, in particular DNases, yielding genomic DNA-free RNA extracts suitable for metatranscriptomic analysis. PMID:27803690

Rapid methods for extraction and concentration of poliovirus from oyster tissues.

PubMed

Richards, G P; Goldmintz, D; Green, D L; Babinchak, J A

1982-12-01

A procedure is discussed for the extraction of poliovirus from oyster meats by modification of several enterovirus extraction techniques. The modified method uses meat extract and Cat-Floc, a polycationic electrolyte, for virus extraction and concentration. Virus recovery from inoculated oyster homogenates is 93-120%. Adsorption of viruses to oyster proteins by acidification of homogenates does not affect virus recovery. Elution of viruses from oyster proteins appears more efficient at pH 9.5 than at pH 8.0. This technique is relatively simple, economical and requires only 2.5 h to complete the combined extraction and concentration procedure.

Stormwater Characterization and Lagoon Sediment Analysis, Grand Forks Air Force Base, North Dakota

DTIC Science & Technology

1990-08-01

tetrachloroethylene, and 0.0026 mg/l ethyl benzene. Analyses showed no pesticides . 4. Extraction Procedure (EP) Analysis. An AFOEHL contractor performed EP extraction ...runoff met North Dakota state stream standards. Lagoon sediment did not contain Extraction Procedure hazardous chemicals. Stormwater runoff exceeded...Standards for Water Quality for the State of North Dakota ( Extracts ) 39 D Site/Analysis Summary 69 E Lift Station Flow Records 73 F Wastewater

Green procedure with a green solvent for fats and oils' determination. Microwave-integrated Soxhlet using limonene followed by microwave Clevenger distillation.

PubMed

Virot, Matthieu; Tomao, Valérie; Ginies, Christian; Visinoni, Franco; Chemat, Farid

2008-07-04

Here is described a green and original alternative procedure for fats and oils' determination in oleaginous seeds. Extractions were carried out using a by-product of the citrus industry as extraction solvent, namely d-limonene, instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using microwave energy: at first, extractions are attained using microwave-integrated Soxhlet, followed by the elimination of the solvent from the medium using a microwave Clevenger distillation in the second step. Oils extracted from olive seeds were compared with both conventional Soxhlet and microwave-integrated Soxhlet extraction procedures performed with n-hexane in terms of qualitative and quantitative determination. No significant difference was obtained between each extract allowing us to conclude that the proposed method is effective and valuable.

Modified procedure to determine acid-insoluble lignin in wood and pulp

DOE Office of Scientific and Technical Information (OSTI.GOV)

Effland, M.J.

1977-10-01

If wood is treated with strong acid, carbohydrates are hydrolyzed and solubilized. The insoluble residue is by definition lignin and can be measured gravimetrically. The standard method of analysis requires samples of 1 or 2 g of wood or pulp. In research at this laboratory these amounts of sample are often not available for analytical determinations. Thus we developed a modification of the standard procedure suitable for much smaller sample amounts. The modification is based on the procedure of Saeman. Wood samples require extraction prior to lignin analysis to remove acid-insoluble extractives that will be measured as lignin. Usually thismore » involves only a standard extraction with ethanol--benzene. However, woods high in tannin must also be subjected to extraction with alcohol. Pulps seldom require extraction.« less

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DERMAL WIPE AND SURFACE WIPE SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.27)

EPA Science Inventory

The method for extracting and preparing a dermal or surface wipe sample for analysis of acidic persistent organic pollutants is summarized in this standard operating procedure. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mas...

The utilization of modified BCR three-step sequential extraction procedure for the fractionation of Cd, Cr, Cu, Ni, Pb and Zn in soil reference materials of different origins.

PubMed

Zemberyová, Mária; Barteková, Jana; Hagarová, Ingrid

2006-12-15

A modified three-step sequential extraction procedure for the fractionation of heavy metals, proposed by the Commission of the European Communities Bureau of Reference (BCR) has been applied to the Slovak reference materials of soils (soil orthic luvisols, soil rendzina and soil eutric cambisol), which represent pedologically different types of soils in Slovakia. Analyses were carried out by flame or electrothermal atomic absorption spectrometry (FAAS or ETAAS). The fractions extracted were: exchangeable (extraction step 1), reducible-iron/manganese oxides (extraction step 2), oxidizable-organic matter and sulfides (extraction step 3). The sum of the element contents in the three fractions plus aqua-regia extractable content of the residue was compared to the aqua-regia extractable content of the elements in the origin soils. The accuracy obtained by comparing the determined contents of the elements with certified values, using BCR CRM 701, certified for the extractable contents (mass fractions) of Cd, Cr, Cu, Ni, Pb and Zn in sediment following a modified BCR-three step sequential extraction procedure, was found to be satisfactory.

Analysis of simulated angiographic procedures. Part 2: extracting efficiency data from audio and video recordings.

PubMed

Duncan, James R; Kline, Benjamin; Glaiberman, Craig B

2007-04-01

To create and test methods of extracting efficiency data from recordings of simulated renal stent procedures. Task analysis was performed and used to design a standardized testing protocol. Five experienced angiographers then performed 16 renal stent simulations using the Simbionix AngioMentor angiographic simulator. Audio and video recordings of these simulations were captured from multiple vantage points. The recordings were synchronized and compiled. A series of efficiency metrics (procedure time, contrast volume, and tool use) were then extracted from the recordings. The intraobserver and interobserver variability of these individual metrics was also assessed. The metrics were converted to costs and aggregated to determine the fixed and variable costs of a procedure segment or the entire procedure. Task analysis and pilot testing led to a standardized testing protocol suitable for performance assessment. Task analysis also identified seven checkpoints that divided the renal stent simulations into six segments. Efficiency metrics for these different segments were extracted from the recordings and showed excellent intra- and interobserver correlations. Analysis of the individual and aggregated efficiency metrics demonstrated large differences between segments as well as between different angiographers. These differences persisted when efficiency was expressed as either total or variable costs. Task analysis facilitated both protocol development and data analysis. Efficiency metrics were readily extracted from recordings of simulated procedures. Aggregating the metrics and dividing the procedure into segments revealed potential insights that could be easily overlooked because the simulator currently does not attempt to aggregate the metrics and only provides data derived from the entire procedure. The data indicate that analysis of simulated angiographic procedures will be a powerful method of assessing performance in interventional radiology.

Standard Operating Procedure for the Grinding and Extraction of Lead in Paint using Nitric Acid and a Rotor/Stator System Powered by a High Speed Motor

EPA Science Inventory

This Standard Operating Procedure (SOP) describes a new, rapid, and relatively inexpensive one step procedure which grinds the paint samples removed from the substrate and simultaneously quantitatively extracts the Pb from the paint in only one step in preparation for quantitativ...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF SOIL/HOUSE DUST FOR GC/MS ANALYSIS OF PESTICIDES (BCO-L-14.0)

EPA Science Inventory

The purpose of this SOP is to describe procedures for extracting and preparing dust or soil samples for gas chromatography/mass spectrometry (GC/MS) analysis of pesticides. This procedure was followed to ensure consistent data retrieval during the Arizona NHEXAS project and the "...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF PESTICIDES FROM SURFACE WIPE SAMPLES (BCO-L-13.0)

EPA Science Inventory

The purpose of this SOP is to describe the procedures for extracting and preparing a sill surface wipe sample for gas chromatography/mass spectrometry (GC/MS) analysis of pesticides. This procedure is also used for the pre-shipment analysis of sill wipe samples for materials sui...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF PESTICIDES FROM DERMAL WIPE SAMPLES (BCO-L-12.1)

EPA Science Inventory

The purpose of this SOP is to describe procedures for extracting and preparing a dermal wipe sample for GC/MS analysis of pesticides. This procedure was followed to ensure consistent data retrieval during the Arizona NHEXAS project and the "Border" study. Keywords: dermal wipe;...

Extraction Methods in Soil Phosphorus Characterisation

NASA Astrophysics Data System (ADS)

Soinne, Helena

2010-05-01

Extraction methods are widely used to assess the bioavailability of P and to characterise soil P reserves. Even though new and more sophisticated methods to characterise soil P are constantly developed the use of extraction methods is not likely to be replaced because of the relatively simple analytical equipment needed for the analysis. However, the large variety of extractants, pre-treatments and sample preparation procedures complicate the comparison of published results. In order to improve our understanding of the behaviour and cycling of P in soil, it is important to know the role of extracted P in the soil P cycle. The knowledge of the factors affecting the analytical outcome is a prerequisite for justified interpretation of the results. In this study, the effect of sample pre-treatment and properties of the used extractant on extractable molybdate-reactive phosphorus (MRP) and molybdate-unreactive phosphorus (MUP) was studied. Furthermore, the effect of sample preparation procedures prior the analysis on measured MRP and MUP was studied. Two widely used sequential extraction procedures were compared on their ability to show management induced differences on soil P. These results revealed that pre-treatments changed soil properties and air-drying was found to affect soil P, particularly extractable MUP, thought to represent organic P, by disrupting organic matter. This was evidenced by an increase in the water-extractable small-sized (<0.2 µm) P that, at least partly, took place at the expense of the large-sized (>0.2 µm) P. In addition to the effects of sample pre-treatment, the results showed that extractable organic P was sensitive to the chemical nature of the used extractant and to the sample preparation procedures employed prior to P analysis, including centrifugation and filtering of soil suspensions. Filtering may remove a major proportion of extractable MUP; therefore filtering cannot be recommended in the characterisation of solubilised MUP. However, extractants having high ionic strength may cause the organic molecules to collapse during centrifugation and thus affect the recovered concentration of MUP. These findings highlight the importance of characterising the nature of the MUP extracted with different extractants and acknowledging the sensitivity of MUP to analytical procedures when comparing published results. Widely used sequential fractionation procedures proved to be able to detect land-use -derived differences in the distribution of P among fractions of different solubilities. The results of this study demonstrate that, although the extraction methods do not reveal the biogeochemical function of a given P pool in soil, the extraction methods can be used to detect changes in soil P pools with different solubilities. To obtain the most benefit from extraction methods, we need a better understanding of the biological availability of P and the role of extracted P fraction in the P cycle in soils from different environments (climatic and weather) and land-uses.

Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

PubMed

Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

2017-03-01

An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of endocrine-disrupting compounds in water samples by magnetic nanoparticle-assisted dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry.

PubMed

Pérez, Rosa Ana; Albero, Beatriz; Tadeo, José Luis; Sánchez-Brunete, Consuelo

2016-11-01

A rapid extraction procedure is presented for the determination of five endocrine-disrupting compounds, estrone, ethinylestradiol, bisphenol A, triclosan, and 2-ethylhexylsalicylate, in water samples. The analysis involves a two-step extraction procedure that combines dispersive liquid-liquid microextraction (DLLME) with dispersive micro-solid phase extraction (D-μ-SPE), using magnetic nanoparticles, followed by in situ derivatization in the injection port of a gas chromatograph coupled to triple quadrupole mass spectrometry. The use of uncoated or oleate-coated Fe 3 O 4 nanoparticles as sorbent in the extraction process was evaluated and compared. The main parameters involved in the extraction process were optimized applying experimental designs. Uncoated Fe 3 O 4 nanoparticles were selected in order to simplify and make more cost-effective the procedure. DLLME was carried out at pH 3, during 2 min, followed by the addition of the nanoparticles for D-μ-SPE employing 1 min in the extraction. Analysis of spiked water samples of different sources gave satisfactory recovery results for all the compounds with detection limits ranging from 7 to 180 ng l -1 . Finally, the procedure was applied in tap, well, and river water. Graphical abstract Diagram of the extraction method using magnetic nanoparticles (MNPs).

A new organic-rich soil reference material certified for its EDTA- and acetic acid- extractable contents of Cd, Cr, Cu, Ni, Pb and Zn, following collaboratively tested and harmonised procedures.

PubMed

Pueyo, M; Rauret, G; Bacon, J R; Gomez, A; Muntau, H; Quevauviller, P; López-Sánchez, J F

2001-02-01

There is an increasing requirement for assessment of the bioavailable metal fraction and the mobility of trace elements in soils upon disposal. One of the approaches is the use of leaching procedures, but the results obtained are operationally defined; therefore, their significance is highly dependent on the extraction protocol performed. So, for this type of study, there is a need for reference materials that allow the quality of measurements to be controlled. This paper describes the steps involved in the certification of an organic-rich soil reference material, BCR-700, for the EDTA- and acetic acid-extractable contents of some trace elements, following collaboratively tested and harmonised extraction procedures. Details are given for the preparation of the soil, homogeneity and stability testing, analytical procedures and the statistical selection of data to be included in the certification.

A comparison of DNA extraction procedures for the detection of Mycobacterium ulcerans, the causative agent of Buruli ulcer, in clinical and environmental specimens.

PubMed

Durnez, Lies; Stragier, Pieter; Roebben, Karen; Ablordey, Anthony; Leirs, Herwig; Portaels, Françoise

2009-02-01

Mycobacterium ulcerans is the causative agent of Buruli ulcer, the third most common mycobacterial disease in humans after tuberculosis and leprosy. Although the disease is associated with aquatic ecosystems, cultivation of the bacillus from the environment is difficult to achieve. Therefore, at the moment, research is based on the detection by PCR of the insertion sequence IS2404 present in M. ulcerans and some closely related mycobacteria. In the present study, we compared four DNA extraction methods for detection of M. ulcerans DNA, namely the one tube cell lysis and DNA extraction procedure (OT), the FastPrep procedure (FP), the modified Boom procedure (MB), and the Maxwell 16 Procedure (M16). The methods were performed on serial dilutions of M. ulcerans, followed by PCR analysis with different PCR targets in M. ulcerans to determine the detection limit (DL) of each method. The purity of the extracted DNA and the time and effort needed were compared as well. All methods were performed on environmental specimens and the two best methods (MB and M16) were tested on clinical specimens for detection of M. ulcerans DNA. When comparing the DLs of the DNA extraction methods, the MB and M16 had a significantly lower DL than the OT and FP. For the different PCR targets, IS2404 showed a significantly lower DL than mlsA, MIRU1, MIRU5 and VNTR6. The FP and M16 were considerably faster than the MB and OT, while the purity of the DNA extracted with the MB was significantly higher than the DNA extracted with the other methods. The MB performed best on the environmental and clinical specimens. This comparative study shows that the modified Boom procedure, although lengthy, provides a better method of DNA extraction than the other methods tested for detection and identification of M. ulcerans in both clinical and environmental specimens.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bae, Wookeun; Shin, Eung Bai; Lee, Kil Chul

The potential hazard of landfill wastes was previously evaluated by examining the extraction procedures for individual waste, although various wastes were co-disposed of in actual landfills. This paper investigates the reduction of extraction-procedure toxicity by co-disposing various combinations of two wastes. When two wastes are mixed homogeneously, the extraction of heavy metals from the waste mixture is critically affected by the extract pH. Thus, co-disposal wastes will have a resultant pH between the pH values of its constituent. The lower the resultant pH, the lower the concentrations of heavy metals in the extract. When these wastes are extracted sequentially, themore » latter extracted waste has a stronger influence on the final concentration of heavy metals in the extract. Small-scale lysimeter experiments confirm that when heavy-metal-bearing leachates Generated from hazardous-waste lysimeters are passed through a nonhazardous-waste lysimeter filled with compost, briquette ash, or refuse-incineration ashes, the heavy-metal concentration in the final leachates decreases significantly. Thus, the heavy-metal leaching could be attenuated if a less extraction-procedure-toxic waste were placed at the bottom of a landfill. 3 refs., 4 figs., 5 tabs.« less

Determination of cadmium in sediments by diluted HCI extraction and isotope dilution ICP-MS.

PubMed

Terán-Baamonde, Javier; Soto-Ferreiro, Rosa-María; Carlosena, Alatzne; Andrade, José-Manuel; Prada, Darío

2018-08-15

Isotope dilution ICP-MS is proposed to measure the mass fraction of Cd extracted by diluted HCl in marine sediments, using a fast and simple extraction procedure based on ultrasonic probe agitation. The 111 Cd isotope was added before the extraction to achieve isotope equilibration with native Cd solubilized from the sample. The parameters affecting trueness and precision of isotope ratio measurements were evaluated carefully and subsequently corrected in order to minimize errors; they were: detector dead time, spectral interferences, mass discrimination factor and optimum sample/spike ratio. The mass fraction of Cd extracted was compared with the sum of the certified contents of the three steps of the sequential extraction procedure of the Standards, Measurements and Testing Programme (SM&T) analysing the BCR 701 sediment to validate the method. The certified and measured values agreed, giving a measured / certified mass fraction ratio of 1.05. Further, the extraction procedure itself was studied by adding the enriched isotope after the extraction step, which allowed verifying that analyte losses occurred during this process. Two additional reference sediments with certified total cadmium contents were also analysed. The method provided very good precision (0.9%, RSD) and a low detection limit, 1.8 ng g -1 . The procedural uncertainty budget was estimated following the EURACHEM Guide by means of the 'GUM Workbench' software, obtaining a relative expanded uncertainty of 1.5%. The procedure was applied to determine the bioaccessible mass fraction of Cd in sediments from two environmentally and economically important areas of Galicia (rias of Arousa and Vigo, NW of Spain). Copyright © 2018 Elsevier B.V. All rights reserved.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF PESTICIDES FROM DERMAL WIPE SAMPLES (BCO-L-12.1)

EPA Science Inventory

The purpose of this SOP is to describe procedures for extracting and preparing a dermal wipe sample for GC/MS analysis of pesticides. This procedure was followed to ensure consistent data retrieval during the Arizona NHEXAS project and the Border study. Keywords: dermal wipe; p...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF SOIL AND HOUSE DUST SAMPLES FOR GC/MS ANALYSIS OF PESTICIDE AND PAH (BCO-L-28.0)

EPA Science Inventory

The purpose of this SOP is to describe procedures for extracting and preparing a dust or soil sample for gas chromatography mass spectrometry (GC/MS) analysis of pesticides and polyaromatic hydrocarbons (PAHs). This procedure was followed to ensure consistent data retrieval durin...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF AIR SAMPLES FOR GC/MS ANALYSIS OF PESTICIDES (BCO-L-11.0)

EPA Science Inventory

The purpose of this SOP is to describe the procedures for extracting and preparing an air sample consisting of a polyurethane foam (PUF) plug and Teflon-coated glass fiber filter (Pallflex T60A20) for analysis of pesticides. This procedure covers sample preparation for samples t...

Procedure optimization for green synthesis of silver nanoparticles by aqueous extract of Eucalyptus oleosa.

PubMed

Pourmortazavi, Seied Mahdi; Taghdiri, Mehdi; Makari, Vajihe; Rahimi-Nasrabadi, Mehdi

2015-02-05

The present study is dealing with the green synthesis of silver nanoparticles using the aqueous extract of Eucalyptus oleosa as a green synthesis procedure without any catalyst, template or surfactant. Colloidal silver nanoparticles were synthesized by reacting aqueous AgNO3 with E. oleosa leaf extract at non-photomediated conditions. The significance of some synthesis conditions such as: silver nitrate concentration, concentration of the plant extract, time of synthesis reaction and temperature of plant extraction procedure on the particle size of synthesized silver particles was investigated and optimized. The participations of the studied factors in controlling the particle size of reduced silver were quantitatively evaluated via analysis of variance (ANOVA). The results of this investigation showed that silver nanoparticles could be synthesized by tuning significant parameters, while performing the synthesis procedure at optimum conditions leads to form silver nanoparticles with 21nm as averaged size. Ultraviolet-visible spectroscopy was used to monitor the development of silver nanoparticles formation. Meanwhile, produced silver nanoparticles were characterized by scanning electron microscopy, energy-dispersive X-ray, and FT-IR techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of a standardized sequential extraction protocol for simultaneous extraction of multiple actinide elements

DOE PAGES

Faye, Sherry A.; Richards, Jason M.; Gallardo, Athena M.; ...

2017-02-07

Sequential extraction is a useful technique for assessing the potential to leach actinides from soils; however, current literature lacks uniformity in experimental details, making direct comparison of results impossible. This work continued development toward a standardized five-step sequential extraction protocol by analyzing extraction behaviors of 232Th, 238U, 239,240Pu and 241Am from lake and ocean sediment reference materials. Results produced a standardized procedure after creating more defined reaction conditions to improve method repeatability. A NaOH fusion procedure is recommended following sequential leaching for the complete dissolution of insoluble species.

On the problem of nonsense correlations in allergological tests after routine extraction.

PubMed

Rijckaert, G

1981-01-01

The influence of extraction procedures and culturing methods of material used for the preparation of allergenic extracts on correlation patterns found in allergological testing (skin test and RAST) was investigated. In our laboratory a short extraction procedure performed at O degrees C was used for Aspergillus repens. A. penicilloides, Wallemia sebi, their rearing media and non-inoculated medium. For the commercially available extracts from house dust, house-dust mite, pollen of Dactylus glomerata and A. penicilloides a longer procedure (several days) performed at room temperature was used. Statistical analysis showed a separation of all test results into two clusters, each cluster being composed of correlations between extracts from only one the manufacturers did not show any correlation. The correlations found between the short time incubated extracts of the xerophilic fungi and their rearing media could be explained by genetical and biochemical relationships between these fungi depending on ecological conditions. However, while the correlation found between house dust and house-dust mite is understandable, correlations found between long time incubated extracts from house-dust mite and D. glomerata or A. penicilloides may be nonsense correlations, that do not adequately describe the in vivo situation. The similarity of these extracts is presumably artificially created during extraction.

Unerupted lower third molar extractions and their risks for mandibular fracture.

PubMed

Corrêa, Ana Paula Simões; Faverani, Leonardo Perez; Ramalho-Ferreira, Gabriel; Ferreira, Sabrina; Ávila Souza, Francisley; de Oliveira Puttini, Igor; Rangel Garcia-Júnior, Idelmo

2014-05-01

As every surgical procedure extraction of third molars can result in several complications, among them the mandibular angle fracture. Predisposing factors for fracture should be analyzed during and after the surgery. This paper aims to discuss the predisposing factors to the occurrence of mandibular angle fractures during and after the procedure for third molars extraction, as well as surgical principles to avoid this complication.

A standardized method for sampling and extraction methods for quantifying microplastics in beach sand.

PubMed

Besley, Aiken; Vijver, Martina G; Behrens, Paul; Bosker, Thijs

2017-01-15

Microplastics are ubiquitous in the environment, are frequently ingested by organisms, and may potentially cause harm. A range of studies have found significant levels of microplastics in beach sand. However, there is a considerable amount of methodological variability among these studies. Methodological variation currently limits comparisons as there is no standard procedure for sampling or extraction of microplastics. We identify key sampling and extraction procedures across the literature through a detailed review. We find that sampling depth, sampling location, number of repeat extractions, and settling times are the critical parameters of variation. Next, using a case-study we determine whether and to what extent these differences impact study outcomes. By investigating the common practices identified in the literature with the case-study, we provide a standard operating procedure for sampling and extracting microplastics from beach sand. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparison of results from simple expressions for MOSFET parameter extraction

NASA Technical Reports Server (NTRS)

Buehler, M. G.; Lin, Y.-S.

1988-01-01

In this paper results are compared from a parameter extraction procedure applied to the linear, saturation, and subthreshold regions for enhancement-mode MOSFETs fabricated in a 3-micron CMOS process. The results indicate that the extracted parameters differ significantly depending on the extraction algorithm and the distribution of I-V data points. It was observed that KP values vary by 30 percent, VT values differ by 50 mV, and Delta L values differ by 1 micron. Thus for acceptance of wafers from foundries and for modeling purposes, the extraction method and data point distribution must be specified. In this paper measurement and extraction procedures that will allow a consistent evaluation of measured parameters are discussed.

Determination of available phosphorus in soils by using a new extraction procedure and a flow injection amperometric system.

PubMed

Jakmunee, Jaroon; Junsomboon, Jaroon

2009-09-15

A new extraction procedure based on an off-line extraction column was proposed for extracting of available phosphorus from soils. The column was fabricated from a plastic syringe fitted at the bottom with a cotton wool and a piece of filter paper to support a soil sample. An aliquot (50 mL) of extracting solution (0.05 M HCl+0.0125 M H(2)SO(4)) was used to extract the sample under gravity flow and the eluate was collected in a polyethylene bottle. The extract was then analyzed for phosphorus contents by a simple flow injection amperometric system, employing a set of three-way solenoid valves as an injection valve. The method is based on the electrochemical reduction of 12-molybdophosphate which is produced on-line by the reaction of orthophosphate with acidic molybdate and the electrical current produced was directly proportional to the concentration of phosphate in range of 0.1-10.0 mg L(-1) PO(4)-P, with a detection limit of 0.02 mg L(-1). Relative standard for 11 replicate injections of 5 mg L(-1) PO(4)-P was 0.5%. A sample through put of 35 h(-1) was achieved, with consumption of 14 mg KCl, 10mg ammonium molybdate and 0.05 mL H(2)SO(4) per analysis. The detection system does not suffer from the interferences that are encountered in the photometric method such as colored substances, colloids, metal ions, silicate and refractive index effect (Schlieren effect). The results obtained by the column extraction procedure were well correlated with those obtained by the steady-state extraction procedure, but showed slightly higher extraction efficiency.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SOLID FOOD SAMPLES FOR ANALYSIS OF PERSISTENT ORGANIC POLLUTANTS (SOP-5.20)

EPA Science Inventory

This SOP describes the procedures for homogenizing, extracting and concentrating solid food samples for persistent organic pollutants such as organochlorine compounds, organophosphate compounds, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, substituted phenols, and...

CTEPP STANDARD OPERATING PROCEDURE FOR DETECTION AND QUANTIFICATION OF TARGET ANALYTES BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS) (SOP-5.24)

EPA Science Inventory

This standard operating procedure describes the method used for the determination of target analytes in sample extracts and related quality assurance/quality control sample extracts generated in the CTEPP study.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING LIQUID FOOD SAMPLES FOR ANALYSIS OF PERSISTENT ORGANIC POLLUTANTS (SOP-5.19)

EPA Science Inventory

This SOP describes the procedures for homogenizing, extracting, and concentrating liquid food samples for neutral persistent organic pollutants such as organochlorine compounds, organophosphate compounds, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, and phenols.

Immobilization of microalgae cells in alginate facilitates isolation of DNA and RNA.

PubMed

Lopez, Blanca R; Hernandez, Juan-Pablo; Bashan, Yoav; de-Bashan, Luz E

2017-04-01

Isolation of nucleic acids from Chlorella is difficult, given the chemically complex nature of their cell walls and variable production of metabolites. Immobilization of microalgae in polymers adds additional difficulty. Here, we modified, amended, and standardized methods for isolation of nucleic acids and compared the yield of DNA and RNA from free-living and encapsulated microalgae C. sorokiniana. Isolation of nucleic acids from immobilized cells required two steps in dissolving the alginate matrix, releasing the cells, and mechanical disruption with glass beads. For DNA extraction, we used modified versions of a commercial kit along with the hexadecyltrimethylammonium bromide (CTAB) method. For RNA extraction, we used the commercial TRI reagent procedure and the CTAB-dithiotreitol method. Quantity and quality of nucleic acids in extracts varied with growth conditions, isolation procedures, and time of incubation of the original culture. There were consistently higher amounts of DNA and RNA in extracts from immobilized cells. Quantitatively, the modified procedure with the commercial Promega kit was the most reliable procedure for isolating DNA and a modified commercial TRI reagent procedure was the choice for isolating RNA. All four procedures eliminated proteins efficiently and had low levels of contamination from residual polysaccharides from the matrices and/or metabolites naturally produced by the microalgae. All DNA extracts under both growth conditions, time of incubation, and two isolation methods successfully amplified the 18S ribosomal RNA by PCR and quantitative reverse transcription (RT-qPCR). Copyright © 2017 Elsevier B.V. All rights reserved.

Modified extraction procedure for gas-liquid chromatography applied to the identification of anaerobic bacteria.

PubMed Central

Thomann, W R; Hill, G B

1986-01-01

Chloroform and ether commonly are used as solvents to extract metabolic organic acids for analysis by gas-liquid chromatography in the identification of anaerobic bacteria. Because these solvents are potentially hazardous to personnel, modified extraction procedures involving the use of a safer solvent, methyl tert-butyl ether were developed which remained both simple to perform and effective for organism identification. PMID:3700623

Automated extraction of temporal motor activity signals from video recordings of neonatal seizures based on adaptive block matching.

PubMed

Karayiannis, Nicolaos B; Sami, Abdul; Frost, James D; Wise, Merrill S; Mizrahi, Eli M

2005-04-01

This paper presents an automated procedure developed to extract quantitative information from video recordings of neonatal seizures in the form of motor activity signals. This procedure relies on optical flow computation to select anatomical sites located on the infants' body parts. Motor activity signals are extracted by tracking selected anatomical sites during the seizure using adaptive block matching. A block of pixels is tracked throughout a sequence of frames by searching for the most similar block of pixels in subsequent frames; this search is facilitated by employing various update strategies to account for the changing appearance of the block. The proposed procedure is used to extract temporal motor activity signals from video recordings of neonatal seizures and other events not associated with seizures.

The automatic extraction of pitch perturbation using microcomputers: some methodological considerations.

PubMed

Deem, J F; Manning, W H; Knack, J V; Matesich, J S

1989-09-01

A program for the automatic extraction of jitter (PAEJ) was developed for the clinical measurement of pitch perturbations using a microcomputer. The program currently includes 12 implementations of an algorithm for marking the boundary criteria for a fundamental period of vocal fold vibration. The relative sensitivity of these extraction procedures for identifying the pitch period was compared using sine waves. Data obtained to date provide information for each procedure concerning the effects of waveform peakedness and slope, sample duration in cycles, noise level of the analysis system with both direct and tape recorded input, and the influence of interpolation. Zero crossing extraction procedures provided lower jitter values regardless of sine wave frequency or sample duration. The procedures making use of positive- or negative-going zero crossings with interpolation provided the lowest measures of jitter with the sine wave stimuli. Pilot data obtained with normal-speaking adults indicated that jitter measures varied as a function of the speaker, vowel, and sample duration.

Method 1664: N-hexane extractable material (hem) and silica gel treated n-hexane extractable material (SGT-HEM) by extraction and gravimetry (oil and grease and total petroleum hydrocarbons), April 1995

DOE Office of Scientific and Technical Information (OSTI.GOV)

NONE

Method 1664 was developed by the United States Environmental Protection Agency Office of Science and Technology to replace previously used gravimetric procedures that employed Freon-113, a Class I CFC, as the extraction solvent for the determination of oil and grease and petroleum hydrocarbons. Method 1664 is a performance-based method applicable to aqueous matrices that requires the use of n-hexane as the extraction solvent and gravimetry as the determinative technique. In addition, QC procedures designed to monitor precision and accuracy have been incorporated into Method 1664.

Development of an analytical procedure to study linear alkylbenzenesulphonate (LAS) degradation in sewage sludge-amended soils.

PubMed

Comellas, L; Portillo, J L; Vaquero, M T

1993-12-24

A procedure for determining linear alkylbenzenesulphonates (LASs) in sewage sludge and amended soils has been developed. Extraction by sample treatment with 0.5 M potassium hydroxide in methanol and reflux was compared with a previously described extraction procedure in Soxhlet with methanol and solid sodium hydroxide in the sample. Repeatability results were similar with savings in extraction time, solvents and evaporation time. A clean-up method involving a C18 cartridge has been developed. Analytes were quantified by a reversed-phase HPLC method with UV and fluorescence detectors. Recoveries obtained were higher than 84%. The standing procedure was applied to high doses of sewage sludge-amended soils (15%) with increasing quantities of added LASs. Degradation data for a 116-day period are presented.

Computational physics in RISC environments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rhoades, C.E. Jr.

The new high performance Reduced Instruction Set Computers (RISC) promise near Cray-level performance at near personal-computer prices. This paper explores the performance, conversion and compatibility issues associated with developing, testing and using our traditional, large-scale simulation models in the RISC environments exemplified by the IBM RS6000 and MISP R3000 machines. The questions of operating systems (CTSS versus UNIX), compilers (Fortran, C, pointers) and data are addressed in detail. Overall, it is concluded that the RISC environments are practical for a very wide range of computational physic activities. Indeed, all but the very largest two- and three-dimensional codes will work quitemore » well, particularly in a single user environment. Easily projected hardware-performance increases will revolutionize the field of computational physics. The way we do research will change profoundly in the next few years. There is, however, nothing more difficult to plan, nor more dangerous to manage than the creation of this new world.« less

Computational physics in RISC environments. Revision 1

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rhoades, C.E. Jr.

The new high performance Reduced Instruction Set Computers (RISC) promise near Cray-level performance at near personal-computer prices. This paper explores the performance, conversion and compatibility issues associated with developing, testing and using our traditional, large-scale simulation models in the RISC environments exemplified by the IBM RS6000 and MISP R3000 machines. The questions of operating systems (CTSS versus UNIX), compilers (Fortran, C, pointers) and data are addressed in detail. Overall, it is concluded that the RISC environments are practical for a very wide range of computational physic activities. Indeed, all but the very largest two- and three-dimensional codes will work quitemore » well, particularly in a single user environment. Easily projected hardware-performance increases will revolutionize the field of computational physics. The way we do research will change profoundly in the next few years. There is, however, nothing more difficult to plan, nor more dangerous to manage than the creation of this new world.« less

Clean-up of aqueous acetone vegetable extracts by solid-matrix partition for pyrethroid residue determination by gas chromatography-electron-capture detection.

PubMed

Di Muccio, A; Barbini, D A; Generali, T; Pelosi, P; Ausili, A; Vergori, F; Camoni, I

1997-03-21

Disposable, ready-to-use cartridges filled with macroporous diatomaceous material are used to carry out a partition clean-up that, in a single step, is capable of transferring pesticide residues from aqueous acetone extracts into light petroleum-dichloromethane (75:25, v/v). This procedure takes the place of some functions (such as separatory-funnel partition, drying over anhydrous sodium sulphate and partial adsorption clean-up) usually performed by separate steps in classical schemes. Fourteen pyrethroid pesticides, including tefluthrin, tetramethrin, cyphenothrin, cyfluthrin, flucythrinate, tau-fluvalinate, deltamethrin, bioallethrin, fenpropathrin, lambda-cyhalothrin, permethrin, alpha-cypermethrin, esfenvalerate and tralomethrin were determined using the described procedure with satisfactory recoveries for most of them, at spiking levels ranging from 0.08 to 0.82 mg/kg for the different compounds. Crops subjected to the described procedure included strawberry, apple, and orange gave extracts containing a mass of co-extractives that was between 5 and 30 mg. Compared with classical schemes, the described procedure is simple, less labour intensive, allows parallel handling of several extracts and does not require the preparation and maintenance of equipment. Troublesome emulsions such as those frequently observed in separation funnel partitioning do not occur.

Comparison of procedure coding systems for level 1 and 2 hospitals in South Africa.

PubMed

Montewa, Lebogang; Hanmer, Lyn; Reagon, Gavin

2013-01-01

The ability of three procedure coding systems to reflect the procedure concepts extracted from patient records from six hospitals was compared, in order to inform decision making about a procedure coding standard for South Africa. A convenience sample of 126 procedure concepts was extracted from patient records at three level 1 hospitals and three level 2 hospitals. Each procedure concept was coded using ICPC-2, ICD-9-CM, and CCSA-2001. The extent to which each code assigned actually reflected the procedure concept was evaluated (between 'no match' and 'complete match'). For the study sample, CCSA-2001 was found to reflect the procedure concepts most completely, followed by ICD-9-CM and then ICPC-2. In practice, decision making about procedure coding standards would depend on multiple factors in addition to coding accuracy.

Birch pollinosis and atopy caused by apple, peach, and hazelnut; comparison of three extraction procedures with two apple strains.

PubMed

de Groot, H; de Jong, N W; Vuijk, M H; Gerth van Wijk, R

1996-10-01

This study aimed, first, to study the prevalence in The Netherlands of atopy caused by apple, peach, and hazelnut in patients with tree pollinosis, and, second, to compare three extraction procedures for skin prick testing with two different apple strains. Skin prick tests and RAST were performed on 79 consecutive patients with tree pollinosis, visiting the department of allergology during spring 1995. In skin prick tests, we used three different extracts (juice, freeze-dried extract, and low-temperature acetone powder extract) of two apple strains, Golden Delicious and Granny Smith. Case histories for apple, peach, and hazelnut were positive in 35 (44.3%), 23 (29%), and 35 (44.3%) patients, respectively. More than two-thirds of the patients had symptoms characteristic of oral allergy syndrome. Skin prick tests for apple, peach, and hazelnut were positive in 51 (64.6%), 61 (77.2%), and 71 (89.9%) patients, respectively. Granny Smith showed more positive skin reactions and a better agreement with clinical history than Golden Delicious, and juice was superior to the two other extraction procedures for both apple strains. RAST for apple, peach, and hazelnut was positive in 53 (68.8%), 13 (16.9%), and 31 (40.3%) patients, respectively. Concordance between skin prick test and case history was found in 77%, 52%, and 54%, for apple, peach, and hazelnut, respectively. We found a high percentage of concurrence of clinical allergy to birch pollen and apple, peach, and hazelnut, confirmed by both skin prick testing and RAST. Approximately half of these patients had symptoms (especially oral allergy syndrome) after eating these products. We also found an easy extraction procedure (juice extract) suitable for apple skin prick testing, superior even to freeze-dried extraction or the low-temperature acetone powder technique.

Development of extraction procedure for determination of mercury species using SPME-assisted dispersive derivative agent

NASA Astrophysics Data System (ADS)

Abdullah, Md Pauzi; Khalik, Wan Mohd Afiq Wan Mohd; Othman, Mohamed Rozali

2016-11-01

The extraction procedure for determination of low level mercury using solid phase microextraction was successfully carried out. Design of experimental works using factorial design and central composite design were applied to screen and predict the optimum condition for extraction step. In this study, variables namely concentration level (5 % m/v) and volume of derivatization solution (150 µL) has depicted as main effect for controlling the suitability of derivative reagent condition. Maximum of signal response (account as total peak areas for mercury species) was obtained when extraction procedure was set up at pH of water sample (5.8), extraction time (14 min), extraction temperature (43 °C) and stirring rate (450 rpm). Reducing time required to reach equilibrium is new improvement achieved in this study. Detection limit for each species (MeHg 26.17 ngL-1; EtHg 48.84 ngL-1 and IHg 14.11 ngL-1) was calculated lower than our previous work. Recovery, repeatability and reproducibility trial were recorded varied at acceptable range and relative standard deviation was calculated below than 10 %.

New procedure for extraction of algal lipids from wet biomass: a green clean and scalable process.

PubMed

Dejoye Tanzi, Celine; Abert Vian, Maryline; Chemat, Farid

2013-04-01

A new procedure, called Simultaneous Distillation and Extraction Process (SDEP), for lipid extraction from wet microalgae (Nannochloropsis oculata and Dunaliella salina) was reported. This method does not require a pre-drying of the biomass and employs alternative solvents such as d-limonene, α-pinene and p-cymene. This procedure has been compared with Soxhlet extraction (Sox) and Bligh & Dyer method (B&D). For N. oculata, results showed that SDEP-cymene provided similar lipid yields to B&D (21.45% and 23.78%), while SDEP-limonene and pinene provided lower yields (18.73% and 18.75% respectively). For D. salina, SDEP-pinene provided the maximum lipid yield (3.29%) compared to the other solvents, which is quite close to B&D result (4.03%). No significant differences in terms of distribution of lipid classes and fatty acid composition have been obtained for different techniques. Evaluation of energy consumption indicates a substantial saving in the extraction cost by SDEP compared to the conventional extraction technique, Soxhlet. Copyright © 2013 Elsevier Ltd. All rights reserved.

ASSESSMENT OF A SEQUENTIAL EXTRACTION PROCEDURE FOR PERTURBED LEAD-CONTAMINATED SAMPLES WITH AND WITHOUT PHOSPHOROUS AMENDMENTS

EPA Science Inventory

Sequential extraction procedures are used to determine the solid-phase association in which elements of interest exist in soil and sediment matrices. Foundational work by Tessier et al. (1) has found widespread acceptance and has worked tolerably as an operational definition for...

Optimizing the extraction, storage, and analysis of airborne endotoxins

USDA-ARS?s Scientific Manuscript database

While the Limulus amebocyte lysate (LAL) assay is part of most procedures to assess airborne endotoxin exposure, there is no universally agreed upon standard procedure. The purpose of this study was to fill in additional knowledge gaps with respect to the extraction, storage, and analysis of endotox...

Surgical and social implications of extraction of mandibular third molars as a separate procedure before bilateral sagittal split osteotomy.

PubMed

Morton, L; Downie, I

2017-11-01

In some units, lower wisdom teeth are extracted in a separate procedure before bilateral sagittal split osteotomy (BSSO), whereas in others they are removed at the time of the osteotomy. We identified 57 patients who had BSSO at Salisbury Hospital between October 2013 and September 2015, 40 of whom had their wisdom teeth extracted at the same time. The remaining 17 did not have wisdom teeth. Patients who have these teeth extracted as a separate procedure require at least one day off work, which can result in a loss of earnings. Our findings showed that the removal of third molars at the time of orthognathic surgery has considerable social and financial benefits, and does not increase the risk of morbidity. Copyright © 2017. Published by Elsevier Ltd.

A comparison of recovery of virus from wastewaters by beef extract-Celite, ferric chloride, and filter concentration procedures.

PubMed

Dahling, D R; Wright, B A

1988-12-01

An improved concentration method using sample volumes as large as 1500 ml has been developed to monitor for viruses in wastewaters. Non-precipitating dry beef extract powder is added to wastewater samples to give a 3% concentration and mixed until dissolved. This is followed by the addition of Celite as a virus adsorbent. By manipulating pH, viruses are eluted from the Celite in small volumes of phosphate buffer. This procedure was further tested without the aid of the Celite additives using a precipitating beef extract powder and substituting FeCl3 as an alternate reagent for the Celite. Comparison testing was also made with the currently recommended cartridge and disc filter procedures. In all cases, the non-precipitating beef extract-Celite method gave higher recovery rates in highly polluted waters.

Cleanup procedure for water, soil, animal and plant extracts for the use of electron-capture detector in the gas chromatographic analysis of organophosphorus insecticide residues.

PubMed

Kadoum, A M

1968-07-01

A simple, aqueous acetonitrile partition cleanup method for analyses of some common organophosphorus insecticide residues is described. The procedure described is for cleanup and quantitative recovery of parathion, methyl parathion, diazinon, malathion and thimet from different extracts. Those insecticides in the purified extracts of ground water, grain, soil, plant and animal tissues can be detected quantitatively by gas chromatography with an electron capture-detector at 0.01 ppm. Cleanup is satisfactory for paper and thin-layer chromatography for further identification of individual insecticides in the extracts.

[Determination of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla by HPLC].

PubMed

Yang, Xiu-Juan; Hong, Yan-Long; Wu, Fei; Ruan, Ke-Feng; Feng, Yi

2013-03-01

To explore an HPLC method for determination of rhnchophylline and isorhnchophylline in Uncaria rhnchophylla. An HPLC method has been developed for determination of rhnchophylline and isorhnchophylline. The transformation of rhnchophylline and isorhnchophylline after heating was also studied by HPLC-ESI-MS. Good linearities of rhynchophylline and isorhynchophylline were 0.064-5.100, 0.064-5.110 mg, respectively. The average recoveries were from 87.51% to 88.83% for rhynchophylline and from 107.9% to 113.9% for isorhynchophylline. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 12.60% and 40.00% in the reflux extraction procedure, respectively. While in the ultrasonic extraction procedure, the average recoveries of rhynchophylline and isorhynchophylline was from 99.48% to 103.2% and from 97.00% to 99.59%, resepectively. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 47.08% and 51.03%, respectively. The unqualified recovery could be elucidated by HPLC-ESI-MS analysis, indicating that trhynchophylline could be transformed mostly into isorhynchophylline and a little amount of unkown composition, while isorhynchophylline could be transformed into rhynchophylline isocorynoxeine, corynoxeine and 22-O-beta-D-glucopyranosyl isocorynoxeinic acid during the extraction procedure. Ultrasonic extraction procedure was more sutble for HPLC determination of the content of rhynchophylline and isorhynchophylline in U. rhnchophylla, however, the recovery problems should be paid attention to when it comes to the determination.

Extraction and analysis of adenosine triphosphate from aquatic environments

USGS Publications Warehouse

Stephens, Doyle W.; Shultz, David J.

1981-01-01

A variety of adenosine triphosphate (ATP) extraction procedures have been investigated for their applicability to samples from aquatic environments. The cold sulfuric-oxalic acid procedure was best suited to samples consisting of water, periphyton, and sediments. Due to cation and fulvic acid interferences, a spike with a known quantity of ATP was necessary to estimate losses when sediments were extracted. Variable colonization densities for periphyton required that several replicates be extracted to characterize acdurately the periphyton community. Extracted samples were stable at room temperature for one to five hours, depending on the ATP concentration, if the pH was below 2. Neutralized samples which were quick frozen and stored at -30°C were stable for months.

Comparison of methods for hydrocarbon analysis of marine biota

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gritz, R.L.; Shaw, D.G.

1977-04-01

A comparison was made of several procedures for the isolation of hydrocarbons from other matter and for the fractionation of hydrocarbons according to chemical type. The efficiency of Soxhlet extraction followed by saponification with extraction by alkaline digestion (direct saponification) was compared using two hour and 24 hour reaction times. All procedures were performed on approximately 60 g of soft parts of Saxidomus gigantea (butter clam). The 24 hour saponification and column chromatography on partially deactivated columns constituted the best procedure tested. Soxhlet extraction followed by two hour saponification did not completely remove methyl esters and was the most laboriousmore » technique. Direct two hour saponification was also questionable in the removal of esters and led to severe emulsion problems. The recoveries of hydrocarbons by the three procedures was substantially the same.« less

The Measurement of Human Body-Fluid Volumes: Resting Fluid Volumes Before and After Heat Acclimation

DTIC Science & Technology

2001-01-01

equilibration period. Erythrocytes aliquots were haemolysed before counting with saponin . Both counts were used to correct the derived ECFV, which was...was largely in accordance with the procedures of Greenleaf et al. (1980). This technique used an extraction procedure in which the dye was first...collection. Therefore, the above extraction procedure was not used. A major limitation of using a cellulose column is the possibility of not collecting all

EVALUATION OF THE RCRA (RESOURCE CONSERVATION AND RECOVERY ACT) EXTRACTION PROCEDURE - LYSIMETER STUDIES WITH MUNICIPAL/INDUSTRIAL WASTES

EPA Science Inventory

A study was initiated to determine the accuracy with which the Extraction Procedures (EP), employed in the regulations promulgated under Section 3001 of the Resource Conservation and Recovery Act (40 CFR 26.124), simulates the leaching an industrial waste would undergo when codis...

Multicenter Comparative Evaluation of Five Commercial Methods for Toxoplasma DNA Extraction from Amniotic Fluid▿

PubMed Central

Yera, H.; Filisetti, D.; Bastien, P.; Ancelle, T.; Thulliez, P.; Delhaes, L.

2009-01-01

Over the past few years, a number of new nucleic acid extraction methods and extraction platforms using chemistry combined with magnetic or silica particles have been developed, in combination with instruments to facilitate the extraction procedure. The objective of the present study was to investigate the suitability of these automated methods for the isolation of Toxoplasma gondii DNA from amniotic fluid (AF). Therefore, three automated procedures were compared to two commercialized manual extraction methods. The MagNA Pure Compact (Roche), BioRobot EZ1 (Qiagen), and easyMAG (bioMérieux) automated procedures were compared to two manual DNA extraction kits, the QIAamp DNA minikit (Qiagen) and the High Pure PCR template preparation kit (Roche). Evaluation was carried out with two specific Toxoplasma PCRs (targeting the 529-bp repeat element), inhibitor search PCRs, and human beta-globin PCRs. The samples each consisted of 4 ml of AF with or without a calibrated Toxoplasma gondii RH strain suspension (0, 1, 2.5, 5, and 25 tachyzoites/ml). All PCR assays were laboratory-developed real-time PCR assays, using either TaqMan or fluorescent resonance energy transfer probes. A total of 1,178 PCRs were performed, including 978 Toxoplasma PCRs. The automated and manual methods were similar in sensitivity for DNA extraction from T. gondii at the highest concentration (25 Toxoplasma gondii cells/ml). However, our results showed that the DNA extraction procedures led to variable efficacy in isolating low concentrations of tachyzoites in AF samples (<5 Toxoplasma gondii cells/ml), a difference that might have repercussions since low parasite concentrations in AF exist and can lead to congenital toxoplasmosis. PMID:19846633

Validation of an updated fractionation and indirect speciation procedure for inorganic arsenic in oxic and suboxic soils and sediments.

PubMed

Lock, Alan; Wallschläger, Dirk; McMurdo, Colin; Tyler, Laura; Belzile, Nelson; Spiers, Graeme

2016-12-01

A sequential extraction procedure (SEP) for the speciation analysis of As(III) and As(V) in oxic and suboxic soils and sediments was validated using a natural lake sediment and three certified reference materials, as well as spike recoveries of As(III) and As(V). Many of the extraction steps have been previously validated making the procedure useful for comparisons to similar previous SEP studies. The novel aspect of this research is the validation for the SEP to maintain As(III) and As(V) species. The proposed five step extraction procedure includes the extraction agents (NH 4 ) 2 SO 4 , NH 4 H 2 PO 4 , H 3 PO 4  + NH 2 OH·HCl, oxalate + ascorbic acid (heated), and HNO 3  + HCl + HF, targeting operationally defined easily exchangeable, strongly sorbed, amorphous Fe oxide bound, crystalline Fe oxide bound, and residual As fractions, respectively. The third extraction step, H 3 PO 4  + NH 2 OH·HCl, has not been previously validated for fraction selectivity. We present evidence for this extraction step to target As complexed with amorphous Fe oxides when used in the SEP proposed here. All solutions were analyzed on ICP-MS. The greatest concentrations of As were extracted from the amorphous Fe oxide fraction and the dominant species was As(V). Lake sediment materials were found to have higher As(III) concentrations than the soil materials. Because different soils/sediments have different chemical characteristics, maintenance of As species during extractions must be validated for specific soil/sediment types using spiking experiments. Copyright © 2016 Elsevier Ltd. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Faye, Sherry A.; Richards, Jason M.; Gallardo, Athena M.

Sequential extraction is a useful technique for assessing the potential to leach actinides from soils; however, current literature lacks uniformity in experimental details, making direct comparison of results impossible. This work continued development toward a standardized five-step sequential extraction protocol by analyzing extraction behaviors of 232Th, 238U, 239,240Pu and 241Am from lake and ocean sediment reference materials. Results produced a standardized procedure after creating more defined reaction conditions to improve method repeatability. A NaOH fusion procedure is recommended following sequential leaching for the complete dissolution of insoluble species.

Review of procedures used for the extraction of anti-cancer compounds from tropical plants.

PubMed

Pandey, Saurabh; Shaw, Paul N; Hewavitharana, Amitha K

2015-01-01

Tropical plants are important sources of anti-cancer lead molecules. According to the US National Cancer Institute, out of the 3000 plants identified as active against cancer using in vitro studies, 70% are of tropical origin. The extraction of bioactive compounds from the plant materials is a fundamental step whose efficiency is critical for the success of drug discovery efforts. There has been no review published of the extraction procedures of anti-cancer compounds from tropical plants and hence the following is a critical evaluation of such procedures undertaken prior to the use of these compounds in cancer cell line studies, during the last five years. It presents a comprehensive analysis of all approaches taken to extract anti-cancer compounds from various tropical plants. (Databases searched were PubMed, SciFinder, Web of Knowledge, Scopus, Embase and Google Scholar).

Silybum marianum pericarp yields enhanced silymarin products.

PubMed

AbouZid, Sameh F; Chen, Shao-Nong; McAlpine, James B; Friesen, J Brent; Pauli, Guido F

2016-07-01

An improved method for the purification of silymarin, the flavonolignan complex from the fruits of milk thistle, Silybum marianum, is reported. The method enables a more efficient extraction of silymarin from the pericarp after it has been separated mechanically from the rest of the fruits. Accelerated solvent extraction (ASE) was employed for each extraction procedure. Quantitation of the eight major silymarin components in the pericarp extract was compared to that of the whole fruit extract using two orthogonal analytical methods. The pericarp extract showed higher silymarin content (2.24-fold by HPLC and 2.12-fold by qHNMR) than whole fruit extract using acetone as an extraction solvent following defatting with hexane. Furthermore, the mg/g recovery of silymarin major components was not diminished by eliminating the hexane defatting step from the pericarp extraction procedure. The efficiencies of acetone, ethanol, and methanol as extraction solvents were compared. Methanol pericarp extract showed the highest content of the silymarin major components, 2.72-fold higher than an extract prepared from the whole fruits using acetone. Finally, all of the major silymarin components showed a higher w/w content in the pericarp extract than in a commercial extract. Copyright © 2016 Elsevier B.V. All rights reserved.

A magnet built on bronchoscopic suction for extraction of tracheobronchial headscarf pins: a novel technique and review of a tertiary centre experience†

PubMed Central

Elsayed, Hany H.; Mostafa, Ahmed M.; Soliman, Saleh; El-Bawab, Hatem Y.; Moharram, Adel A.; El-Nori, Ahmed A.

2016-01-01

OBJECTIVES Airway metal pins are one of the most commonly inhaled foreign bodies in Eastern societies in young females wearing headscarves. We innovated a modified bronchoscopic technique to extract tracheobronchial headscarf pins by the insertion of a magnet to allow an easy and non-traumatic extraction of the pins. The aim of this study was to assess the feasibility and safety of our new technique and compare it with our large previous experience with the classic bronchoscopic method of extraction of tracheobronchial headscarf pins. METHODS We performed a study comparing our retrospective experience of classic bronchoscopic extraction from February 2004 to January 2014 and prospective experience with our modified technique using the magnet from January 2014 to June 2015. An institutional review board and new device approval were obtained. RESULTS Three hundred and twenty-six procedures on 315 patients were performed during our initial 10-year experience. Of them, 304 patients were females. The median age of our group was 13 (0–62). The median time from inhalation to procedure was 1 day (0–1022). After introducing our modified new technique using the magnet, 20 procedures were performed. Nineteen were females. The median time of the procedure and the need to forcefully bend the pin for extraction were in favour of the new technique in comparison with our classic approach (2 vs 6 min; P < 0.001) (2 patients = 20% vs 192 = 58%; P < 0.001). The conversion rate to surgery was also in favour of the modified technique but did not reach statistical significance (0 = 0% vs 15 = 4.8%; P = 0.32). All patients who underwent the modified technique were discharged home on the same day of the procedure. No procedural complications were recorded. All remain well on a follow-up period of up to 14 months. CONCLUSIONS Bronchoscopic extraction of tracheobronchial inhaled headscarf pins using a novel technique using homemade magnets was safer and simpler in comparison with our large experience with the classic approach. We advise the use of this device (or concept) in selected patients in centres dealing with this problem. PMID:26850113

Forensic analysis of Salvia divinorum using multivariate statistical procedures. Part I: discrimination from related Salvia species.

PubMed

Willard, Melissa A Bodnar; McGuffin, Victoria L; Smith, Ruth Waddell

2012-01-01

Salvia divinorum is a hallucinogenic herb that is internationally regulated. In this study, salvinorin A, the active compound in S. divinorum, was extracted from S. divinorum plant leaves using a 5-min extraction with dichloromethane. Four additional Salvia species (Salvia officinalis, Salvia guaranitica, Salvia splendens, and Salvia nemorosa) were extracted using this procedure, and all extracts were analyzed by gas chromatography-mass spectrometry. Differentiation of S. divinorum from other Salvia species was successful based on visual assessment of the resulting chromatograms. To provide a more objective comparison, the total ion chromatograms (TICs) were subjected to principal components analysis (PCA). Prior to PCA, the TICs were subjected to a series of data pretreatment procedures to minimize non-chemical sources of variance in the data set. Successful discrimination of S. divinorum from the other four Salvia species was possible based on visual assessment of the PCA scores plot. To provide a numerical assessment of the discrimination, a series of statistical procedures such as Euclidean distance measurement, hierarchical cluster analysis, Student's t tests, Wilcoxon rank-sum tests, and Pearson product moment correlation were also applied to the PCA scores. The statistical procedures were then compared to determine the advantages and disadvantages for forensic applications.

Extraction of polycyclic aromatic hydrocarbons and organochlorine pesticides from soils: a comparison between Soxhlet extraction, microwave-assisted extraction and accelerated solvent extraction techniques.

PubMed

Wang, Wentao; Meng, Bingjun; Lu, Xiaoxia; Liu, Yu; Tao, Shu

2007-10-29

The methods of simultaneous extraction of polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs) from soils using Soxhlet extraction, microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) were established, and the extraction efficiencies using the three methods were systemically compared from procedural blank, limits of detection and quantification, method recovery and reproducibility, method chromatogram and other factors. In addition, soils with different total organic carbon contents were used to test the extraction efficiencies of the three methods. The results showed that the values obtained in this study were comparable with the values reported by other studies. In some respects such as method recovery and reproducibility, there were no significant differences among the three methods for the extraction of PAHs and OCPs. In some respects such as procedural blank and limits of detection and quantification, there were significant differences among the three methods. Overall, ASE had the best extraction efficiency compared to MAE and Soxhlet extraction, and the extraction efficiencies of MAE and Soxhlet extraction were comparable to each other depending on the property such as TOC content of the studied soil. Considering other factors such as solvent consumption and extraction time, ASE and MAE are preferable to Soxhlet extraction.

Leaching of CCA-treated wood: implications for waste disposal.

PubMed

Townsend, Timothy; Tolaymat, Thabet; Solo-Gabriele, Helena; Dubey, Brajesh; Stook, Kristin; Wadanambi, Lakmini

2004-10-18

Leaching of arsenic, chromium, and copper from chromated copper arsenate (CCA)-treated wood poses possible environmental risk when disposed. Samples of un-weathered CCA-treated wood were tested using a variety of the US regulatory leaching procedures, including the toxicity characteristic leaching procedure (TCLP), synthetic precipitation leaching procedure (SPLP), extraction procedure toxicity method (EPTOX), waste extraction test (WET), multiple extraction procedure (MEP), and modifications of these procedures which utilized actual MSW landfill leachates, a construction and demolition (C and D) debris leachate, and a concrete enhanced leachate. Additional experiments were conducted to assess factors affecting leaching, such as particle size, pH, and leaching contact time. Results from the regulatory leaching tests provided similar results with the exception of the WET, which extracted greater quantities of metals. Experiments conducted using actual MSW leachate, C and D debris leachate, and concrete enhanced leachate provided results that were within the same order of magnitude as results obtained from TCLP, SPLP, and EPTOX. Eleven of 13 samples of CCA-treated dimensional lumber exceeded the US EPA's toxicity characteristic (TC) threshold for arsenic (5 mg/L). If un-weathered arsenic-treated wood were not otherwise excluded from the definition of hazardous waste, it frequently would require management as such. When extracted with simulated rainwater (SPLP), 9 of the 13 samples leached arsenic at concentrations above 5 mg/L. Metal leachability tended to increase with decreasing particle size and at pH extremes. All three metals leached above the drinking water standards thus possibly posing a potential risk to groundwater. Arsenic is a major concern from a disposal point of view with respect to ground water quality.

Laboratory study of the response of select insecticides to toxicity identification evaluation procedures

USGS Publications Warehouse

Kuivila, Kathryn; Crepeau, Kathryn L.

1999-01-01

A laboratory study was used to evaluate the response of select insecticides to toxicity identification evaluation procedures. Fourteen insecticides, one degradation product, and one synergist were spiked into organic-grade water and carried through toxicity identification evaluation procedures. Concentrations of each compound were analyzed by gas chromatography/mass spectrometry. During Phase I, the water sample was pumped through a C-8 solid-phase extraction cartridge and then eluted with methanol. Dimethoate was not removed by the extraction, but remained in the rinsate. In contrast, permethrin was removed by the extraction, but was not recovered by the methanol elution, and 80 percent of the permethrin remained on the cartridge, teflon tubing, and glassware. Chlorpyrifos also was not recovered completely with the methanol elution (only 62 percent was recovered). The other insecticides were extracted by C-8 solid-phase extraction cartridge and recovered by elution with methanol (80 percent or greater). During Phase II, a new spiked water sample was extracted by C-8 solid-phase extraction cartridge and then eluted with varying concentrations of methanol and water into different fractions. Each methanol:water fraction was analyzed for the added compounds. Most of the insecticides eluted in two fractions, with concentrations of 10 percent or greater. The largest number of insecticides eluted in the 75 percent methanol:water fraction.

Isolation of friedelin from black condensate of cork.

PubMed

Pires, Ricardo A; Aroso, Ivo; Silva, Susana P; Mano, João F; Reis, Rui L

2011-11-01

Black condensates (BC) are wastes of the insulation corkboard industry that contain several valuable chemicals, including friedelin, a terpene exhibiting biological activity. Herein, we report a straightforward procedure to extract friedelin from BC. Using this procedure, we were able to extract friedelin with yields between 0.4% and 2.9% and to further purify it obtaining purities from 77.0% to 99.3% (HPLC). The initial BC (2 batches), extracted raw product and purified friedelin were analyzed using FTIR. The extraction yields and purities were found to be directly related to the intensity of the carbonyl vibration at 1713 cm(-1) in the FTIR spectrum of the used BC batch. Therefore, these spectra can be used to screen and select BC batches suitable for friedelin extraction.

Determination of phthalate esters in soil using a quick, easy, cheap, effective, rugged, and safe method followed by GC-MS.

PubMed

Liu, Qianjun; Chen, Di; Wu, Jiyuan; Yin, Guangcai; Lin, Qintie; Zhang, Min; Hu, Huawen

2018-04-01

A quick, easy, cheap, effective, rugged, and safe procedure was designed to extract pesticide residues from fruits and vegetables with a high percentage of water. It has not been used extensively for the extraction of phthalate esters from sediments, soils, and sludges. In this work, this procedure was combined with gas chromatography with mass spectrometry to determine 16 selected phthalate esters in soil. The extraction efficiency of the samples was improved by ultrasonic extraction and dissolution of the soil samples in ultra-pure water, which promoted the dispersion of the samples. Furthermore, we have simplified the extraction step and reduced the risk of organic solvent contamination by minimizing the use of organic solvents. Different extraction solvents and clean-up adsorbents were compared to optimize the procedure. Dichloromethane/n-hexane (1:1, v/v) and n-hexane/acetone (1:1, v/v) were selected as the extractants from the six extraction solvents tested. C18/primary secondary amine (1:1, m/m) was selected as the sorbent from the five clean-up adsorbents tested. The recoveries from the spiked soils ranged from 70.00 to 117.90% with relative standard deviation values of 0.67-4.62%. The proposed approach was satisfactorily applied for the determination of phthalate esters in 12 contaminated soil samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Immediate esthetic crown with a facet of the extracted element

PubMed Central

Di Giacomo, Giovanni de Almeida Prado; Magalhães, Amanda; Ajzen, Sergio

2014-01-01

The present report describes a case of implant loading with an immediate temporary crown. The buccal crown surface was removed from the extracted tooth to obtain an aesthetically satisfactory result. After periodontal treatment, tooth 21 appeared proclined and showed Grade 3 mobility, indicating the need for its extraction. The remaining bone was imaged using computed tomography, and virtual surgical planning was performed using these results. The implant was immediately loaded postextraction into the fresh alveolus without a graft and flap procedure. The temporary tooth, which was manufactured using the extracted buccal surface, was a simple, fast, and low cost procedure that produced an excellent esthetic outcome. PMID:25202225

Data on DNA gel sample load, gel electrophoresis, PCR and cost analysis.

PubMed

Kuhn, Ramona; Böllmann, Jörg; Krahl, Kathrin; Bryant, Isaac Mbir; Martienssen, Marion

2018-02-01

The data presented in this article provide supporting information to the related research article "Comparison of ten different DNA extraction procedures with respect to their suitability for environmental samples" (Kuhn et al., 2017) [1]. In that article, we compared the suitability of ten selected DNA extraction methods based on DNA quality, purity, quantity and applicability to universal PCR. Here we provide the data on the specific DNA gel sample load, all unreported gel images of crude DNA and PCR results, and the complete cost analysis for all tested extraction procedures and in addition two commercial DNA extraction kits for soil and water.

Optimisation of solid-phase microextraction coupled to HPLC-UV for the determination of organochlorine pesticides and their metabolites in environmental liquid samples.

PubMed

Torres Padrón, M E; Sosa Ferrera, Z; Santana Rodríguez, J J

2006-09-01

A solid-phase microextraction (SPME) procedure using two commercial fibers coupled with high-performance liquid chromatography (HPLC) is presented for the extraction and determination of organochlorine pesticides in water samples. We have evaluated the extraction efficiency of this kind of compound using two different fibers: 60-mum polydimethylsiloxane-divinylbenzene (PDMS-DVB) and Carbowax/TPR-100 (CW/TPR). Parameters involved in the extraction and desorption procedures (e.g. extraction time, ionic strength, extraction temperature, desorption and soaking time) were studied and optimized to achieve the maximum efficiency. Results indicate that both PDMS-DVB and CW/TPR fibers are suitable for the extraction of this type of compound, and a simple calibration curve method based on simple aqueous standards can be used. All the correlation coefficients were better than 0.9950, and the RSDs ranged from 7% to 13% for 60-mum PDMS-DVB fiber and from 3% to 10% for CW/TPR fiber. Optimized procedures were applied to the determination of a mixture of six organochlorine pesticides in environmental liquid samples (sea, sewage and ground waters), employing HPLC with UV-diode array detector.

AN EVALUATION OF SAMPLE DISPERSION MEDIAS USED WITH ACCELERATED SOLVENT EXTRACTION FOR THE EXTRACTION AND RECOVERY OF ARSENICALS FROM LFB AND DORM-2

EPA Science Inventory

An accelerated solvent extraction (ASE) device was evaluated as a semi-automated means for extracting arsenicals from quality control (QC) samples and DORM-2 [standard reference material (SRM)]. Unlike conventional extraction procedures, the ASE requires that the sample be dispe...

Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.

PubMed

Carro, N; García, I; Ignacio, M-C; Llompart, M; Yebra, M-C; Mouteira, A

2002-10-01

A sample-preparation procedure (extraction and saponification) using microwave energy is proposed for determination of organochlorine pesticides in oyster samples. A Plackett-Burman factorial design has been used to optimize the microwave-assisted extraction and mild saponification on a freeze dried sample spiked with a mixture of aldrin, endrin, dieldrin, heptachlor, heptachorepoxide, isodrin, transnonachlor, p, p'-DDE, and p, p'-DDD. Six variables: solvent volume, extraction time, extraction temperature, amount of acetone (%) in the extractant solvent, amount of sample, and volume of NaOH solution were considered in the optimization process. The results show that the amount of sample is statistically significant for dieldrin, aldrin, p, p'-DDE, heptachlor, and transnonachlor and solvent volume for dieldrin, aldrin, and p, p'-DDE. The volume of NaOH solution is statistically significant for aldrin and p, p'-DDE only. Extraction temperature and extraction time seem to be the main factors determining the efficiency of extraction process for isodrin and p, p'-DDE, respectively. The optimized procedure was compared with conventional Soxhlet extraction.

Pesticide analysis in coffee leaves using a quick, easy, cheap, effective, rugged and safe approach and liquid chromatography tandem mass spectrometry: Optimization of the clean-up step.

PubMed

Trevisan, Maria Teresa Salles; Owen, Robert Wyn; Calatayud-Vernich, Pau; Breuer, Andrea; Picó, Yolanda

2017-08-25

An analytical method using a quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure for multi-residue determination of 52 pesticides in coffee leaf extractshas been developed and validated according to SANTE/11945/2015 guidelines. Different sorbent combinations for dispersive solid phase extraction (d-SPE) clean-up as well as dispersive liquid-liquid microextraction (DLLME) were tested. The relative standard deviations (RSDs) for the recovery of 87-94% of pesticides added to coffee leaf extracts,was ≤20% for samples spiked at concentrations up to 50ng*g -1 depending on the clean-up procedures. However, samples spiked with a 100ng*g -1 pesticide mixture gave RSDs>20% for most pesticides when d-SPE was carried out adding Supelclean ENVI-Carb 120/400. To explain this fact,the secondary metabolic profile was analyzed in all the extraction and clean-up procedures. Only in the clean-up procedure with the addition of Supel QuE Z-Sep+, does caffeine show a constant adsorption between blank and spiked samples. In other clean-up procedures, the amount of caffeine was higher in those samples spiked with pesticides. This indicates competition between caffeine and pesticides for adsorption to the sorbent. Addition of Supel QuE Z-Sep+ to the procedure revealed only a 32% matrix effect, whereas using PSA+ C18 the matrix effect was close to 97%. The process efficiency is up to 54% with the addition of Supel QuE Z-Sep+ and just up to 7% for the other clean-up procedures. The method was successfully tested in coffee leaves from different types of cultivars. Pesticides were not detected in organic coffee leaf extracts, but thiametoxan was clearly detected in 50% of coffee leaf extracts harvested from coffee trees grown under traditional conditions as determined by UHPLC-TOFMSLC/QqTOF-MS/MS. Copyright © 2017 Elsevier B.V. All rights reserved.

A new automated spectral feature extraction method and its application in spectral classification and defective spectra recovery

NASA Astrophysics Data System (ADS)

Wang, Ke; Guo, Ping; Luo, A.-Li

2017-03-01

Spectral feature extraction is a crucial procedure in automated spectral analysis. This procedure starts from the spectral data and produces informative and non-redundant features, facilitating the subsequent automated processing and analysis with machine-learning and data-mining techniques. In this paper, we present a new automated feature extraction method for astronomical spectra, with application in spectral classification and defective spectra recovery. The basic idea of our approach is to train a deep neural network to extract features of spectra with different levels of abstraction in different layers. The deep neural network is trained with a fast layer-wise learning algorithm in an analytical way without any iterative optimization procedure. We evaluate the performance of the proposed scheme on real-world spectral data. The results demonstrate that our method is superior regarding its comprehensive performance, and the computational cost is significantly lower than that for other methods. The proposed method can be regarded as a new valid alternative general-purpose feature extraction method for various tasks in spectral data analysis.

Critical evaluation of the ability of sequential extraction procedures to quantify discrete forms of selenium in sediments and soils.

PubMed

Wright, Michael T; Parker, David R; Amrhein, Christopher

2003-10-15

Sequential extraction procedures (SEPs) have been widely used to characterize the mobility, bioavailibility, and potential toxicity of trace elements in soils and sediments. Although oft-criticized, these methods may perform best with redox-labile elements (As, Hg, Se) for which more discrete biogeochemical phases may arise from variations in oxidation number. We critically evaluated two published SEPs for Se for their specificity and precision by applying them to four discrete components in an inert silica matrix: soluble Se(VI) (selenate), Se(IV) (selenite) adsorbed onto goethite, elemental Se, and a metal selenide (FeSe; achavalite). These were extracted both individually and in a mixed model sediment. The more selective of the two procedures was modified to further improve its selectivity (SEP 2M). Both SEP 1 and SEP 2M quantitatively recovered soluble selenate but yielded incomplete recoveries of adsorbed selenite (64% and 81%, respectively). SEP 1 utilizes 0.1 M K2S2O8 to target "organically associated" Se, but this extractant also solubilized most of the elemental (64%) and iron selenide (91%) components of the model sediment. In SEP 2M, the Na2SO3 used in step III is effective in extracting elemental Se but also extracted 17% of the Se from the iron selenide, such that the elemental fraction would be overestimated should both forms coexist. Application of SEP 2M to eight wetland sediments further suggested that the Na2SO3 in step III extracts some organically associated Se, so a NaOH extraction was inserted beforehand to yield a further modification, SEP 2OH. Results using this five-step procedure suggested that the four-step SEP 2M could overestimate elemental Se by as much as 43% due to solubilization of organic Se. Although still imperfect in its selectivity, SEP 20H may be the most suitable procedure for routine, accurate fractionation of Se in soils and sediments. However, the strong oxidant (NaOCl) used in the final step cannot distinguish between refractory organic forms of Se and pyritic Se that might form under sulfur-reducing conditions.

Bloody traditional procedures performed during infancy in the oropharyngeal area among HIV+ children: implication from the perspective of mother-to-child transmission of HIV.

PubMed

Mitke, Yifru Berhan

2010-12-01

Although bloody traditional procedures are very common in Ethiopia, this is the first report on infants. None of the literature attributed such practices as risk factor for mother-to-child transmission (MTCT) of HIV. Analysis was done to 1,163 children and found that 552 (47.5%) bloody traditional procedures were performed in the oral cavity to 399 (34.3%): uvulectomy 41.8%, milk tooth extraction 33.7% and tonsillectomy 24.5%. Multinomial logistic regression showed strong association of uvulectomy with Tigray ethnicity. Milk teeth extractions were highest among girls, rural residence, Tigray and Amhara ethnicity. When procedures performed, children were under 1 month (88.9% of tonsillectomies), under 6 months (83.5% of uvulectomies) and 4-6 months (54.3% of milk tooth extractions) of age. More than 97% for whom procedures performed were breast fed, and about 88% were from the northern part of the country. Taking into account the deep invasiveness of the procedures, they are assumed as one of the strong risk factors for MTCT of HIV during lactation.

Multineuronal vectorization is more efficient than time-segmental vectorization for information extraction from neuronal activities in the inferior temporal cortex.

PubMed

Kaneko, Hidekazu; Tamura, Hiroshi; Tate, Shunta; Kawashima, Takahiro; Suzuki, Shinya S; Fujita, Ichiro

2010-08-01

In order for patients with disabilities to control assistive devices with their own neural activity, multineuronal spike trains must be efficiently decoded because only limited computational resources can be used to generate prosthetic control signals in portable real-time applications. In this study, we compare the abilities of two vectorizing procedures (multineuronal and time-segmental) to extract information from spike trains during the same total neuron-seconds. In the multineuronal vectorizing procedure, we defined a response vector whose components represented the spike counts of one to five neurons. In the time-segmental vectorizing procedure, a response vector consisted of components representing a neuron's spike counts for one to five time-segment(s) of a response period of 1 s. Spike trains were recorded from neurons in the inferior temporal cortex of monkeys presented with visual stimuli. We examined whether the amount of information of the visual stimuli carried by these neurons differed between the two vectorizing procedures. The amount of information calculated with the multineuronal vectorizing procedure, but not the time-segmental vectorizing procedure, significantly increased with the dimensions of the response vector. We conclude that the multineuronal vectorizing procedure is superior to the time-segmental vectorizing procedure in efficiently extracting information from neuronal signals. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

Enhancing to method for extracting Social network by the relation existence

NASA Astrophysics Data System (ADS)

Elfida, Maria; Matyuso Nasution, M. K.; Sitompul, O. S.

2018-01-01

To get the trusty information about the social network extracted from the Web requires a reliable method, but for optimal resultant required the method that can overcome the complexity of information resources. This paper intends to reveal ways to overcome the constraints of social network extraction leading to high complexity by identifying relationships among social actors. By changing the treatment of the procedure used, we obtain the complexity is smaller than the previous procedure. This has also been demonstrated in an experiment by using the denial sample.

Recovery of viruses from water by a modified flocculation procedure for second-step concentration.

PubMed Central

Dahling, D R; Wright, B A

1986-01-01

A reduction in virus recovery efficiencies stemming from a change in the commercial processing of powdered beef extract was reversed by the addition of Celite analytical filter aid. Supplementing beef extract with this silicate is recommended as a modification to the organic flocculation procedure for second-step concentration in monitoring for waterborne viruses. Considerable differences in virus recovery were found among lots of beef extract and Celite preparations; this indicates that the performance of each lot of these substances should be checked before use. PMID:3015024

New approaches for extraction and determination of betaine from Beta vulgaris samples by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

PubMed

Rivoira, Luca; Studzińska, Sylwia; Szultka-Młyńska, Malgorzata; Bruzzoniti, Maria Concetta; Buszewski, Bogusław

2017-08-01

Betaine is one of most studied biologically active compounds, due its role in the main biological processes. Although it may be found in several plants and roots, such as the Beta vulgaris family, present in typical diets, just a few analytical methods have been developed for its extraction from roots. A new, quick and effective procedure for the isolation and determination of betaine from two different varieties of B. vulgaris (red and gold) is presented. For betaine extraction, an accelerated solvent extraction (ASE) was coupled with solid-phase extraction. For betaine determination, a separation method based on hydrophilic interaction chromatography coupled with tandem mass spectrometry was optimized for a sensible detection of betaine by means of experimental design. Recoveries were about 93%, with RSD <5%, for both the matrices, without evidence of interfering species. The total content of betaine in extracts of various parts of plants (juice, peel, root) have been determined, obtaining concentrations in the range 3000-4000 mg/L for the juice and in the range 2-5 mg/g for the pulp and for the peel. The B. vulgaris gold species exhibited a higher concentration of betaine, compared to the red variety. Additionally, a micro extraction by packed sorbent technique and a modified quick, easy, cheap, rugged and safe (QuEChERS) procedure, were also tested and compared. Despite the lower recoveries of the latter, with respect to the ASE/SPE procedure (75-89%, RSD <1.5%), the ease of the method, which can be applied without the SPE purification procedure, can represent a positive improvement. Graphical abstract Determination of betaine from Beta vulgaris samples.

Chemical mimicking of bio-assisted aluminium extraction by Aspergillus niger's exometabolites.

PubMed

Boriová, Katarína; Urík, Martin; Bujdoš, Marek; Pifková, Ivana; Matúš, Peter

2016-11-01

Presence of microorganisms in soils strongly affects mobility of metals. This fact is often excluded when mobile metal fraction in soil is studied using extraction procedures. Thus, the first objective of this paper was to evaluate strain Aspergillus niger's exometabolites contribution on aluminium mobilization. Fungal exudates collected in various time intervals during cultivation were analyzed and used for two-step bio-assisted extraction of alumina and gibbsite. Oxalic, citric and gluconic acids were identified in collected culture media with concentrations up to 68.4, 2.0 and 16.5 mmol L -1 , respectively. These exometabolites proved to be the most efficient agents in mobile aluminium fraction extraction with aluminium extraction efficiency reaching almost 2.2%. However, fungal cultivation is time demanding process. Therefore, the second objective was to simplify acquisition of equally efficient extracting agent by chemically mimicking composition of main organic acid components of fungal exudates. This was successfully achieved with organic acids mixture prepared according to medium composition collected on the 12th day of Aspergillus niger cultivation. This mixture extracted similar amounts of aluminium from alumina compared to culture medium. The aluminium extraction efficiency from gibbsite by organic acids mixture was lesser than 0.09% which is most likely because of more rigid mineral structure of gibbsite compared to alumina. The prepared organic acid mixture was then successfully applied for aluminium extraction from soil samples and compared to standard single step extraction techniques. This showed there is at least 2.9 times higher content of mobile aluminium fraction in soils than it was previously considered, if contribution of microbial metabolites is considered in extraction procedures. Thus, our contribution highlights the significance of fungal metabolites in aluminium extraction from environmental samples, but it also simplifies the extraction procedure inspired by bio-assisted extraction of aluminium by common soil fungus A. niger. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparison of bioavailable vanadium in alfalfa rhizosphere soil extracted by an improved BCR procedure and EDTA, HCl, and NaNO₃ single extractions in a pot experiment with V-Cd treatments.

PubMed

Yang, Jie; Teng, Yanguo; Zuo, Rui; Song, Liuting

2015-06-01

The BCR sequential extraction procedure was compared with EDTA, HCl, and NaNO3 single extractions for evaluating vanadium bioavailability in alfalfa rhizosphere soil. The amounts of vanadium extracted by these methods were in the following order: BCR (bioavailable V) > EDTA ≈ HCl > NaNO3. Both correlation analysis and stepwise regression were adopted to illustrate the extractable vanadium between different reagents. The correlation coefficients between extracted vanadium and the vanadium contents in alfalfa roots were R NaNO3 = 0.948, R HCl = 0.902, R EDTA = 0.816, and R bioavailable V = 0.819. The stepwise multiple regression equation of the NaNO3 extraction was the most significant at a 95 % confidence interval. The influence of pH, total organic carbon, and cadmium content of soil to vanadium bioavailability were not definite. In summary, both the BCR sequential extraction and the single extraction methods were valid approaches for predicting vanadium bioavailability in alfalfa rhizosphere soil, especially the single extractions.

SW-846 Test Method 3200: Mercury Species Fractionation and Quantification by Microwave Assisted Extraction, Selective Solvent Extraction and/or Solid Phase Extraction

EPA Pesticide Factsheets

a sequential extraction and separation procedure that maybe used in conjunction with a determinative method to differentiate mercury species that arepresent in soils and sediments. provides information on both total mercury andvarious mercury species.

EXTRACTION METHODS FOR RECOVERY OF VOLATILE ORGANIC COMPOUNDS FROM FORTIFIED DRY SOILS

EPA Science Inventory

Recovery of 8 volatile organic compounds (VOCs) from dry soils, each fortified at 800 ng/g soil, was studied in relation to the extraction method and time of extraction. Extraction procedures studied on desiccator-dried soils were modifications of EPA low-and high-level purge-and...

Procedure for extraction of disparate data from maps into computerized data bases

NASA Technical Reports Server (NTRS)

Junkin, B. G.

1979-01-01

A procedure is presented for extracting disparate sources of data from geographic maps and for the conversion of these data into a suitable format for processing on a computer-oriented information system. Several graphic digitizing considerations are included and related to the NASA Earth Resources Laboratory's Digitizer System. Current operating procedures for the Digitizer System are given in a simplified and logical manner. The report serves as a guide to those organizations interested in converting map-based data by using a comparable map digitizing system.

Development of a screening method for the determination of 49 priority pollutants in soil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kiang, P.H.; Grob, R.L.

1986-01-01

A screening procedure was develop for the determination of 49 priority pollutants in soil. An extraction procedure followed by the capillary gas chromatographic technique was used. Dual pH solutions with methylene chloride were used as extraction solvent system; no sample clean-up procedure was applied. Both base/neutral and acid fractions were analyzed on the same capillary column (SPB-1). The relative standard deviation for 5.1 ppm (51 ..mu..g/ 10 g) concentration in zero soil was less than 25%.

One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion.

PubMed

Tu, Xijuan; Ma, Shuangqin; Gao, Zhaosheng; Wang, Jing; Huang, Shaokang; Chen, Wenbin

2017-11-01

Flavonoids are frequently found as glycosylated derivatives in plant materials. To determine contents of flavonoid aglycones in these matrices, procedures for the extraction and hydrolysis of flavonoid glycosides are required. The current sample preparation method is both labour and time consuming. Develop a modified matrix solid phase dispersion (MSPD) procedure as an alternative methodology for the one-step extraction and hydrolysis of flavonoid glycosides. HPLC-DAD was applied for demonstrating the one-step extraction and hydrolysis of flavonoids in rape bee pollen. The obtained contents of flavonoid aglycones (quercetin, kaempferol, isorhamnetin) were used for the optimisation and validation of the method. The extraction and hydrolysis were accomplished in one step. The procedure completes in 2 h with silica gel as dispersant, a 1:2 ratio of sample to dispersant, and 60% aqueous ethanol with 0.3 M hydrochloric acid as the extraction solution. The relative standard deviations (RSDs) of repeatability were less than 5%, and the recoveries at two fortified levels were between 88.3 and 104.8%. The proposed methodology is simple and highly efficient, with good repeatability and recovery. Compared with currently available methods, the present work has advantages of using less time and labour, higher extraction efficiency, and less consumption of the acid catalyst. This method may have applications for the one-step extraction and hydrolysis of bioactive compounds from plant materials. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Optimization of a wet microalgal lipid extraction procedure for improved lipid recovery for biofuel and bioproduct production.

PubMed

Sathish, Ashik; Marlar, Tyler; Sims, Ronald C

2015-10-01

Methods to convert microalgal biomass to bio based fuels and chemicals are limited by several processing and economic hurdles. Research conducted in this study modified/optimized a previously published procedure capable of extracting transesterifiable lipids from wet algal biomass. This optimization resulted in the extraction of 77% of the total transesterifiable lipids, while reducing the amount of materials and temperature required in the procedure. In addition, characterization of side streams generated demonstrated that: (1) the C/N ratio of the residual biomass or lipid extracted (LE) biomass increased to 54.6 versus 10.1 for the original biomass, (2) the aqueous phase generated contains nitrogen, phosphorous, and carbon, and (3) the solid precipitate phase was composed of up to 11.2 wt% nitrogen (70% protein). The ability to isolate algal lipids and the possibility of utilizing generated side streams as products and/or feedstock material for downstream processes helps promote the algal biorefinery concept. Copyright © 2015 Elsevier Ltd. All rights reserved.

Utilization of optimized BCR three-step sequential and dilute HCl single extraction procedures for soil-plant metal transfer predictions in contaminated lands.

PubMed

Kubová, Jana; Matús, Peter; Bujdos, Marek; Hagarová, Ingrid; Medved', Ján

2008-05-30

The prediction of soil metal phytoavailability using the chemical extractions is a conventional approach routinely used in soil testing. The adequacy of such soil tests for this purpose is commonly assessed through a comparison of extraction results with metal contents in relevant plants. In this work, the fractions of selected risk metals (Al, As, Cd, Cu, Fe, Mn, Ni, Pb, Zn) that can be taken up by various plants were obtained by optimized BCR (Community Bureau of Reference) three-step sequential extraction procedure (SEP) and by single 0.5 mol L(-1) HCl extraction. These procedures were validated using five soil and sediment reference materials (SRM 2710, SRM 2711, CRM 483, CRM 701, SRM RTH 912) and applied to significantly different acidified soils for the fractionation of studied metals. The new indicative values of Al, Cd, Cu, Fe, Mn, P, Pb and Zn fractional concentrations for these reference materials were obtained by the dilute HCl single extraction. The influence of various soil genesis, content of essential elements (Ca, Mg, K, P) and different anthropogenic sources of acidification on extraction yields of individual risk metal fractions was investigated. The concentrations of studied elements were determined by atomic spectrometry methods (flame, graphite furnace and hydride generation atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry). It can be concluded that the data of extraction yields from first BCR SEP acid extractable step and soil-plant transfer coefficients can be applied to the prediction of qualitative mobility of selected risk metals in different soil systems.

A novel procedure for the extraction of protein deposits from soft hydrophilic contact lenses for analysis.

PubMed

Keith, D; Hong, B; Christensen, M

1997-05-01

A quick, simple, and efficient extraction technique was developed for the removal of protein from soft hydrophilic contact lenses. An extraction solvent consisting of a 50:50 mix of 0.2% trifluoroacetic acid and acetonitrile was used to remove protein from in vitro laboratory-deposited and human-worn contact lenses. The protein removed was analyzed using HPLC, bicinchoninic acid (BCA) analysis, and SDS-PAGE gel electreophoresis. Extraction efficiency for lysozyme from laboratory-deposited Group IV lenses was determined to be approximately 100%. Group IV human-worn contact lenses were extracted and analyzed for lysozyme by HPLC and total protein by bicinchoninic acid (BCA) analysis. Groups I, II, III, and IV contact lenses deposited with an artificial tear protein solution and human-worn lenses were extracted and analyzed by SDS-PAGE gel electreophoresis and micro-BCA. The ACN/TFA procedure offers a simple, quick, and efficient extraction technique for removal of protein from contact lenses for subsequent analysis.

Extraction of Oil from Flaxseed (Linum usitatissimum L.) Using Enzyme-Assisted Three-Phase Partitioning.

PubMed

Tan, Zhi-Jian; Yang, Zi-Zhen; Yi, Yong-Jian; Wang, Hong-Ying; Zhou, Wan-Lai; Li, Fen-Fang; Wang, Chao-Yun

2016-08-01

In this study, enzyme-assisted three-phase partitioning (EATPP) was used to extract oil from flaxseed. The whole procedure is composed of two parts: the enzymolysis procedure in which the flaxseed was hydrolyzed using an enzyme solution (the influencing parameters such as the type and concentration of enzyme, temperature, and pH were optimized) and three-phase partitioning (TPP), which was conducted by adding salt and t-butanol to the crude flaxseed slurry, resulting in the extraction of flaxseed oil into alcohol-rich upper phase. The concentration of t-butanol, concentration of salt, and the temperature were optimized to maximize the extraction yield. Under optimized conditions of a 49.29 % t-butanol concentration, 30.43 % ammonium sulfate concentration, and 35 °C extraction temperature, a maximum extraction yield of 71.68 % was obtained. This simple and effective EATPP can be used to achieve high extraction yields and oil quality, and thus, it is potential for large-scale oil production.

Evaluation of different extraction methods from pomegranate whole fruit or peels and the antioxidant and antiproliferative activity of the polyphenolic fraction.

PubMed

Masci, Alessandra; Coccia, Andrea; Lendaro, Eugenio; Mosca, Luciana; Paolicelli, Patrizia; Cesa, Stefania

2016-07-01

Pomegranate is a functional food of great interest, due to its multiple beneficial effects on human health. This fruit is rich in anthocyanins and ellagitannins, which exert a protective role towards degenerative diseases. The aim of the present work was to optimize the extraction procedure, from different parts of the fruit, to obtain extracts enriched in selected polyphenols while retaining biological activity. Whole fruits or peels of pomegranate cultivars, with different geographic origin, were subjected to several extraction methods. The obtained extracts were analyzed for polyphenolic content, evaluated for antioxidant capacity and tested for antiproliferative activity on human bladder cancer T24 cells. Two different extraction procedures, employing ethyl acetate as a solvent, were useful in obtaining extracts enriched in ellagic acid and/or punicalagins. Antioxidative and antiproliferative assays demonstrated that the antioxidant capability is directly related to the phenolic content, whereas the antiproliferative activity is to be mainly attributed to ellagic acid. Copyright © 2016 Elsevier Ltd. All rights reserved.

Separation and characterization of antioxidants from Spirulina platensis microalga combining pressurized liquid extraction, TLC, and HPLC-DAD.

PubMed

Jaime, Laura; Mendiola, José A; Herrero, Miguel; Soler-Rivas, Cristina; Santoyo, Susana; Señorans, F Javier; Cifuentes, Alejandro; Ibáñez, Elena

2005-11-01

A new procedure has been developed to separate and characterize antioxidant compounds from Spirulina platensis microalga based on the combination of pressurized liquid extraction (PLE) and different chromatographic procedures, such as TLC, at preparative scale, and HPLC with a diode array detector (DAD). Different solvents were tested for PLE extraction of antioxidants from S. platensis microalga. An optimized PLE process using ethanol (generally recognized as safe, GRAS) as extraction solvent has been obtained that provides natural extracts with high yields and good antioxidant properties. TLC analysis of this ethanolic extract obtained at 115 degrees C for 15 min was carried out and the silica layer was stained with a DPPH (diphenyl-pycril-hydrazyl) radical solution to determine the antioxidant activity of different chromatographic bands. Next, these colored bands were collected for their subsequent analysis by HPLC-DAD, revealing that the compounds with the most important antioxidant activity present in Spirulina extracts were carotenoids, as well as phenolic compounds and degradation products of chlorophylls.

Analysis of malondialdehyde in human plasma samples through derivatization with 2,4-dinitrophenylhydrazine by ultrasound-assisted dispersive liquid-liquid microextraction-GC-FID approach.

PubMed

Malaei, Reyhane; Ramezani, Amir M; Absalan, Ghodratollah

2018-05-04

A sensitive and reliable ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) procedure was developed and validated for extraction and analysis of malondialdehyde (MDA) as an important lipids-peroxidation biomarker in human plasma. In this methodology, to achieve an applicable extraction procedure, the whole optimization processes were performed in human plasma. To convert MDA into readily extractable species, it was derivatized to hydrazone structure-base by 2,4-dinitrophenylhydrazine (DNPH) at 40 °C within 60 min. Influences of experimental variables on the extraction process including type and volume of extraction and disperser solvents, amount of derivatization agent, temperature, pH, ionic strength, sonication and centrifugation times were evaluated. Under the optimal experimental conditions, the enhancement factor and extraction recovery were 79.8 and 95.8%, respectively. The analytical signal linearly (R 2  = 0.9988) responded over a concentration range of 5.00-4000 ng mL -1 with a limit of detection of 0.75 ng mL -1 (S/N = 3) in the plasma sample. To validate the developed procedure, the recommend guidelines of Food and Drug Administration for bioanalytical analysis have been employed. Copyright © 2018. Published by Elsevier B.V.

Evaluation of sequential extraction procedures for soluble and insoluble hexavalent chromium compounds in workplace air samples.

PubMed

Ashley, Kevin; Applegate, Gregory T; Marcy, A Dale; Drake, Pamela L; Pierce, Paul A; Carabin, Nathalie; Demange, Martine

2009-02-01

Because toxicities may differ for Cr(VI) compounds of varying solubility, some countries and organizations have promulgated different occupational exposure limits (OELs) for soluble and insoluble hexavalent chromium (Cr(VI)) compounds, and analytical methods are needed to determine these species in workplace air samples. To address this need, international standard methods ASTM D6832 and ISO 16740 have been published that describe sequential extraction techniques for soluble and insoluble Cr(VI) in samples collected from occupational settings. However, no published performance data were previously available for these Cr(VI) sequential extraction procedures. In this work, the sequential extraction methods outlined in the relevant international standards were investigated. The procedures tested involved the use of either deionized water or an ammonium sulfate/ammonium hydroxide buffer solution to target soluble Cr(VI) species. This was followed by extraction in a sodium carbonate/sodium hydroxide buffer solution to dissolve insoluble Cr(VI) compounds. Three-step sequential extraction with (1) water, (2) sulfate buffer and (3) carbonate buffer was also investigated. Sequential extractions were carried out on spiked samples of soluble, sparingly soluble and insoluble Cr(VI) compounds, and analyses were then generally carried out by using the diphenylcarbazide method. Similar experiments were performed on paint pigment samples and on airborne particulate filter samples collected from stainless steel welding. Potential interferences from soluble and insoluble Cr(III) compounds, as well as from Fe(II), were investigated. Interferences from Cr(III) species were generally absent, while the presence of Fe(II) resulted in low Cr(VI) recoveries. Two-step sequential extraction of spiked samples with (first) either water or sulfate buffer, and then carbonate buffer, yielded quantitative recoveries of soluble Cr(VI) and insoluble Cr(VI), respectively. Three-step sequential extraction gave excessively high recoveries of soluble Cr(VI), low recoveries of sparingly soluble Cr(VI), and quantitative recoveries of insoluble Cr(VI). Experiments on paint pigment samples using two-step extraction with water and carbonate buffer yielded varying percentages of relative fractions of soluble and insoluble Cr(VI). Sequential extractions of stainless steel welding fume air filter samples demonstrated the predominance of soluble Cr(VI) compounds in such samples. The performance data obtained in this work support the Cr(VI) sequential extraction procedures described in the international standards.

Relative extraction ratio (RER) for arsenic and heavy metals in soils and tailings from various metal mines, Korea.

PubMed

Son, Hye Ok; Jung, Myung Chae

2011-01-01

This study focused on the evaluation of leaching behaviours for arsenic and heavy metals (Cd, Cu, Ni, Pb and Zn) in soils and tailings contaminated by mining activities. Ten representative mine soils were taken at four representative metal mines in Korea. To evaluate the leaching characteristics of the samples, eight extraction methods were adapted namely 0.1 M HCl, 0.5 M HCl, 1.0 M HCl, 3.0 M HCl, Korean Standard Leaching Procedure for waste materials (KSLP), Synthetic Precipitation Leaching Procedure (SPLP), Toxicity Characteristic Leaching Procedure (TCLP) and aqua regia extraction (AR) methods. In order to compare element concentrations as extraction methods, relative extraction ratios (RERs, %), defined as element concentration extracted by the individual leaching method divided by that extracted by aqua regia based on USEPA method 3050B, were calculated. Although the RER values can vary upon sample types and elements, they increase with increasing ionic strength of each extracting solution. Thus, the RER for arsenic and heavy metals in the samples increased in the order of KSLP < SPLP < TCLP < 0.1 M HCl < 0.5 M HCl < 1.0 M HCl < 3.0 M HCl. In the same extraction method, the RER values for Cd and Zn were relatively higher than those for As, Cu, Ni and Pb. This may be due to differences in geochemical behaviour of each element, namely high solubility of Cd and Zn and low solubility of As, Cu, Ni and Pb in surface environment. Thus, the extraction results can give important information on the degree and extent of arsenic and heavy metal dispersion in the surface environment.

A magnet built on bronchoscopic suction for extraction of tracheobronchial headscarf pins: a novel technique and review of a tertiary centre experience.

PubMed

Elsayed, Hany H; Mostafa, Ahmed M; Soliman, Saleh; El-Bawab, Hatem Y; Moharram, Adel A; El-Nori, Ahmed A

2016-05-01

Airway metal pins are one of the most commonly inhaled foreign bodies in Eastern societies in young females wearing headscarves. We innovated a modified bronchoscopic technique to extract tracheobronchial headscarf pins by the insertion of a magnet to allow an easy and non-traumatic extraction of the pins. The aim of this study was to assess the feasibility and safety of our new technique and compare it with our large previous experience with the classic bronchoscopic method of extraction of tracheobronchial headscarf pins. We performed a study comparing our retrospective experience of classic bronchoscopic extraction from February 2004 to January 2014 and prospective experience with our modified technique using the magnet from January 2014 to June 2015. An institutional review board and new device approval were obtained. Three hundred and twenty-six procedures on 315 patients were performed during our initial 10-year experience. Of them, 304 patients were females. The median age of our group was 13 (0-62). The median time from inhalation to procedure was 1 day (0-1022). After introducing our modified new technique using the magnet, 20 procedures were performed. Nineteen were females. The median time of the procedure and the need to forcefully bend the pin for extraction were in favour of the new technique in comparison with our classic approach (2 vs 6 min; P < 0.001) (2 patients = 20% vs 192 = 58%; P < 0.001). The conversion rate to surgery was also in favour of the modified technique but did not reach statistical significance (0 = 0% vs 15 = 4.8%; P = 0.32). All patients who underwent the modified technique were discharged home on the same day of the procedure. No procedural complications were recorded. All remain well on a follow-up period of up to 14 months. Bronchoscopic extraction of tracheobronchial inhaled headscarf pins using a novel technique using homemade magnets was safer and simpler in comparison with our large experience with the classic approach. We advise the use of this device (or concept) in selected patients in centres dealing with this problem. © The Author 2016. Published by Oxford University Press on behalf of the European Association for Cardio-Thoracic Surgery. All rights reserved.

Extractive procedure for uranium determination in water samples by liquid scintillation counting.

PubMed

Gomez Escobar, V; Vera Tomé, F; Lozano, J C; Martín Sánchez, A

1998-07-01

An extractive procedure for uranium determination using liquid scintillation counting with the URAEX cocktail is described. Interference from radon and a strong influence of nitrate ion were detected in this procedure. Interference from radium, thorium and polonium emissions were very low when optimal operating conditions were reached. Quenching effects were considered and the minimum detectable activity was evaluated for different sample volumes. Isotopic analysis of samples can be performed using the proposed method. Comparisons with the results obtained with the general procedure used in alpha spectrometry with passivated implanted planar silicon detectors showed good agreement. The proposed procedure is thus suitable for uranium determination in water samples and can be considered as an alternative to the laborious conventional chemical preparations needed for alpha spectrometry methods using semiconductor detectors.

"Supermarket Column Chromatography of Leaf Pigments" Revisited: Simple and Ecofriendly Separation of Plant Carotenoids, Chlorophylls, and Flavonoids from Green and Red Leaves

ERIC Educational Resources Information Center

Dias, Alice M.; Ferreira, Maria La Salete

2015-01-01

A simple and ecofriendly procedure was developed in order to prepare extracts from red and green leaves. This procedure enables the separation of yellow, green, and red band pigments and optimizes the previously reported baking soda "supermarket column". The same extract also led to a novel and colorful potato starch column, which can…

Characterization of paprika (Capsicum annuum) extract in orange juices by liquid chromatography of carotenoid profiles.

PubMed

Mouly, P P; Gaydou, E M; Corsetti, J

1999-03-01

The carotenoid pigment profiles of authentic pure orange juices from Spain and Florida and an industrial paprika (Capsicum annuum) extract used for food coloring were obtained using reversed-phase liquid chromatography with a C18 packed column and an acetone/methanol/water eluent system. The procedure involving the carotenoid extraction is described. Both retention times and spectral properties using photodiode array detection for characterization of the major carotenoids at 430 and 519 nm are given. The influence of external addition of tangerine juice and/or paprika extract on orange juice color is described using the U.S. Department of Agriculture scale and adulterated orange juice. The procedure for quantitation of externally added paprika extract to orange juice is investigated, and the limit of quantitation, coefficient of variation, and recoveries are determined.

Hard cap espresso extraction and liquid chromatography determination of bioactive compounds in vegetables and spices.

PubMed

Martinez-Sena, María Teresa; de la Guardia, Miguel; Esteve-Turrillas, Francesc A; Armenta, Sergio

2017-12-15

A new analytical procedure, based on liquid chromatography with diode array and fluorescence detection, has been proposed for the determination of bioactive compounds in vegetables and spices after hard cap espresso extraction. This novel extraction system has been tested for the determination of capsaicin and dihydrocapsaicin from fresh chilli and sweet pepper, piperine from ground pepper, curcumin from turmeric and curry, and myristicin from nutmeg. Extraction efficiency was evaluated by using acetonitrile:water and ethanol:water mixtures. The proposed method allows the extraction of samples with 100mL of 60% (v/v) ethanol in water. The obtained limits of quantification for the proposed procedure ranged from 0.07 to 0.30mgg -1 and results were statistically comparable with those obtained by ultrasound assisted extraction. Hard cap espresso machines offer a fast, effective and quantitative tool for the extraction of bioactive compounds from food samples with an extraction time lower than 30s, using a global available and low cost equipment. Copyright © 2017 Elsevier Ltd. All rights reserved.

Metal speciation of environmental samples using SPE and SFC-AED analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mitchell, S.C.; Burford, M.D.; Robson, M.

1995-12-31

Due to growing public concern over heavy metals in the environment, soil, water and air particulate samples azre now routinely screened for their metal content. Conventional metal analysis typically involves acid digestion extraction and results in the generation of large aqueous and organic solvent waste. This harsh extraction process is usually used to obtain the total metal content of the sample, the extract being analysed by atomic emission or absorption spectroscoply techniques. A more selective method of metal extraction has been investigated which uses a supercritical fluid modified with a complexing agent. The relatively mild extraction method enables both organometallicmore » and inorganic metal species to be recovered intact. The various components from the supercritical fluid extract can be chromatographically separated using supercritical fluid chromatography (SFC) and positive identification of the metals achieved using atomic emission detection (AED). The aim of the study is to develop an analytical extraction procedure which enables a rapid, sensitive and quantitative analysis of metals in environmental samples, using just one extraction (eg SFE) and one analysis (eg SFC-AED) procedure.« less

Diversified Structural Basis of a Conserved Molecular Mechanism for pH-Dependent Dimerization in Spider Silk N-Terminal Domains.

PubMed

Otikovs, Martins; Chen, Gefei; Nordling, Kerstin; Landreh, Michael; Meng, Qing; Jörnvall, Hans; Kronqvist, Nina; Rising, Anna; Johansson, Jan; Jaudzems, Kristaps

2015-08-17

Conversion of spider silk proteins from soluble dope to insoluble fibers involves pH-dependent dimerization of the N-terminal domain (NT). This conversion is tightly regulated to prevent premature precipitation and enable rapid silk formation at the end of the duct. Three glutamic acid residues that mediate this process in the NT from Euprosthenops australis major ampullate spidroin 1 are well conserved among spidroins. However, NTs of minor ampullate spidroins from several species, including Araneus ventricosus ((Av)MiSp NT), lack one of the glutamic acids. Here we investigate the pH-dependent structural changes of (Av)MiSp NT, revealing that it uses the same mechanism but involves a non-conserved glutamic acid residue instead. Homology modeling of the structures of other MiSp NTs suggests that these harbor different compensatory residues. This indicates that, despite sequence variations, the molecular mechanism underlying pH-dependent dimerization of NT is conserved among different silk types. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Regenerative Needs Following Alveolar Ridge Preservation Procedures in Compromised and Noncompromised Extraction Sockets: A Cone Beam Computed Tomography Study.

PubMed

Koutouzis, Theofilos; Lipton, David

2016-01-01

The aim of this study was to evaluate the necessity for additional regenerative procedures following healing of compromised and noncompromised extraction sockets with alveolar ridge preservation procedures through the use of virtual implant imaging software. The cohort was comprised of 87 consecutive patients subjected to a single maxillary tooth extraction with an alveolar ridge preservation procedure for subsequent implant placement. Patients were divided into two main groups based on the integrity of the buccal bone plate following teeth extraction. Patients in the compromised socket (CS) group (n = 52) had partial or complete buccal bone plate loss, and patients in the noncompromised socket (NCS) group (n = 35) exhibited no bone loss of their socket walls following tooth extraction. Following 4 to 6 months of healing, all patients had a cone beam computed tomography (CBCT) study. Root-formed implants were placed virtually in an ideal prosthetic position. The number of implants per group and location (anterior, premolar, molar) exhibiting exposed buccal implant surface was calculated. In the CS group, 5 out of 19 anterior implants (26.3%), 4 out of 14 premolar implants (28.5%), and 7 out of 19 molar implants (36.8%) had exposed buccal surfaces. In the NCS group, 4 out of 9 anterior implants (44.4%), 2 out of 9 premolar implants (22.2%), and 4 out of 17 molar implants (23.5%) had exposed buccal surfaces. There were no statistically significant differences for intragroup and intergroup comparisons (χ² test, P > .05). This study failed to find statistically significant differences in the frequency of implants with exposed buccal surfaces placed virtually, following treatment of compromised and noncompromised sockets. A high proportion (22% to 44%) of sites had implants that potentially needed additional regenerative procedures.

Matrix effect on the determination of synthetic corticosteroids and diuretics by liquid chromatography-tandem mass spectrometry

NASA Astrophysics Data System (ADS)

Dikunets, M. A.; Appolonova, S. A.; Rodchenkov, G. M.

2009-04-01

This work presents a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) procedure for selective and reliable screening of corticosteroids and diuretics in human urine. Sample preparation included the extraction, evaporation of the organic extract under nitrogen, and solution of the dry residue. The extract was analyzed by HPLC combined with tandem mass spectrometry using electro-spraying ionization at atmospheric pressure with negative ion recording. The mass spectra of all compounds were recorded, and the characteristic ions, retention times, and detection limits were determined. The procedure was validated by evaluating the degree of the matrix suppression of ionization, extraction of analytes from human biological liquid, and the selectivity and specificity of determination.

Bioavailability of butachlor and myclobutanil residues in soil to earthworms.

PubMed

Yu, Y L; Wu, X M; Li, S N; Fang, H; Tan, Y J; Yu, J Q

2005-05-01

To establish chemical extraction procedures for predicting bioavailability of butachlor and myclobutanil in soil, several solvent systems, including methanol, methanol-water (9:1), methanol-water (1:1), acetone-water (5:3), petroleum ether and water, were assessed for their feasibility in determining extractability of the target compounds from soil samples. Experimental data showed that the extractability of butachlor and myclobutanil by the solvents was well linearly correlated with their bioavailability to Eisenia foetida and Allolobophora caliginosa, indicating that these extraction procedures may be efficient for predicting bioavailability of the two pesticides. The concentrations of the pesticides accumulated in E. foetida and A. caliginosa varied with species, suggesting that the availability of the soil-sequestered pesticide is a species-dependent process.

Extraction of Maltol from Fraser Fir: A Comparison of Microwave-Assisted Extraction and Conventional Heating Protocols for the Organic Chemistry Laboratory

ERIC Educational Resources Information Center

Koch, Andrew S.; Chimento, Clio A.; Berg, Allison N.; Mughal, Farah D.; Spencer, Jean-Paul; Hovland, Douglas E.; Mbadugha, Bessie; Hovland, Allan K.; Eller, Leah R.

2015-01-01

Two methods for the extraction of maltol from Fraser fir needles are performed and compared in this two-week experiment. A traditional benchtop extraction using dichloromethane is compared to a microwave-assisted extraction using aqueous ethanol. Students perform both procedures and weigh the merits of each technique. In doing so, students see a…

Development of a nucleic Acid extraction procedure for simultaneous recovery of DNA and RNA from diverse microbes in water.

PubMed

Hill, Vincent R; Narayanan, Jothikumar; Gallen, Rachel R; Ferdinand, Karen L; Cromeans, Theresa; Vinjé, Jan

2015-05-26

Drinking and environmental water samples contain a diverse array of constituents that can interfere with molecular testing techniques, especially when large volumes of water are concentrated to the small volumes needed for effective molecular analysis. In this study, a suite of enteric viruses, bacteria, and protozoan parasites were seeded into concentrated source water and finished drinking water samples, in order to investigate the relative performance of nucleic acid extraction techniques for molecular testing. Real-time PCR and reverse transcription-PCR crossing threshold (CT) values were used as the metrics for evaluating relative performance. Experimental results were used to develop a guanidinium isothiocyanate-based lysis buffer (UNEX buffer) that enabled effective simultaneous extraction and recovery of DNA and RNA from the suite of study microbes. Procedures for bead beating, nucleic acid purification, and PCR facilitation were also developed and integrated in the protocol. The final lysis buffer and sample preparation procedure was found to be effective for a panel of drinking water and source water concentrates when compared to commercial nucleic acid extraction kits. The UNEX buffer-based extraction protocol enabled PCR detection of six study microbes, in 100 L finished water samples from four drinking water treatment facilities, within three CT values (i.e., within 90% difference) of the reagent-grade water control. The results from this study indicate that this newly formulated lysis buffer and sample preparation procedure can be useful for standardized molecular testing of drinking and environmental waters.

Development of a Nucleic Acid Extraction Procedure for Simultaneous Recovery of DNA and RNA from Diverse Microbes in Water

PubMed Central

Hill, Vincent R.; Narayanan, Jothikumar; Gallen, Rachel R.; Ferdinand, Karen L.; Cromeans, Theresa; Vinjé, Jan

2015-01-01

Drinking and environmental water samples contain a diverse array of constituents that can interfere with molecular testing techniques, especially when large volumes of water are concentrated to the small volumes needed for effective molecular analysis. In this study, a suite of enteric viruses, bacteria, and protozoan parasites were seeded into concentrated source water and finished drinking water samples, in order to investigate the relative performance of nucleic acid extraction techniques for molecular testing. Real-time PCR and reverse transcription-PCR crossing threshold (CT) values were used as the metrics for evaluating relative performance. Experimental results were used to develop a guanidinium isothiocyanate-based lysis buffer (UNEX buffer) that enabled effective simultaneous extraction and recovery of DNA and RNA from the suite of study microbes. Procedures for bead beating, nucleic acid purification, and PCR facilitation were also developed and integrated in the protocol. The final lysis buffer and sample preparation procedure was found to be effective for a panel of drinking water and source water concentrates when compared to commercial nucleic acid extraction kits. The UNEX buffer-based extraction protocol enabled PCR detection of six study microbes, in 100 L finished water samples from four drinking water treatment facilities, within three CT values (i.e., within 90% difference) of the reagent-grade water control. The results from this study indicate that this newly formulated lysis buffer and sample preparation procedure can be useful for standardized molecular testing of drinking and environmental waters. PMID:26016775

High-Temperature Lubricant Analyses Using the System for Thermal Diagnostic Studies (STDS). A Feasibility Study

DTIC Science & Technology

1990-07-01

permeation chromatography (GPC) have been applied to lubricant type samples. 8 Most recently the newly introduced supercritical fluid chromatography (SFC... fluids , such as lubricants and hydraulic fluids can also be examined using various inverse chromatography procedures. Another mode, known as reaction...introduction of new gaseous extraction techniques, e.g., supercritical fluid extraction, procedures such as IGC will probably be developed for vastly

Development of analytical procedures for the determination of hexavalent chromium in corrosion prevention coatings used in the automotive industry.

PubMed

Séby, F; Castetbon, A; Ortega, R; Guimon, C; Niveau, F; Barrois-Oudin, N; Garraud, H; Donard, O F X

2008-05-01

The European directive 2000/53/EC limits the use of Cr(VI) in vehicle manufacturing. Although a maximum of 2 g of Cr(VI) was authorised per vehicle for corrosion prevention coatings of key components, since July 2007 its use has been prohibited except for some particular applications. Therefore, the objective of this work was to develop direct analytical procedures for Cr(VI) determination in the different steel coatings used for screws. Instead of working directly with screws, the optimisation of the procedures was carried out with metallic plates homogeneously coated to improve the data comparability. Extraction of Cr(VI) from the metallic parts was performed by sonication. Two extraction solutions were tested: a direct water extraction solution used in standard protocols and an ammonium/ammonia buffer solution at pH 8.9. The extracts were further analysed for Cr speciation by high-performance liquid chromatography (HPLC) inductively coupled plasma (ICP) atomic emission spectrometry or HPLC ICP mass spectrometry depending on the concentration level. When possible, the coatings were also directly analysed by solid speciation techniques (X-ray photoelectron spectroscopy, XPS, and X-ray absorption near-edge structure, XANES) for validation of the results. Very good results between the different analytical approaches were obtained for the sample of coating made up of a heated paint containing Zn, Al and Cr when using the extracting buffer solution at pH 8.9. After a repeated four-step extraction procedure on the same portion test, taking into account the depth of the surface layer reached, good agreement with XPS and XANES results was obtained. In contrast, for the coatings composed of an alkaline Zn layer where Cr(VI) and Cr(III) are deposited, only the extraction procedure using water allowed the detection of Cr(VI). To elucidate the Cr(VI) reduction during extraction at pH 8.9, the reactivity of Cr(VI) towards different species of Zn generally present in the coatings (metallic Zn and zinc oxide) was studied. The results showed that metallic Zn rapidly reduces Cr(VI), whereas this reaction is less evident in the presence of zinc oxide. Water was then retained for coatings containing metallic Zn.

Selenium speciation in phosphate mine soils and evaluation of a sequential extraction procedure using XAFS.

PubMed

Favorito, Jessica E; Luxton, Todd P; Eick, Matthew J; Grossl, Paul R

2017-10-01

Selenium is a trace element found in western US soils, where ingestion of Se-accumulating plants has resulted in livestock fatalities. Therefore, a reliable understanding of Se speciation and bioavailability is critical for effective mitigation. Sequential extraction procedures (SEP) are often employed to examine Se phases and speciation in contaminated soils but may be limited by experimental conditions. We examined the validity of a SEP using X-ray absorption spectroscopy (XAS) for both whole and a sequence of extracted soils. The sequence included removal of soluble, PO 4 -extractable, carbonate, amorphous Fe-oxide, crystalline Fe-oxide, organic, and residual Se forms. For whole soils, XANES analyses indicated Se(0) and Se(-II) predominated, with lower amounts of Se(IV) present, related to carbonates and Fe-oxides. Oxidized Se species were more elevated and residual/elemental Se was lower than previous SEP results from ICP-AES suggested. For soils from the SEP sequence, XANES results indicated only partial recovery of carbonate, Fe-oxide and organic Se. This suggests Se was incompletely removed during designated extractions, possibly due to lack of mineral solubilization or reagent specificity. Selenium fractions associated with Fe-oxides were reduced in amount or removed after using hydroxylamine HCl for most soils examined. XANES results indicate partial dissolution of solid-phases may occur during extraction processes. This study demonstrates why precautions should be taken to improve the validity of SEPs. Mineralogical and chemical characterizations should be completed prior to SEP implementation to identify extractable phases or mineral components that may influence extraction effectiveness. Sequential extraction procedures can be appropriately tailored for reliable quantification of speciation in contaminated soils. Copyright © 2017 Elsevier Ltd. All rights reserved.

A Metabolomic Approach Applied to a Liquid Chromatography Coupled to High-Resolution Tandem Mass Spectrometry Method (HPLC-ESI-HRMS/MS): Towards the Comprehensive Evaluation of the Chemical Composition of Cannabis Medicinal Extracts.

PubMed

Citti, Cinzia; Battisti, Umberto Maria; Braghiroli, Daniela; Ciccarella, Giuseppe; Schmid, Martin; Vandelli, Maria Angela; Cannazza, Giuseppe

2018-03-01

Cannabis sativa L. is a powerful medicinal plant and its use has recently increased for the treatment of several pathologies. Nonetheless, side effects, like dizziness and hallucinations, and long-term effects concerning memory and cognition, can occur. Most alarming is the lack of a standardised procedure to extract medicinal cannabis. Indeed, each galenical preparation has an unknown chemical composition in terms of cannabinoids and other active principles that depends on the extraction procedure. This study aims to highlight the main differences in the chemical composition of Bediol® extracts when the extraction is carried out with either ethyl alcohol or olive oil for various times (0, 60, 120 and 180 min for ethyl alcohol, and 0, 60, 90 and 120 min for olive oil). Cannabis medicinal extracts (CMEs) were analysed by liquid chromatography coupled to high-resolution tandem mass spectrometry (LC-MS/MS) using an untargeted metabolomics approach. The data sets were processed by unsupervised multivariate analysis. Our results suggested that the main difference lies in the ratio of acid to decarboxylated cannabinoids, which dramatically influences the pharmacological activity of CMEs. Minor cannabinoids, alkaloids, and amino acids contributing to this difference are also discussed. The main cannabinoids were quantified in each extract applying a recently validated LC-MS and LC-UV method. Notwithstanding the use of a standardised starting plant material, great changes are caused by different extraction procedures. The metabolomics approach is a useful tool for the evaluation of the chemical composition of cannabis extracts. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Autologous plasma rich in growth factors in the prevention of severe bleeding after teeth extractions in patients with bleeding disorders: a controlled comparison with fibrin glue

PubMed Central

Cocero, Nadia; Pucci, Fabrizio; Messina, Maria; Pollio, Berardino; Mozzati, Marco; Bergamasco, Laura

2015-01-01

Background Dental extractions in haemophiliacs may cause secondary bleeding, requiring repeated surgical and haematological interventions. As a local haemostatic, fibrin glue has recognised efficacy but, as a plasma-derived product, it carries the risk of viral infections. We, therefore, compared fibrin glue with an autologous haemostatic, plasma rich in growth factors (PRGF), in a controlled trial. Material and methods One hundred and twenty patients with different blood disorders were randomised into two cohorts to undergo dental extraction procedures without hospitalisation. Prior to the extractions, patients underwent systemic haematological treatment. Complications were defined as secondary bleeding after the 7-day follow-up period or protracting after the repair procedure. Results There were 106 extractions (7 retained 3rd molars) in the group managed with fibrin glue: secondary bleeding affected 3/60 patients (5%) on the third day after extraction and necessitated additional surgery and systemic treatment (in one case the procedure had to be repeated on the 7th day). In the PRGF arm there were 98 extractions (23 retained 3rd molars): secondary bleeding affected two patients (3.3%) on the first day after extraction and was arrested with surgery without systemic treatment. Four out of the five secondary bleeds occurred in patients with haemophilia A. Concomitant diabetes or liver disease significantly increased the bleeding risk. Discussion The bleeding rates in the study and control arm prove that PRGF works as well as fibrin glue as a local haemostatic. Further assets are that PRGF has autologous origin, does not require additional systemic treatment in post-extraction repair surgery, is associated with an earlier onset of neo-angiogenesis and, overall, can reduce patients’ distress and costs to the health system. PMID:25369587

Capillary electrophoresis for analyzing pesticides in fruits and vegetables using solid-phase extraction and stir-bar sorptive extraction.

PubMed

Juan-García, Ana; Picó, Yolanda; Font, Guillermina

2005-05-06

Two procedures based on solid-phase extraction (SPE) and stir-bar sorptive extraction (SBSE) in combination with micellar electrokinetic chromatography (MEKC)--diode array detection (DAD) were compared for the simultaneous extraction of acrinathrin, bitertanol, cyproconazole, fludioxonil, flutriafol, myclobutanil, pyriproxyfen, and tebuconazole in lettuce, tomato, grape, and strawberry. Selectivity and resolution of the MEKC procedure were studied changing the pH and the molarity of the buffer, the type and the concentration of surfactant, and the methanol content in the mobile phase. A buffer consisting of 6 mM sodium tetraborate decahydrate with 75 mM of cholic acid sodium solution (pH 9.2) gave the best results. Linearity, extraction efficiencies and limits of quantitation (LOQs) of both extraction methods were compared. The recoveries obtained by SPE ranged from 40 to 106% with relative standard deviations (R.S.D.s) from 10 to 19% whereas by the SBSE method, the recoveries were 12-47% and the R.S.D.s 3-17%. The LOQs were much better by SPE (0.2-0.5 mg kg(-1) depending on the processed sample amount) than those obtained by SBSE (1 mg kg(-1) for each compound). Advantages and disadvantages of both procedures are also discussed. As SPE is more robust, rapid, and sensitive than SBSE, its application in combination with MEKC is recommended because provided LOQs below the MRLs established, which is not always attained by SBSE.

Rapid filtration separation-based sample preparation method for Bacillus spores in powdery and environmental matrices.

PubMed

Isabel, Sandra; Boissinot, Maurice; Charlebois, Isabelle; Fauvel, Chantal M; Shi, Lu-E; Lévesque, Julie-Christine; Paquin, Amélie T; Bastien, Martine; Stewart, Gale; Leblanc, Eric; Sato, Sachiko; Bergeron, Michel G

2012-03-01

Authorities frequently need to analyze suspicious powders and other samples for biothreat agents in order to assess environmental safety. Numerous nucleic acid detection technologies have been developed to detect and identify biowarfare agents in a timely fashion. The extraction of microbial nucleic acids from a wide variety of powdery and environmental samples to obtain a quality level adequate for these technologies still remains a technical challenge. We aimed to develop a rapid and versatile method of separating bacteria from these samples and then extracting their microbial DNA. Bacillus atrophaeus subsp. globigii was used as a simulant of Bacillus anthracis. We studied the effects of a broad variety of powdery and environmental samples on PCR detection and the steps required to alleviate their interference. With a benchmark DNA extraction procedure, 17 of the 23 samples investigated interfered with bacterial lysis and/or PCR-based detection. Therefore, we developed the dual-filter method for applied recovery of microbial particles from environmental and powdery samples (DARE). The DARE procedure allows the separation of bacteria from contaminating matrices that interfere with PCR detection. This procedure required only 2 min, while the DNA extraction process lasted 7 min, for a total of <10 min. This sample preparation procedure allowed the recovery of cleaned bacterial spores and relieved detection interference caused by a wide variety of samples. Our procedure was easily completed in a laboratory facility and is amenable to field application and automation.

Rapid Filtration Separation-Based Sample Preparation Method for Bacillus Spores in Powdery and Environmental Matrices

PubMed Central

Isabel, Sandra; Boissinot, Maurice; Charlebois, Isabelle; Fauvel, Chantal M.; Shi, Lu-E; Lévesque, Julie-Christine; Paquin, Amélie T.; Bastien, Martine; Stewart, Gale; Leblanc, Éric; Sato, Sachiko

2012-01-01

Authorities frequently need to analyze suspicious powders and other samples for biothreat agents in order to assess environmental safety. Numerous nucleic acid detection technologies have been developed to detect and identify biowarfare agents in a timely fashion. The extraction of microbial nucleic acids from a wide variety of powdery and environmental samples to obtain a quality level adequate for these technologies still remains a technical challenge. We aimed to develop a rapid and versatile method of separating bacteria from these samples and then extracting their microbial DNA. Bacillus atrophaeus subsp. globigii was used as a simulant of Bacillus anthracis. We studied the effects of a broad variety of powdery and environmental samples on PCR detection and the steps required to alleviate their interference. With a benchmark DNA extraction procedure, 17 of the 23 samples investigated interfered with bacterial lysis and/or PCR-based detection. Therefore, we developed the dual-filter method for applied recovery of microbial particles from environmental and powdery samples (DARE). The DARE procedure allows the separation of bacteria from contaminating matrices that interfere with PCR detection. This procedure required only 2 min, while the DNA extraction process lasted 7 min, for a total of <10 min. This sample preparation procedure allowed the recovery of cleaned bacterial spores and relieved detection interference caused by a wide variety of samples. Our procedure was easily completed in a laboratory facility and is amenable to field application and automation. PMID:22210204

Estimation of Cadmium uptake by tobacco plants from laboratory leaching tests.

PubMed

Marković, Jelena P; Jović, Mihajlo D; Smičiklas, Ivana D; Šljivić-Ivanović, Marija Z; Smiljanić, Slavko N; Onjia, Antonije E; Popović, Aleksandar R

2018-03-21

The objective of the present study was to determine the impact of cadmium (Cd) concentration in the soil on its uptake by tobacco plants, and to compare the ability of diverse extraction procedures for determining Cd bioavailability and predicting soil-to-plant transfer and Cd plant concentrations. The pseudo-total digestion procedure, modified Tessier sequential extraction and six standard single-extraction tests for estimation of metal mobility and bioavailability were used for the leaching of Cd from a native soil, as well as samples artificially contaminated over a wide range of Cd concentrations. The results of various leaching tests were compared between each other, as well as with the amounts of Cd taken up by tobacco plants in pot experiments. In the native soil sample, most of the Cd was found in fractions not readily available under natural conditions, but with increasing pollution level, Cd amounts in readily available forms increased. With increasing concentrations of Cd in the soil, the quantity of pollutant taken up in tobacco also increased, while the transfer factor (TF) decreased. Linear and non-linear empirical models were developed for predicting the uptake of Cd by tobacco plants based on the results of selected leaching tests. The non-linear equations for ISO 14870 (diethylenetriaminepentaacetic acid extraction - DTPA), ISO/TS 21268-2 (CaCl 2 leaching procedure), US EPA 1311 (toxicity characteristic leaching procedure - TCLP) single step extractions, and the sum of the first two fractions of the sequential extraction, exhibited the best correlation with the experimentally determined concentrations of Cd in plants over the entire range of pollutant concentrations. This approach can improve and facilitate the assessment of human exposure to Cd by tobacco smoking, but may also have wider applicability in predicting soil-to-plant transfer.

Evaluation of asphalt cement extraction and recovery methods : final report.

DOT National Transportation Integrated Search

1982-07-01

This study was concerned with the quality of recovered asphalt cement which may be attributable to the method used for extraction or to the Abson recovery. Variables of these procedures such as the time an asphalt cement was exposed to extraction sol...

Chemical optimization of protein extraction from sweet potato (Ipomoea batatas) peel

USDA-ARS?s Scientific Manuscript database

Proteins isolated from sweet potatoes (Ipomoea batatas) have been shown to possess antidiabetic, antioxidant, and antiproliferative properties. The objective of this study was to chemically optimize a process for extracting proteins from sweet potato peel. The extraction procedure involved mixing pe...

Procedure for the determination of retinol and alpha-tocopherol in poultry tissues using capillary gas chromatography with solvent venting injection.

PubMed

Maraschiello, C; García Regueiro, J A

1998-08-28

A procedure designed for the determination of retinol (vitamin A) and alpha-tocopherol (vitamin E) in poultry tissues has been developed. The procedure involves lipid extraction, saponification, solid-phase clean-up and capillary gas chromatography (cGC). Retinol and alpha-tocopherol were determined separately by cGC-flame ionisation detection using a fused-silica open tubular capillary column, 30 m x 0.25 mm I.D. coated with 5% phenylmethylsilicone and with a film thickness of 0.25 micron. Solvent extraction followed by saponification were sufficient to provide a purified extract which was directly analyzed for retinol by cGC in the solvent venting mode. However, in order to accurately determine alpha-tocopherol by cGC, further purification of the extract by solid-phase extraction was necessary. A silica SPE column was used to remove interfering cholesterol from the extract. alpha-Tocopherol was analyzed in its derivatized form. Absolute and relative recoveries for both vitamins from spiked samples were evaluated. Absolute and relative recoveries ranging from 80 to 95% were obtained for both compounds. 5 alpha-Cholestane and alpha-tocopheryl acetate were used as internal standards. Poultry muscle meat and liver tissue were analyzed for their retinol and alpha-tocopherol content and the peaks detected by cGC were confirmed by cGC-mass spectrometry.

Toxic reagents and expensive equipment: are they really necessary for the extraction of good quality fungal DNA?

PubMed

Rodrigues, P; Venâncio, A; Lima, N

2018-01-01

The aim of this work was to evaluate a fungal DNA extraction procedure with the lowest inputs in terms of time as well as of expensive and toxic chemicals, but able to consistently produce genomic DNA of good quality for PCR purposes. Two types of fungal biological material were tested - mycelium and conidia - combined with two protocols for DNA extraction using Sodium Dodecyl Sulphate (SDS) and Cetyl Trimethyl Ammonium Bromide as extraction buffers and glass beads for mechanical disruption of cell walls. Our results showed that conidia and SDS buffer was the combination that lead to the best DNA quality and yield, with the lowest variation between samples. This study clearly demonstrates that it is possible to obtain high yield and pure DNA from pigmented conidia without the use of strong cell disrupting procedures and of toxic reagents. There are numerous methods for DNA extraction from fungi. Some rely on expensive commercial kits and/or equipments, unavailable for many laboratories, or make use of toxic chemicals such as chloroform, phenol and mercaptoethanol. This study clearly demonstrates that it is possible to obtain high yields of pure DNA from pigmented conidia without the use of strong and expensive cell disrupting procedures and of toxic reagents. The method herein described is simultaneously inexpensive and adequate to DNA extraction from several different types of fungi. © 2017 The Society for Applied Microbiology.

Biosafety evaluation of the DNA extraction protocol for Mycobacterium tuberculosis complex species, as implemented at the Instituto Nacional de Salud, Colombia.

PubMed

Castro, Claudia; González, Liliana; Rozo, Juan Carlos; Puerto, Gloria; Ribón, Wellman

2009-12-01

Manipulating Mycobacterium tuberculosis clinical specimens and cultures represents a risk factor for laboratory personnel. One of the processes that requires high concentrations of microorganisms is DNA extraction for molecular procedures. Pulmonary tuberculosis cases have occurred among professionals in charge of molecular procedures that require manipulation of massive quantities of microorganisms. This has prompted research studies on biosafety aspects of extraction protocols; however, as yet, no consensus has been reached regarding risks associated with the process. The biosafety was evaluated for the DNA extraction protocol of van Soolingen, et al. 2002 by determining M. tuberculosis viability at each process stage. Eight hundred eighty cultures were grown from 220 M. tuberculosis clinical isolates that had been processed through the first three DNA extraction stages. Molecular identifications of positive cultures used a PCR isolation of a fragment of the heat shock protein PRA-hsp65 and examination of its restriction enzyme profile (spoligotyping). Growth was seen in one culture with one of the procedures used. The molecular characterization did not correspond to the initially analyzed isolate, and therefore was deduced to be the product of a cross-contamination. The DNA extraction protocol, as described by van Soolingen, et al. 2002 and as implemented at the Instituto Nacional de Salud, was established to be safe for laboratory personnel as well as for the environment.

A reproducible and scalable procedure for preparing bacterial extracts for cell-free protein synthesis.

PubMed

Katsura, Kazushige; Matsuda, Takayoshi; Tomabechi, Yuri; Yonemochi, Mayumi; Hanada, Kazuharu; Ohsawa, Noboru; Sakamoto, Kensaku; Takemoto, Chie; Shirouzu, Mikako

2017-11-01

Cell-free protein synthesis is a useful method for preparing proteins for functional or structural analyses. However, batch-to-batch variability with regard to protein synthesis activity remains a problem for large-scale production of cell extract in the laboratory. To address this issue, we have developed a novel procedure for large-scale preparation of bacterial cell extract with high protein synthesis activity. The developed procedure comprises cell cultivation using a fermentor, harvesting and washing of cells by tangential flow filtration, cell disruption with high-pressure homogenizer and continuous diafiltration. By optimizing and combining these methods, ∼100 ml of the cell extract was prepared from 150 g of Escherichia coli cells. The protein synthesis activities, defined as the yield of protein per unit of absorbance at 260 nm of the cell extract, were shown to be reproducible, and the average activity of several batches was twice that obtained using a previously reported method. In addition, combinatorial use of the high-pressure homogenizer and diafiltration increased the scalability, indicating that the cell concentration at disruption varies from 0.04 to 1 g/ml. Furthermore, addition of Gam protein and examinations of the N-terminal sequence rendered the extract prepared here useful for rapid screening with linear DNA templates. © The Authors 2017. Published by Oxford University Press on behalf of the Japanese Biochemical Society. All rights reserved.

Environmentally friendly microwave-assisted sequential extraction method followed by ICP-OES and ion-chromatographic analysis for rapid determination of sulphur forms in coal samples.

PubMed

Mketo, Nomvano; Nomngongo, Philiswa N; Ngila, J Catherine

2018-05-15

A rapid three-step sequential extraction method was developed under microwave radiation followed by inductively coupled plasma-optical emission spectroscopic (ICP-OES) and ion-chromatographic (IC) analysis for the determination of sulphur forms in coal samples. The experimental conditions of the proposed microwave-assisted sequential extraction (MW-ASE) procedure were optimized by using multivariate mathematical tools. Pareto charts generated from 2 3 full factorial design showed that, extraction time has insignificant effect on the extraction of sulphur species, therefore, all the sequential extraction steps were performed for 5 min. The optimum values according to the central composite designs and counter plots of the response surface methodology were 200 °C (microwave temperature) and 0.1 g (coal amount) for all the investigated extracting reagents (H 2 O, HCl and HNO 3 ). When the optimum conditions of the proposed MW-ASE procedure were applied in coal CRMs, SARM 18 showed more organic sulphur (72%) and the other two coal CRMs (SARMs 19 and 20) were dominated by sulphide sulphur species (52-58%). The sum of the sulphur forms from the sequential extraction steps have shown consistent agreement (95-96%) with certified total sulphur values on the coal CRM certificates. This correlation, in addition to the good precision (1.7%) achieved by the proposed procedure, suggests that the sequential extraction method is reliable, accurate and reproducible. To safe-guard the destruction of pyritic and organic sulphur forms in extraction step 1, water was used instead of HCl. Additionally, the notorious acidic mixture (HCl/HNO 3 /HF) was replaced by greener reagent (H 2 O 2 ) in the last extraction step. Therefore, the proposed MW-ASE method can be applied in routine laboratories for the determination of sulphur forms in coal and coal related matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Arsenic release from Fe/Mn oxide-rich (model) soils/sediments - A comparison of single extraction procedures

NASA Astrophysics Data System (ADS)

Vanek, A.; Komarek, M.; Galuskova, I.

2012-04-01

Arsenic extractability in As-modified Fe(III) and Mn(III,IV) oxide-coated sands was tested using five widely used 2-h single extraction procedures: deionised water, 0.01 M CaCl2, 1 M NH4NO3, 0.1 M Na2HPO4 and 0.005 DTPA. In general, the highest As recoveries reaching 39-50% of total As concentration were observed for all extracting media in the birnessite (delta-MnO2) system, indicating relatively weak adsorption of As onto the Mn oxides. The Na2HPO4 extracts from the Fe oxide systems (i.e., associated with ferrihydrite and goethite) were highest in As, accounting for up to 34% of total As amount. Surprisingly, comparable recoveries of As (14-20%) yielded deionised water, CaCl2, NH4NO3, DTPA as extracting media for both ferrihydrite and goethite coatings. Deionised water and Na2HPO4 extractions are suggested for quick estimation of easily soluble, exchangeable and/or specifically adsorbed As in real soil/sediment samples.

An optimized protocol for DNA extraction in plants with a high content of secondary metabolites, based on leaves of Mimosa tenuiflora (Willd.) Poir. (Leguminosae).

PubMed

Arruda, S R; Pereira, D G; Silva-Castro, M M; Brito, M G; Waldschmidt, A M

2017-07-06

Some species are characterized by a high content of tannins, alkaloids, and phenols in their leaves. These secondary metabolites are released during DNA extraction and might hinder molecular studies based on PCR (polymerase chain reaction). To provide an efficient method to extract DNA, Mimosa tenuiflora, an important leguminous plant from Brazilian semiarid region used in popular medicine and as a source of fuelwood or forage, was used. Eight procedures previously reported for plants were tested and adapted from leaf tissues of M. tenuiflora stored at -20°C. The optimized procedure in this study encompassed the utilization of phenol during deproteinization, increased concentrations of cetyltrimethylammonium bromide and sodium chloride, and a shorter period and lower temperature of incubation concerning other methods. The extracted DNA did not present degradation, and amplification via PCR was successful using ISSR, trnL, ITS, and ETS primers. Besides M. tenuiflora, this procedure was also tested and proved to be efficient in genetic studies of other plant species.

Extraction and derivatization of polar herbicides for GC-MS analyses.

PubMed

Ranz, Andreas; Maier, Eveline; Motter, Herbert; Lankmayr, Ernst

2008-09-01

A sample preparation procedure including a simultaneous microwave-assisted (MA) extraction and derivatization for the determination of chlorophenoxy acids in soil samples is presented. For a selective and sensitive measurement, an analytical technique such as GC coupled with MS needs to be adopted. For GC analyses, chlorophenoxy acids have to be converted into more volatile and thermally stable derivatives. Derivatization by means of microwave radiation offers new alternatives in terms of shorter derivatization time and reduces susceptibility for the formation of artefacts. Extraction and derivatization into methyl esters (ME) were performed with sulphuric acid and methanol. Due to the novelty of the simultaneous extraction and derivatization assisted by means of microwave radiation, a careful investigation and optimization of influential reaction parameters was necessary. It could be shown that the combination of sulphuric acid and methanol provides a fast sample preparation including an efficient clean up procedure. The data obtained by the described method are in good agreement with those published for the reference material. Finally, compared to conventional heating and also to the standard procedure of the EPA, the sample preparation time could be considerably shortened.

Immediate Implant Placement in Single-Tooth Molar Extraction Sockets: A 1- to 6-Year Retrospective Clinical Study.

PubMed

Amato, Francesco; Polara, Giorgio

The aim of this study was to investigate the survival rate of implants immediately placed in fresh extraction sockets of molars in the maxilla and mandible with a single-stage procedure. A total of 102 patients were treated, and 107 implants (53 in the maxilla and 54 in the mandible) were placed in a fresh molar extraction socket and connected to a healing abutment. After a mean follow-up of 3 years (range: 1 to 6 years) 1 implant failed, for a cumulative success rate of 99.06% (98.11% for the mandible and 100% for the maxilla). The results of this study support placement of an implant immediately after the extraction of a molar, applying a single-stage procedure.

A rapid and simple method for estimating sulfate reduction activity and quantifying inorganic sulfides

USGS Publications Warehouse

Ulrich, G.A.; Krumholz, L.R.; Suflita, J.M.

1997-01-01

A simplified passive extraction procedure for quantifying reduced inorganic sulfur compounds from sediments and water is presented. This method may also be used for the estimation of sulfate reduction rates. Efficient extraction of FeS, FeS(inf2), and S(sup2-) was obtained with this procedure; however, the efficiency for S(sup0) depended on the form that was tested. Passive extraction can be used with samples containing up to 20 mg of reduced sulfur. We demonstrated the utility of this technique in a determination of both sulfate reduction rates and reduced inorganic sulfur pools in marine and freshwater sediments. A side-by-side comparison of the passive extraction method with the established single-step distillation technique yielded comparable results with a fraction of the effort.

Ultrasound extraction and thin layer chromatography-flame ionization detection analysis of the lipid fraction in marine mucilage samples.

PubMed

Mecozzi, M; Amici, M; Romanelli, G; Pietrantonio, E; Deluca, A

2002-07-19

This paper reports an analytical procedure based on ultrasound to extract lipids in marine mucilage samples. The experimental conditions of the ultrasound procedure (solvent and time) were identified by a FT-IR study performed on different standard samples of lipids and of a standard humic sample, before and after the sonication treatment. This study showed that diethyl ether was a more suitable solvent than methanol for the ultrasonic extraction of lipids from environmental samples because it allowed to minimize the possible oxidative modifications of lipids due to the acoustic cavitation phenomena. The optimized conditions were applied to the extraction of total lipid amount in marine mucilage samples and TLC-flame ionization detection analysis was used to identify the relevant lipid sub-fractions present in samples.

Bilateral cataract extraction with posterior chamber intraocular lens implantation simultaneous in pediatric cataracts.

PubMed

Caça, Ihsan; Sakalar, Yildirim Bayezit; Ari, Seyhmus; Alakus, Fuat; Dogan, Eyüp

2008-01-01

We evaluated the results of simultaneous bilateral cataract extraction with intraocular lens (IOL) inplantation 32 pediatric cataract patients. Simultaneous cataract extraction and posterior capsulotomy with anterior vitrectomy and IOL implantation is an effective and safe procedure in bilateral pediatric cataracts treatment.

A SIMPLE METHOD FOR THE EXTRACTION AND QUANTIFICATION OF PHOTOPIGMENTS FROM SYMBIODINIUM SPP.

EPA Science Inventory

John E. Rogers and Dragoslav Marcovich. Submitted. Simple Method for the Extraction and Quantification of Photopigments from Symbiodinium spp.. Limnol. Oceanogr. Methods. 19 p. (ERL,GB 1192).

We have developed a simple, mild extraction procedure using methanol which, when...

Environmentally friendly and cost-efficient analysis of aflatoxins in corn

USDA-ARS?s Scientific Manuscript database

The extraction procedure adds a significant cost to the overall expense of aflatoxin analysis in agricultural commodities. An inexpensive and low-waste extraction method using a household espresso coffee maker was tested. This appliance was used for the high-temperature /high-pressure extraction of ...

Rapid Training of Information Extraction with Local and Global Data Views

DTIC Science & Technology

2012-05-01

relation type extension system based on active learning a relation type extension system based on semi-supervised learning, and a crossdomain...bootstrapping system for domain adaptive named entity extraction. The active learning procedure adopts features extracted at the sentence level as the local

Comparison study of two procedures for the determination of emamectin benzoate in medicated fish feed.

PubMed

Farer, Leslie J; Hayes, John M

2005-01-01

A new method has been developed for the determination of emamectin benzoate in fish feed. The method uses a wet extraction, cleanup by solid-phase extraction, and quantitation and separation by liquid chromatography (LC). In this paper, we compare the performance of this method with that of a previously reported LC assay for the determination of emamectin benzoate in fish feed. Although similar to the previous method, the new procedure uses a different sample pretreatment, wet extraction, and quantitation method. The performance of the new method was compared with that of the previously reported method by analyses of 22 medicated feed samples from various commercial sources. A comparison of the results presented here reveals slightly lower assay values obtained with the new method. Although a paired sample t-test indicates the difference in results is significant, this difference is within the method precision of either procedure.

Supercritical fluid extraction and characterization of lipids from algae Scenedesmus obliquus

NASA Technical Reports Server (NTRS)

Choi, K. J.; Nakhost, Z.; Krukonis, V. J.; Karel, M.

1987-01-01

Lipids were extracted from a protein concentrate of green algae (Scenedesmus obliquus), using a one-step supercritical carbon dioxide extraction procedure in presence of ethanol as an entrainer, and were characterized. The compositions of neutral lipids, glycolipids, and phospholipids, separated into individual components by column, thin-layer, and gas-liquid chromatography procedures, are presented. Fatty acid composition patterns indicated that the major fatty acids were 16:0, 16:1, 16:2, 16:3, 16:4, 18:1, 18:2, and 18:3. The lipids of S. obliquus were found to contain relatively high concentrations of polyunsaturated fatty acids and essential fatty acids.

GLC analysis of poison ivy and poison oak urushiol components in vegetable oil preparations.

PubMed

Elsohly, M A; Turner, C E

1980-05-01

A procedure is described for the analysis of urushiol content of pharmaceutical preparations containing extracts of poison ivy (Toxicodendron radicans) and poison oak (T. diversilobum) in vegetable oils. The procedure involves extraction of the urushiols from the oily solutions using 90% methanol in water followed by GLC analysis of the extracts. Recoveries of both poison ivy and poison oak urushiols from solutions in corn oil, olive oil, sesame seed oil, and cottonseed oil were calculated. Correlation coefficients (r2) ranged from 0.97 to 1.00, and the coefficients of variations ranged from 3.08 to 7.90%.

Evaluating operational vacuum for landfill biogas extraction.

PubMed

Fabbricino, Massimiliano

2007-01-01

This manuscript proposes a practical methodology for estimating the operational vacuum for landfill biogas extraction from municipal landfills. The procedure is based on two sub-models which simulate landfill gas production from organic waste decomposition and distribution of gas pressure and gas movement induced by suction at a blower station. The two models are coupled in a single mass balance equation, obtaining a relationship between the operational vacuum and the amount of landfill gas that can be extracted from an assigned system of vertical wells. To better illustrate the procedure, it is applied to a case study, where a good agreement between simulated and measured data, within +/- 30%, is obtained.

A rapid and simple procedure to detect the presence of MVM in conditioned cell fluids or culture media.

PubMed

Chang, A; Havas, S; Borellini, F; Ostrove, J M; Bird, R E

1997-12-01

During the manufacture of biopharmaceuticals, numerous adventitious agents have been detected in Master Cell Banks, end-of-production cells as well as bulk harvest fluid. Recently, a number of large-scale production bioreactors have become infected with Minute Virus of Mice (MVM) during cGMP (current good manufacturing practices) operations, and this has resulted in both the loss of product and the need for major cleaning validation procedures to be put in place. We have developed a simple DNA extraction/PCR assay to detect the presence of MVM in cell culture supernatant (conditioned cell fluids). This highly specific assay can detect 10 or fewer genome equivalents (copies) of MVM following PCR and gel electrophoresis visualization. For routine high-throughput detection, 300-100 copies could be consistently detected. The extraction procedure was shown to reliably detect MVM at a concentration of 1 TCID50/ml. The combination of the extraction/PCR procedure establishes a powerful, sensitive, specific assay that can detect the presence of MVM sequences with a 1-day turnaround time.

A new procedure for extraction of collagen from modern and archaeological bones for 14C dating.

PubMed

Maspero, F; Sala, S; Fedi, M E; Martini, M; Papagni, A

2011-10-01

Bones are potentially the best age indicators in a stratigraphic study, because they are closely related to the layer in which they are found. Collagen is the most suitable fraction and is the material normally used in radiocarbon dating. Bone contaminants can strongly alter the carbon isotopic fraction values of the samples, so chemical pretreatment for (14)C dating by accelerator mass spectrometry (AMS) is essential. The most widespread method for collagen extraction is based on the Longin procedure, which consists in HCl demineralization to dissolve the inorganic phase of the samples, followed by dissolution of collagen in a weak acid solution. In this work the possible side effects of this procedure on a modern bone are presented; the extracted collagen was analyzed by ATR-IR spectroscopy. An alternative procedure, based on use of HF instead of HCl, to minimize unwanted degradation of the organic fraction, is also given. A study by ATR-IR spectroscopic analysis of collagen collected after different demineralization times and with different acid volumes, and a study of an archaeological sample, are also presented.

Effect of humidity during artificial extraction on the subsequent vigor of pine pollen

Treesearch

Russell A. Ryker

1963-01-01

Controlled pollination of pines generally has been disappointing because cones contain too few seeds. We need to develop better techniques for collecting, extracting, and storing pollen, as well as better bagging procedures. A logical first step is to learn more about collecting and extracting pollen. In a recent study I found that extracting pollen of jack pine (Pinus...

Determination of Oleanolic and Ursolic Acids in Hedyotis diffusa Using Hyphenated Ultrasound-Assisted Supercritical Carbon Dioxide Extraction and Chromatography

PubMed Central

Hong, Show-Jen

2015-01-01

Oleanolic acid (OA) and ursolic acid (UA) were extracted from Hedyotis diffusa using a hyphenated procedure of ultrasound-assisted and supercritical carbon dioxide (HSC–CO2) extraction at different temperatures, pressures, cosolvent percentages, and SC–CO2 flow rates. The results indicated that these parameters significantly affected the extraction yield. The maximal yields of OA (0.917 mg/g of dry plant) and UA (3.540 mg/g of dry plant) were obtained at a dynamic extraction time of 110 min, a static extraction time of 15 min, 28.2 MPa, and 56°C with a 12.5% (v/v) cosolvent (ethanol/water = 82/18, v/v) and SC–CO2 flowing at 2.3 mL/min (STP). The extracted yields were then analyzed by high performance liquid chromatography (HPLC) to quantify the OA and UA. The present findings revealed that H. diffusa is a potential source of OA and UA. In addition, using the hyphenated procedure for extraction is a promising and alternative process for recovering OA and UA from H. diffusa at high concentrations. PMID:26089939

Extraction of pacemaker and implantable cardioverter defibrillator leads: a single-centre study of electrosurgical and laser extraction.

PubMed

Scott, Paul A; Chow, Whitney; Ellis, Elizabeth; Morgan, John M; Roberts, Paul R

2009-11-01

Both electrosurgical dissection (EDS) and laser tools are effective in the extraction of chronic implanted endovascular leads. It is unclear which is superior. We undertook a retrospective single-centre study to assess this. In our institution from 2000 to 2004, all extractions requiring an ablative sheath were performed using the EDS system. In 2004, an excimer laser system was acquired, which became the first choice. Consecutive patients undergoing extraction requiring an ablative sheath (EDS or laser) were studied. From 2000 to 2007, 140 leads were extracted from 74 patients (EDS 31 and laser 43). Procedural success was non-significantly higher in the laser vs. the EDS group (95 vs. 87%). In the EDS group, one patient suffered tamponade requiring surgery; in the laser group, one patient suffered a significant pericardial effusion treated conservatively. There were no deaths. Procedure and fluoroscopy times were similar between groups. More patients were referred for primary surgical extraction in the EDS vs. the laser era (7 vs. 0, P = 0.003). Lead extraction using an ablative sheath is safe and effective. In our small study, there were no significant differences between EDS and laser sheaths in terms of success, time, or safety.

Reevaluation of microplastics extraction efficiency with the aim of Munich Plastic Sediment Separator.

NASA Astrophysics Data System (ADS)

Zobkov, Mikhail; Esiukova, Elena; Grave, Aleksei; Khatmullina, Liliya

2017-04-01

Invading of microplastics into marine environment is known as a global ecological threat. Specific density of microplastics can vary significantly depending on a polymer type, technological processes of its production, additives, weathering, and biofouling. Plastic particles can sink or float on the sea surface, but with time, most of drifting plastics become negatively buoyant and sink to the sea floor due to biofouling or adherence of denser particles. As a result, the seabed becomes the ultimate repository for microplastic particles and fibres. A study of microplastics content in aquatic sediments is an important source of information about ways of their migration, sink and accumulation zones. The Munich Plastic Sediment Separator (MPSS), proposed by Imhoff et al. (2012), is considered as the most effective tool for microplastic extraction. However, we observed that the numbers of marine microplastics extracted with this tool from different kinds of bottom sediments were significantly underestimated. We examined the extraction efficiency of the MPSS by adding artificial reference particles (ARPs) to marine sediment sample before the extraction procedure. Extraction was performed by two different methods: the modified NOAA method and using the MPSS. The separation solution with specific density 1.5 g/ml was used. Subsequent cleaning, drying and microscope detection procedures were identical. The microplastics content was determined in supernatant fraction, in the bulk of the extraction solution, in spoil dump fraction of MPSS and in instrument wash-out. While the extraction efficiency from natural sediments of ARPs by the MPSS was really high (100% in most cases), the extraction efficiency of marine microplastics was up to 10 times lower than that obtained with modified NOAA method for the same samples. Less than 40% of the total marine microplastics content has been successfully extracted with the MPSS. Large amounts of marine microplastics were found in the spoil dump and in the bulk solution fractions of the MPSS. Changes in stirring and separation periods had weak impact on the extraction efficiency of ARPs and marine microplastics. Until now, we are unable to find effective working procedures for adequate extraction of marine microplastics with the MPSS. The MPSS was found to be a useful tool for microplastics extraction from large sediment samples for qualitative analysis and to obtain examination specimens. Applying the MPSS for quantitative microplastics analysis requires further testing and elaboration of standardized extraction procedures. The research is supported by the Russian Science Foundation, grant number 15-17-10020 (project MARBLE). Imhof, H. K., Schmid, J., Niessner, R., Ivleva, N. P., Laforsch, C. 2012. A novel, highly efficient method for the separation and quantification of plastic particles in sediments of aquatic environments. Limnology and Oceanography: Methods, 10(7), 524-537. DOI 10.4319/lom.2012.10.524

3D spherical-cap fitting procedure for (truncated) sessile nano- and micro-droplets & -bubbles.

PubMed

Tan, Huanshu; Peng, Shuhua; Sun, Chao; Zhang, Xuehua; Lohse, Detlef

2016-11-01

In the study of nanobubbles, nanodroplets or nanolenses immobilised on a substrate, a cross-section of a spherical cap is widely applied to extract geometrical information from atomic force microscopy (AFM) topographic images. In this paper, we have developed a comprehensive 3D spherical-cap fitting procedure (3D-SCFP) to extract morphologic characteristics of complete or truncated spherical caps from AFM images. Our procedure integrates several advanced digital image analysis techniques to construct a 3D spherical-cap model, from which the geometrical parameters of the nanostructures are extracted automatically by a simple algorithm. The procedure takes into account all valid data points in the construction of the 3D spherical-cap model to achieve high fidelity in morphology analysis. We compare our 3D fitting procedure with the commonly used 2D cross-sectional profile fitting method to determine the contact angle of a complete spherical cap and a truncated spherical cap. The results from 3D-SCFP are consistent and accurate, while 2D fitting is unavoidably arbitrary in the selection of the cross-section and has a much lower number of data points on which the fitting can be based, which in addition is biased to the top of the spherical cap. We expect that the developed 3D spherical-cap fitting procedure will find many applications in imaging analysis.

Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction.

PubMed

Pena, M Teresa; Pensado, Luis; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

2007-04-01

A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 microg kg(-1) dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials.

LC-MS metabolic profiling of Arabidopsis thaliana plant leaves and cell cultures: optimization of pre-LC-MS procedure parameters.

PubMed

t'Kindt, Ruben; De Veylder, Lieven; Storme, Michael; Deforce, Dieter; Van Bocxlaer, Jan

2008-08-01

This study treats the optimization of methods for homogenizing Arabidopsis thaliana plant leaves as well as cell cultures, and extracting their metabolites for metabolomics analysis by conventional liquid chromatography electrospray ionization mass spectrometry (LC-ESI/MS). Absolute recovery, process efficiency and procedure repeatability have been compared between different pre-LC-MS homogenization/extraction procedures through the use of samples fortified before extraction with a range of representative metabolites. Hereby, the magnitude of the matrix effect observed in the ensuing LC-MS based metabolomics analysis was evaluated. Based on relative recovery and repeatability of key metabolites, comprehensiveness of extraction (number of m/z-retention time pairs) and clean-up potential of the approach (minimum matrix effects), the most appropriate sample pre-treatment was adopted. It combines liquid nitrogen homogenization for plant leaves with thermomixer based extraction using MeOH/H(2)O 80/20. As such, an efficient and highly reproducible LC-MS plant metabolomics set-up is achieved, as illustrated by the obtained results for both LC-MS (8.88%+/-5.16 versus 7.05%+/-4.45) and technical variability (12.53%+/-11.21 versus 9.31%+/-6.65) data in a comparative investigation of A. thaliana plant leaves and cell cultures, respectively.

A rapid method for the extraction and analysis of carotenoids and other hydrophobic substances suitable for systems biology studies with photosynthetic bacteria.

PubMed

Bóna-Lovász, Judit; Bóna, Aron; Ederer, Michael; Sawodny, Oliver; Ghosh, Robin

2013-10-11

A simple, rapid, and inexpensive extraction method for carotenoids and other non-polar compounds present in phototrophic bacteria has been developed. The method, which has been extensively tested on the phototrophic purple non-sulphur bacterium Rhodospirillum rubrum, is suitable for extracting large numbers of samples, which is common in systems biology studies, and yields material suitable for subsequent analysis using HPLC and mass spectroscopy. The procedure is particularly suitable for carotenoids and other terpenoids, including quinones, bacteriochlorophyll a and bacteriopheophytin a, and is also useful for the analysis of polar phospholipids. The extraction procedure requires only a single step extraction with a hexane/methanol/water mixture, followed by HPLC using a Spherisorb C18 column, with a mobile phase consisting of acetone-water and a non-linear gradient of 50%-100% acetone. The method was employed for examining the carotenoid composition observed during microaerophilic growth of R. rubrum strains, and was able to determine 18 carotenoids, 4 isoprenoid-quinones, bacteriochlorophyll a and bacteriopheophytin a as well as four different phosphatidylglycerol species of different acyl chain compositions. The analytical procedure was used to examine the dynamics of carotenoid biosynthesis in the major and minor pathways operating simultaneously in a carotenoid biosynthesis mutant of R. rubrum.

Extraction-spectrophotometric determination of tris(2-chloroethyl)amine using phthaleins.

PubMed

Rozsypal, Tomas; Halamek, Emil

2017-06-01

Procedures for the extraction-spectrophotometric determination of tris(2-chloroethyl)amine, an alkylating agent known as a drug as well as a chemical warfare agent (nitrogen mustard HN-3), with 7 acid-base indicators of a triphenylmethane lactone type, phthaleins, were developed. Representatives of phthaleins without an oxygen bridge (thymolphthalein, o-cresolphthalein, naphtholphthalein) and with an oxygen bridge (fluorescein, 2',7'-dichlorofluorescein, eosin B and eosin Y) were used. The methods were based on the formation of ion pair complexes. Chloroform was used as a non-polar solvent for an extraction. The conditions to determine were optimized for the optimal pH of the buffer and the concentration of a phthalein as a reagent. The dependence on the reaction time in a water phase and the stoichiometry of extraction products were studied. The detection limits and the limits of the determination of separate procedures and conditional extraction constants were determined. Comparison with the spectrophotometric method of the group determination of alkyl halides and acyl halides using alkaline ethanol-water solution of thymolphthalein, the so-called T-135 agent, was conducted. While studying the selectivity, the possible interference of bis(2-chloroethyl)sulphide and 3 nitrogen mustards in the proposed procedures were verified. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Features extraction in anterior and posterior cruciate ligaments analysis.

PubMed

Zarychta, P

2015-12-01

The main aim of this research is finding the feature vectors of the anterior and posterior cruciate ligaments (ACL and PCL). These feature vectors have to clearly define the ligaments structure and make it easier to diagnose them. Extraction of feature vectors is obtained by analysis of both anterior and posterior cruciate ligaments. This procedure is performed after the extraction process of both ligaments. In the first stage in order to reduce the area of analysis a region of interest including cruciate ligaments (CL) is outlined in order to reduce the area of analysis. In this case, the fuzzy C-means algorithm with median modification helping to reduce blurred edges has been implemented. After finding the region of interest (ROI), the fuzzy connectedness procedure is performed. This procedure permits to extract the anterior and posterior cruciate ligament structures. In the last stage, on the basis of the extracted anterior and posterior cruciate ligament structures, 3-dimensional models of the anterior and posterior cruciate ligament are built and the feature vectors created. This methodology has been implemented in MATLAB and tested on clinical T1-weighted magnetic resonance imaging (MRI) slices of the knee joint. The 3D display is based on the Visualization Toolkit (VTK). Copyright © 2015 Elsevier Ltd. All rights reserved.

A modal parameter extraction procedure applicable to linear time-invariant dynamic systems

NASA Technical Reports Server (NTRS)

Kurdila, A. J.; Craig, R. R., Jr.

1985-01-01

Modal analysis has emerged as a valuable tool in many phases of the engineering design process. Complex vibration and acoustic problems in new designs can often be remedied through use of the method. Moreover, the technique has been used to enhance the conceptual understanding of structures by serving to verify analytical models. A new modal parameter estimation procedure is presented. The technique is applicable to linear, time-invariant systems and accommodates multiple input excitations. In order to provide a background for the derivation of the method, some modal parameter extraction procedures currently in use are described. Key features implemented in the new technique are elaborated upon.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DRINKING WATER SAMPLES FOR ANALYSIS OF PERSISTENT ORGANIC POLLUTANTS (SOP 5.23)

EPA Science Inventory

The method for extracting and preparing a drinking water sample for analysis of atrazine is summarized in this SOP. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/ mass spectrometry.

SIMPLE METHOD FOR THE EXTRACTION OF PHOTOPIGMENTS AND MYCOSPORINE-LIKE AMINO ACIDS (MAAS) FROM SYMBIODINIUM SPP.

EPA Science Inventory

Numerous extraction methods have been developed and used in the quantitation of both photopigments and mycosporine amino acids (MAAs) found in Symbiodinium sp. and zooanthellate metazoans. We have development of a simple, mild extraction procedure using methanol, which when coupl...

Total milk fat extraction and quantification of polar and neutral lipids of cow, goat, and ewe milk by using a pressurized liquid system and chromatographic techniques.

PubMed

Castro-Gómez, M P; Rodriguez-Alcalá, L M; Calvo, M V; Romero, J; Mendiola, J A; Ibañez, E; Fontecha, J

2014-11-01

Although milk polar lipids such as phospholipids and sphingolipids located in the milk fat globule membrane constitute 0.1 to 1% of the total milk fat, those lipid fractions are gaining increasing interest because of their potential beneficial effects on human health and technological properties. In this context, the accurate quantification of the milk polar lipids is crucial for comparison of different milk species, products, or dairy treatments. Although the official International Organization for Standardization-International Dairy Federation method for milk lipid extraction gives satisfactory results for neutral lipids, it has important disadvantages in terms of polar lipid losses. Other methods using mixtures of solvents such as chloroform:methanol are highly efficient for extracting polar lipids but are also associated with low sample throughput, long time, and large solvent consumption. As an alternative, we have optimized the milk fat extraction yield by using a pressurized liquid extraction (PLE) method at different temperatures and times in comparison with those traditional lipid extraction procedures using 2:1 chloroform:methanol as a mixture of solvents. Comparison of classical extraction methods with the developed PLE procedure were carried out using raw whole milk from different species (cows, ewes, and goats) and considering fat yield, fatty acid methyl ester composition, triacylglyceride species, cholesterol content, and lipid class compositions, with special attention to polar lipids such as phospholipids and sphingolipids. The developed PLE procedure was validated for milk fat extraction and the results show that this method performs a complete or close to complete extraction of all lipid classes and in less time than the official and Folch methods. In conclusion, the PLE method optimized in this study could be an alternative to carry out milk fat extraction as a routine method. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

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.

Does Simultaneous Third Molar Extraction Increase Intraoperative and Perioperative Complications in Orthognathic Surgery?

PubMed

Steinbacher, Derek M; Kontaxis, Katrina L

2016-06-01

Prior to orthognathic surgery, most surgeons recommend third molar extraction. Espoused reasons include potential risk for infection, untoward osteotomies, and worsened postoperative discomfort. However, in addition to being another procedure for the patient, this may necessitate a longer preorthognathic surgery phase. The purpose of this study is to compare the outcomes of orthognathic surgery with staged versus simultaneous third molar extractions. This was a retrospective analysis of patients who underwent orthognathic surgery from 2013 to 2014, with at least a 1-year follow-up period. Patients were stratified into 2 groups: Extraction of third molars at the time of surgery and prior extraction of third molars. Primary outcomes included the occurrence of unfavorable splits, infection, bleeding, malocclusion, and hardware failure. Secondary outcomes were procedure time, postoperative pain, and length of stay. Pearson χ tests and 2-tailed unpaired t tests were performed to determine if there was an association between the simultaneous removal of third molars and the primary and secondary outcome measures, respectively. One hundred patients were included in the study. Forty-nine patients had third molars extracted at the time of surgery and fifty-one did not. Complications included unfavorable split, postoperative infection, mild postoperative bleeding, postoperative malocclusion, and hardware failure. There was no significant difference in the incidence of complications in both groups. Procedure time was not considerably increased with extractions. There was no significant difference in postoperative pain or length of stay between both groups. Removing third molars concurrently with orthognathic surgery does not increase the risk of adverse outcomes, nor does it significantly influence hospital course.

An approach of ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergistic extraction for two coumarins preparation from Cortex fraxini.

PubMed

Liu, Zaizhi; Gu, Huiyan; Yang, Lei

2015-10-23

Ionic liquids/lithium salts solvent system was successfully introduced into the separation technique for the preparation of two coumarins (aesculin and aesculetin) from Cortex fraxini. Ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergy extraction (ILSMP-UMSE) procedure was developed and optimized for the sufficient extraction of these two analytes. Several variables which can potentially influence the extraction yields, including pretreatment time and temperature, [C4mim]Br concentration, LiAc content, ultrasound-microwave synergy extraction (UMSE) time, liquid-solid ratio, and UMSE power were optimized by Plackett-Burman design. Among seven variables, UMSE time, liquid-solid ratio, and UMSE power were the statistically significant variables and these three factors were further optimized by Box-Behnken design to predict optimal extraction conditions and find out operability ranges with maximum extraction yields. Under optimum operating conditions, ILSMP-UMSE showed higher extraction yields of two target compounds than those obtained by reference extraction solvents. Method validation studies also evidenced that ILSMP-UMSE is credible for the preparation of two coumarins from Cortex fraxini. This study is indicative of the proposed procedure that has huge application prospects for the preparation of natural products from plant materials. Copyright © 2015 Elsevier B.V. All rights reserved.

Evaluation of new natural deep eutectic solvents for the extraction of isoflavones from soy products.

PubMed

Bajkacz, Sylwia; Adamek, Jakub

2017-06-01

Natural deep eutectic solvents (NADESs) are considered to be new, safe solvents in green chemistry that can be widely used in many chemical processes such as extraction or synthesis. In this study, a simple extraction method based on NADES was used for the isolation of isoflavones (daidzin, genistin, genistein, daidzein) from soy products. Seventeen different NADES systems each including two or three components were tested. Multivariate data analysis revealed that NADES based on a 30% solution of choline chloride: citric acid (molar ratio of 1:1) are the most effective systems for the extraction of isoflavones from soy products. After extraction, the analytes were detected and quantified using ultra-high performance liquid chromatography with ultraviolet detection (UHPLC-UV). The proposed NADES extraction procedure achieved enrichment factors up to 598 for isoflavones and the recoveries of the analytes were in the range 64.7-99.2%. The developed NADES extraction procedure and UHPLC-UV determination method was successfully applied for the analysis of isoflavones in soy-containing food samples. The obtained results indicated that new natural deep eutectic solvents could be an alternative to traditional solvents for the extraction of isoflavones and can be used as sustainable and safe extraction media for another applications. Copyright © 2017 Elsevier B.V. All rights reserved.

[Preparation procedures of anti-complementary polysaccharides from Houttuynia cordata].

PubMed

Zhang, Juanjuan; Lu, Yan; Chen, Daofeng

2012-07-01

To establish and optimize the preparation procedures of the anti-complementary polysaccharides from Houttuynia cordata. Based on the yield and anti-complementary activity in vitro, the conditions of extraction and alcohol precipitating process were optimized by orthogonal tests. The optimal condition of deproteinization was determined according to the results of protein removed and polysaccharide maintained. The best decoloring method was also optimized by orthogonal experimental design. The optimized preparation procedures were given as follows: extract the coarse powder 3 times with 50 times volume of water at 90 degrees C for 2 hours every time, combine the extracts and concentrate appropriately, equivalent to 0.12 g of H. cordata per milliliter. Add 4 times volume of 90% ethanol to the extract, allow to stand for 24 hours to precipitate totally, filter and the precipitate was successfully washed with anhydrous alcohol, acetone and anhydrous ether. Resolve the residue with water, add trichloroacetic acid (TCA) to a concentration of 20% to remove protein. Decoloration was at a concentration of 3% with activated carbon at pH 3.0, 50 degrees C for 50 min. The above procedures above were tested 3 times, resulting in the average yield of polysaccharides at 4.03% (RSD 0.96%), the average concentrations of polysaccharides and protein at 80.97% (RSD 1.5%) and 2.02% (RSD 2.3%), and average CH50 at 0.079 g x L-(-1) (RSD 3.6%). The established and optimized procedures are repeatable and reliable to prepare the anti-complementary polysaccharides with high quality and activity from H. cordata.

The influence of extraction procedure on ion concentrations in sediment pore water

USGS Publications Warehouse

Winger, P.V.; Lasier, P.J.; Jackson, B.P.

1998-01-01

Sediment pore water has the potential to yield important information on sediment quality, but the influence of isolation procedures on the chemistry and toxicity are not completely known and consensus on methods used for the isolation from sediment has not been reached. To provide additional insight into the influence of collection procedures on pore water chemistry, anion (filtered only) and cation concentrations were measured in filtered and unfiltered pore water isolated from four sediments using three different procedures: dialysis, centrifugation and vacuum. Peepers were constructed using 24-cell culture plates and cellulose membranes, and vacuum extractors consisted of fused-glass air stones attached with airline tubing to 60cc syringes. Centrifugation was accomplished at two speeds (2,500 and 10,000 x g) for 30 min in a refrigerated centrifuge maintained at 4?C. Only minor differences in chemical characteristics and cation and anion concentrations were found among the different collecting methods with differences being sediment specific. Filtering of the pore water did not appreciably reduce major cation concentrations, but trace metals (Cu and Pb) were markedly reduced. Although the extraction methods evaluated produced pore waters of similar chemistries, the vacuum extractor provided the following advantages over the other methods: (1) ease of extraction, (2) volumes of pore water isolated, (3) minimal preparation time and (4) least time required for extraction of pore water from multiple samples at one time.

40 CFR 91.415 - Raw gaseous sampling procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 20 2010-07-01 2010-07-01 false Raw gaseous sampling procedures. 91.415 Section 91.415 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS... Raw gaseous sampling procedures. Fit all heated sampling lines with a heated filter to extract solid...

40 CFR 91.415 - Raw gaseous sampling procedures.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 20 2011-07-01 2011-07-01 false Raw gaseous sampling procedures. 91.415 Section 91.415 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS... Raw gaseous sampling procedures. Fit all heated sampling lines with a heated filter to extract solid...

Rapid recovery of high content phytosterols from corn silk.

PubMed

Zhang, Haiyan; Cao, Xiaowan; Liu, Yong; Shang, Fude

2017-10-18

Phytosterols have important physiological and officinal function. An efficient ultrasonic assisted extraction, purification and crystallization procedure of phytosterols was established from corn silk for the first time. The orthogonal test was applied to optimize the process parameters and a maximum phytosterols recovery as high as 10.5886 mg/g was achieved by ultrasonic treatment for 55 min with liquid-solid ratio of 12:1 at 35 °C, 220 w. The ultrasonic extraction temperature (T, °C) has the most significant effect on extraction yield of phytosterols. An orthogonal crystallization test was performed and the optimal conditions [crystallization temperature of 8 °C, time of 12 h and solid-liquid ratio of 1:1 (g/ml)] afforded maximum phytosterols purity of 92.76 ± 0.43%. An efficient extraction and crystallization procedure was established.

Extraction of intracellular protein from Glaciozyma antarctica for proteomics analysis

NASA Astrophysics Data System (ADS)

Faizura, S. Nor; Farahayu, K.; Faizal, A. B. Mohd; Asmahani, A. A. S.; Amir, R.; Nazalan, N.; Diba, A. B. Farah; Muhammad, M. Nor; Munir, A. M. Abdul

2013-11-01

Two preparation methods of crude extracts of psychrophilic yeast Glaciozyma antarctica were compared in order to obtain a good recovery of intracellular proteins. Extraction with mechanical procedures using sonication was found to be more effective for obtaining good yield compare to alkaline treatment method. The procedure is simple, rapid, and produce better yield. A total of 52 proteins were identified by combining both extraction methods. Most of the proteins identified in this study involves in the metabolic process including glycolysis pathway, pentose phosphate pathway, pyruyate decarboxylation and also urea cyle. Several chaperons were identified including probable cpr1-cyclophilin (peptidylprolyl isomerase), macrolide-binding protein fkbp12 and heat shock proteins which were postulate to accelerate proper protein folding. Characteristic of the fundamental cellular processes inferred from the expressed-proteome highlight the evolutionary and functional complexity existing in this domain of life.

Rapid metal extractability tests from polluted mining soils by ultrasound probe sonication and microwave-assisted extraction systems.

PubMed

García-Salgado, Sara; Quijano, M Ángeles

2016-12-01

Ultrasonic probe sonication (UPS) and microwave-assisted extraction (MAE) were used for rapid single extraction of Cd, Cr, Cu, Ni, Pb, and Zn from soils polluted by former mining activities (Mónica Mine, Bustarviejo, NW Madrid, Spain), using 0.01 mol L -1 calcium chloride (CaCl 2 ), 0.43 mol L -1 acetic acid (CH 3 COOH), and 0.05 mol L -1 ethylenediaminetetraacetic acid (EDTA) at pH 7 as extracting agents. The optimum extraction conditions by UPS consisted of an extraction time of 2 min for both CaCl 2 and EDTA extractions and 15 min for CH 3 COOH extraction, at 30% ultrasound (US) amplitude, whereas in the case of MAE, they consisted of 5 min at 50 °C for both CaCl 2 and EDTA extractions and 15 min at 120 °C for CH 3 COOH extraction. Extractable concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The proposed methods were compared with a reduced version of the corresponding single extraction procedures proposed by the Standards, Measurements and Testing Programme (SM&T). The results obtained showed a great variability on extraction percentages, depending on the metal, the total concentration level and the soil sample, reaching high values in some areas. However, the correlation analysis showed that total concentration is the most relevant factor for element extractability in these soil samples. From the results obtained, the application of the accelerated extraction procedures, such as MAE and UPS, could be considered a useful approach to evaluate rapidly the extractability of the metals studied.

Comparisons between conventional, ultrasound-assisted and microwave-assisted methods for extraction of anthraquinones from Heterophyllaea pustulata Hook f. (Rubiaceae).

PubMed

Barrera Vázquez, M F; Comini, L R; Martini, R E; Núñez Montoya, S C; Bottini, S; Cabrera, J L

2014-03-01

This work reports a comparative study about extraction methods used to obtain anthraquinones (AQs) from stems and leaves of Heterophyllae pustulata Hook (Rubiáceae). One of the conventional procedures used to extract these metabolites from a vegetable matrix is by successive Soxhlet extractions with solvents of increasing polarity: starting with hexane to eliminate chlorophylls and fatty components, following by benzene and finally ethyl acetate. However, this technique shows a low extraction yield of total AQs, and consumes large quantities of solvent and time. Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) have been investigated as alternative methods to extract these compounds, using the same sequence of solvents. It was found that UAE increases the extraction yield of total AQs and reduces the time and amount of solvent used. Nevertheless, the combination UAE with benzene, plus MAE with ethyl acetate at a constant power of 900 W showed the best results. A higher yield of total AQs was obtained in less time and using the same amount of solvent that UAE. The optimal conditions for this latter procedure were UAE with benzene at 50 °C during 60 min, followed by MAE at 900 W during 15 min using ethyl acetate as extraction solvent. Copyright © 2013 Elsevier B.V. All rights reserved.

Supercritical fluid extraction of 11C-labeled metabolites in tissue using supercritical ammonia.

PubMed

Jacobson, G B; Moulder, R; Lu, L; Bergström, M; Markides, K E; Långström, B

1997-02-01

Supercritical fluid extraction (SFE) of 11C-labeled tracer compounds and their metabolites from biological tissue was performed using supercritical ammonia in an attempt to develop a rapid extraction procedure that allowed subsequent analysis of the labeled metabolites. Metabolites were extracted from kidneys and brain in rats given in vivo injections of the radiotracers O-[2-11C]acetyl-L-carnitine and N-[11C]methylpiperidyl benzilate, respectively. Only a minimal sample pretreatment of the tissue was necessary, i.e., cutting into 10-20 pieces and mixing with the drying agent Hydromatrix, before it was loaded into the extraction vessel. Extraction efficiency was measured for SFE at temperatures over the range of 70-150 degrees C and a pressure of 400 bar. For O-[2-11C]acetyl-L-carnitine, 66% of the radioactivity was trapped in the collected fractions and 12% remained in the extraction vessel. For the more lipophilic N-[11C]methylpiperidyl benzilate, 93% of the activity was collected and less than 1% remained in the extraction vessel. Labeled metabolites were analyzed by LC and also, in the case, of O-[2-11C]acetyl-L-carnitine by LC/MS. The complete extraction procedure, from removal of the biological tissue until an extract was ready for analysis, was 25 min, corresponding to about one half-life of the radionuclide 11C.

Long-term study of volatile organic compound recovery from ampulated, dry, fortified soils

DOE Office of Scientific and Technical Information (OSTI.GOV)

Minnich, M.M.; Zimmerman, J.H.; Schumacher, B.A.

1997-01-01

Our objective was to evaluate the stability and extractability of volatile organic compounds (VOCs) when fortified on dry soils and stored in sealed ampules. Two desiccator-dried soils were fortified with benzene, toluene, ethylbenzene, o-xylene, 1,1,1-trichloroethane (TCA), trichloroethene (TCE), tetrachloroethene (PCE), and 1,1,2,2-tetrachloroethane (TTCA) at 800 ng each VOC/g soil. The fortified soil was portioned into ampules, sealed, and stored in the dark at 25{degrees}C for up to 56 wk. Replicate ampules were analyzed after 2 d and 2,4,8,13,34, and 56 wk by two extraction procedures modified from the US Environmental Protection Agency`s (USEPA`s) low- and high-level purge-and-trap procedures (SW-846 Methodsmore » 5030/8021). The modified procedure (1-h methanol extraction at 25{degree}C prior to purge-and-trap analysis) yielded significantly higher recoveries of all compounds on both soils as compared with the low-level procedure, with the exception of benzene on the Charleston soil. Moreover, when measured by the high-level procedure, concentrations of benzene, toluene, ethylbenzene, and o-xylene (BTEX) remained relatively unchanged during the 56-wk study. Results indicate that the 1-h, 25{degrees}C methanol extraction was sufficient for extraction of the BTEX compounds from these soils. For the chlorinated compounds, regression analysis demonstrated significant trends of changing concentrations over time. Recoveries of TCA decreased at a rate of 3 and 4 ng/g/week and recoveries of TTCA decreased at rates of 8 and 17 ng/g/week on the Hayesville and Charleston soils, respectively. PCE concentrations did not show any significant concentration changes, while TCE concentrations increased at 6 and 7 ng/g/week for the Hayesville and Charleston soils, respectively. 19 refs., 2 figs., 5 tabs.« less

Co-evaluation of plant extracts as petrochemical substitutes and for biologically active compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

McChesney, J.D.; Adams, R.P.

Recent efforts to discover phytochemicals that could substitute for petroleum-derived fuels and industrial feedstocks have not given much attention to the potential of these same phytochemicals to provide sources of biologically active compounds. The suitability of extraction products made to assess specific plants as potential botanochemical sources has been evaluated for use in screening procedures for evidence of biologically active compounds. Screening procedures for antibacterial, antifungal and toxic properties are discussed. Screening results are presented for extracts of nearly 80 species of plants from the southeastern United States and southern Great Plains that had previously been evaluated as sources ofmore » botanochemicals.« less

EXTRACTION AND PHYSICO-CHEMICAL STUDIES OF DIASTASE-LIKE ENZYME FROM PIPER BETLE PETIOLES: PART 1

PubMed Central

Ramasarma, G.V.S; Dutta, Sadhan Kumar

1995-01-01

Petioles of the plant piper betle-bengal variety have been subjected for extraction employing standard procedure and the crude extract obtained has been evaluated for its diastase like activity and other physico-chemical properties to investigate further its possible biological and pharmacological activities. PMID:22556729

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SOLID FOOD SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.28)

EPA Science Inventory

This SOP describes the extraction and preparation of a solid food sample for analysis of acidic persistent organic pollutants such as acid herbicides, pentachlorphenol, and 3,5,6-trichloro-2-phenol. It covers the extraction, concentration and derivatization of samples that are to...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DUST AND SOIL SAMPLES FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.14)

EPA Science Inventory

This SOP summarizes the method for extracting and preparing a dust or soil sample for analysis of neutral persistent organic pollutants. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass spectrometry.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DERMAL WIPE SAMPLES FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.16)

EPA Science Inventory

The method for extracting and preparing a dermal (hand) wipe sample for analysis of neutral persistent organic pollutants is summarized in this SOP. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass spectrometry.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING LIQUID FOOD SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.29)

EPA Science Inventory

This SOP describes the extraction and preparation of a liquid food sample for analysis of acidic persistent organic pollutants such as acid herbicides, pentachlorphenol, and 3,5,6-trichloro-2-phenol. It covers the extraction, concentration and derivatization of samples that are t...

Sensibility and taste alterations after impacted lower third molar extractions. A prospective cohort study

PubMed Central

Ridaura-Ruiz, Lourdes; Valmaseda-Castellón, Eduard; Berini-Aytés, Leonardo; Gay-Escoda, Cosme

2012-01-01

Objectives: To determine the incidence, severity and duration of lingual tactile and gustatory function impairments after lower third molar removal. Study Design: Prospective cohort study with intra-subject measures of 16 patients undergoing lower third molar extractions. Sensibility and gustatory functions were evaluated in each subject preoperatively, one week and one month after the extraction, using Semmes-Weinstein monofilaments and 5 different concentrations of NaCl, respectively. Additionally, all patients filled a questionnaire to assess subjective perceptions. Results: Although patients did not perceive any sensibility impairments, a statistically significant decrease was detected when Semmes-Weinstein monofilaments. This alteration was present at one week after the surgical procedure and fully recovered one month after the extraction. There were no variations regarding the gustatory function. Conclusions: Lower third molar removal under local anesthesia may cause light lingual sensibility impairment. Most of these alterations remain undetected to patients. These lingual nerve injuries are present one week after the extraction and recover one month after surgery. The taste seems to remain unaffected after these procedures. Key words:Lingual nerve, third molar, nerve injury, paresthesia, surgical extraction PMID:22322520

Determination of ethyl glucuronide in hair: a rapid sample pretreatment involving simultaneous milling and extraction.

PubMed

Mönch, Bettina; Becker, Roland; Nehls, Irene

2014-01-01

A combination of simultaneous milling and extraction known as micropulverized extraction was developed for the quantification of the alcohol marker ethyl glucuronide (EtG) in hair samples using a homogeneous reference material and a mixer mill. Best extraction results from 50 mg of hair were obtained with 2-mL plastic tubes containing two steel balls (∅ = 5 mm), 0.5 mL of water and with an oscillating frequency of 30 s(-1) over a period of 30 min. EtG was quantified employing a validated GC-MS procedure involving derivatization with pentafluoropropionic acid anhydride. This micropulverization procedure was compared with dry milling followed by separate aqueous extraction and with aqueous extraction after manual cutting to millimeter-size snippets. Micropulverization yielded 28.0 ± 1.70 pg/mg and was seen to be superior to manually cutting (23.0 ± 0.83 pg/mg) and equivalent to dry grinding (27.7 ± 1.71 pg/mg) with regard to completeness of EtG extraction. The option to process up to 20 samples simultaneously makes micropulverization especially valuable for the high throughput of urgent samples.

Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water.

PubMed

Tobiszewski, Marek; Orłowski, Aleksander

2015-03-27

The study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists--decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as an example) were selected as input alternatives to MCDA analysis. Nine different criteria describing the alternatives were chosen from different groups--metrological, economical and the most importantly--environmental impact. The weights for each criterion were obtained from questionnaires that were sent to experts, giving three different scenarios for MCDA results. The results of analysis show that PROMETHEE is very promising tool to choose the analytical procedure with respect to its greenness. The rankings for all three scenarios placed solid phase microextraction and liquid phase microextraction--based procedures high, while liquid-liquid extraction, solid phase extraction and stir bar sorptive extraction--based procedures were placed low in the ranking. The results show that although some of the experts do not intentionally choose green analytical chemistry procedures, their MCDA choice is in accordance with green chemistry principles. The PROMETHEE ranking results were compared with more widely accepted green analytical chemistry tools--NEMI and Eco-Scale. As PROMETHEE involved more different factors than NEMI, the assessment results were only weakly correlated. Oppositely, the results of Eco-Scale assessment were well-correlated as both methodologies involved similar criteria of assessment. Copyright © 2015 Elsevier B.V. All rights reserved.

A novel technique of percutaneous stone extraction in choledocholithiasis after cholecystostomy.

PubMed

Lim, Kyoung Hoon; Kim, Yong Joo

2013-05-01

To evaluate the technical feasibility and clinical efficacy of percutaneous common bile duct stone extraction via cystic duct after percutaneous cholecystostomy. Twenty-five consecutive patients with choledocholithiasis underwent percutaneous stone extraction under conscious sedation. The stones were extracted through the 12-Fr sheath using Wittich nitinol stone basket under fluoroscopic guidance via cystic duct after percutaneous trnas-hepatic cholecystostomy. Common bile duct stones were successfully removed in 22 of the 25 patients (88%) by this new technique. The causes of failure in three patients were bile leakage, hematoma of the gallbladder and failure of cystic duct cannulation. Cystic duct injury during this procedure did not occur and there was no post-procedure mortality. The mean period of indwelling catheter was 8.7±4.6 days and the mean duration of hospitalization was 13.4±5.9 days. Percutaneous commmon bile duct stone extraction via the cystic duct through percutaneous cholecystostomy route is effective and feasible for treating choledocholithiasis.

Optimization of headspace solid-phase microextraction by means of an experimental design for the determination of methyl tert.-butyl ether in water by gas chromatography-flame ionization detection.

PubMed

Dron, Julien; Garcia, Rosa; Millán, Esmeralda

2002-07-19

A procedure for determination of methyl tert.-butyl ether (MTBE) in water by headspace solid-phase microextraction (HS-SPME) has been developed. The analysis was carried out by gas chromatography with flame ionization detection. The extraction procedure, using a 65-microm poly(dimethylsiloxane)-divinylbenzene SPME fiber, was optimized following experimental design. A fractional factorial design for screening and a central composite design for optimizing the significant variables were applied. Extraction temperature and sodium chloride concentration were significant variables, and 20 degrees C and 300 g/l were, respectively chosen for the best extraction response. With these conditions, an extraction time of 5 min was sufficient to extract MTBE. The calibration linear range for MTBE was 5-500 microg/l and the detection limit 0.45 microg/l. The relative standard deviation, for seven replicates of 250 microg/l MTBE in water, was 6.3%.

The optimization of essential oils supercritical CO2 extraction from Lavandula hybrida through static-dynamic steps procedure and semi-continuous technique using response surface method

PubMed Central

Kamali, Hossein; Aminimoghadamfarouj, Noushin; Golmakani, Ebrahim; Nematollahi, Alireza

2015-01-01

Aim: The aim of this study was to examine and evaluate crucial variables in essential oils extraction process from Lavandula hybrida through static-dynamic and semi-continuous techniques using response surface method. Materials and Methods: Essential oil components were extracted from Lavandula hybrida (Lavandin) flowers using supercritical carbon dioxide via static-dynamic steps (SDS) procedure, and semi-continuous (SC) technique. Results: Using response surface method the optimum extraction yield (4.768%) was obtained via SDS at 108.7 bar, 48.5°C, 120 min (static: 8×15), 24 min (dynamic: 8×3 min) in contrast to the 4.620% extraction yield for the SC at 111.6 bar, 49.2°C, 14 min (static), 121.1 min (dynamic). Conclusion: The results indicated that a substantial reduction (81.56%) solvent usage (kg CO2/g oil) is observed in the SDS method versus the conventional SC method. PMID:25598636

Two-Phase Extraction for Comprehensive Analysis of the Plant Metabolome by NMR.

PubMed

Schripsema, Jan; Dagnino, Denise

2018-01-01

Metabolomics is the area of research, which strives to obtain complete metabolic fingerprints, to detect differences between them, and to provide hypothesis to explain those differences [1]. But obtaining complete metabolic fingerprints is not an easy task. Metabolite extraction is a key step during this process, and much research has been devoted to finding the best solvent mixture to extract as much metabolites as possible.Here a procedure is described for analysis of both polar and apolar metabolites using a two-phase extraction system. D 2 O and CDCl 3 are the solvents of choice, and their major advantage is that, for the identification of the compounds, standard databases can be used because D 2 O and CDCl 3 are the solvents most commonly used for pure compound NMR spectra. The procedure enables the absolute quantification of components via the addition of suitable internal standards. The extracts are also suitable for further analysis with other systems like LC-MS or GC-MS.

High-power ultrasonic system for the enhancement of mass transfer in supercritical CO2 extraction processes

NASA Astrophysics Data System (ADS)

Riera, Enrique; Blanco, Alfonso; García, José; Benedito, José; Mulet, Antonio; Gallego-Juárez, Juan A.; Blasco, Miguel

2010-01-01

Oil is an important component of almonds and other vegetable substrates that can show an influence on human health. In this work the development and validation of an innovative, robust, stable, reliable and efficient ultrasonic system at pilot scale to assist supercritical CO2 extraction of oils from different substrates is presented. In the extraction procedure ultrasonic energy represents an efficient way of producing deep agitation enhancing mass transfer processes because of some mechanisms (radiation pressure, streaming, agitation, high amplitude vibrations, etc.). A previous work to this research pointed out the feasibility of integrating an ultrasonic field inside a supercritical extractor without losing a significant volume fraction. This pioneer method enabled to accelerate mass transfer and then, improving supercritical extraction times. To commercially develop the new procedure fulfilling industrial requirements, a new configuration device has been designed, implemented, tested and successfully validated for supercritical fluid extraction of oil from different vegetable substrates.

Selective treatment to reduce contamination of propolis by polycyclic aromatic hydrocarbons (PAHs) still preserving its active polyphenol component and antioxidant activity.

PubMed

Galeotti, Fabio; Crimaldi, Laura; Maccari, Francesca; Zaccaria, Vincenzo; Fachini, Alfredo; Volpi, Nicola

2017-09-01

The adverse effects on health and environment caused by polycyclic aromatic hydrocarbons (PAHs) are critical problems. EFSA has defined 16 priority PAHs that are both genotoxic and carcinogenic, and identified eight (PAH8) priority PAHs as good indicators of the toxicity and occurrence in food. Food supplements containing propolis were also found to contain relatively high quantities of PAHs. We report about an extractive procedure which is able to purify propolis from a high content of PAHs using a balanced mixture of ethanol and water solvents. Extracts were characterised for total content of polyphenols, for in vitro antioxidant activity, and single classes of polyphenols evaluated by HPLC-ESI-MS. Obtained propolis extracts were found to have PAH8 and specific benzo[a]pyrene content below limits recommended by EFSA. The reported extractive procedure is easily applicable for possible industrial productions and may also be adopted to the purification of polyphenols from other plant extracts and natural sources.

RECOMMENDED OPERATING PROCEDURE NO. 45: ANALYSIS OF NITROUS OXIDE FROM COMBUSTION SOURCES

EPA Science Inventory

The recommended operating procedure (ROP) has been prepared for use in research activities conducted by EPA's Air and Energy Engineering Research Laboratory (AEERL). he procedure applies to the measurement of nitrous oxide (N2O) in dry gas samples extracted from gas streams where...

Symbolic dynamic filtering and language measure for behavior identification of mobile robots.

PubMed

Mallapragada, Goutham; Ray, Asok; Jin, Xin

2012-06-01

This paper presents a procedure for behavior identification of mobile robots, which requires limited or no domain knowledge of the underlying process. While the features of robot behavior are extracted by symbolic dynamic filtering of the observed time series, the behavior patterns are classified based on language measure theory. The behavior identification procedure has been experimentally validated on a networked robotic test bed by comparison with commonly used tools, namely, principal component analysis for feature extraction and Bayesian risk analysis for pattern classification.

Speciation of mercury in sludge solids: washed sludge

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.; Lourie, A. P.

2017-10-24

The objective of this applied research task was to study the type and concentration of mercury compounds found within the contaminated Savannah River Site Liquid Waste System (SRS LWS). A method of selective sequential extraction (SSE), developed by Eurofins Frontier Global Sciences1,2 and adapted by SRNL, utilizes an extraction procedure divided into seven separate tests for different species of mercury. In the SRNL’s modified procedure four of these tests were applied to a washed sample of high level radioactive waste sludge.

Optimized manual and automated recovery of amplifiable DNA from tissues preserved in buffered formalin and alcohol-based fixative.

PubMed

Duval, Kristin; Aubin, Rémy A; Elliott, James; Gorn-Hondermann, Ivan; Birnboim, H Chaim; Jonker, Derek; Fourney, Ron M; Frégeau, Chantal J

2010-02-01

Archival tissue preserved in fixative constitutes an invaluable resource for histological examination, molecular diagnostic procedures and for DNA typing analysis in forensic investigations. However, available material is often limited in size and quantity. Moreover, recovery of DNA is often severely compromised by the presence of covalent DNA-protein cross-links generated by formalin, the most prevalent fixative. We describe the evaluation of buffer formulations, sample lysis regimens and DNA recovery strategies and define optimized manual and automated procedures for the extraction of high quality DNA suitable for molecular diagnostics and genotyping. Using a 3-step enzymatic digestion protocol carried out in the absence of dithiothreitol, we demonstrate that DNA can be efficiently released from cells or tissues preserved in buffered formalin or the alcohol-based fixative GenoFix. This preparatory procedure can then be integrated to traditional phenol/chloroform extraction, a modified manual DNA IQ or automated DNA IQ/Te-Shake-based extraction in order to recover DNA for downstream applications. Quantitative recovery of high quality DNA was best achieved from specimens archived in GenoFix and extracted using magnetic bead capture.

Ancient DNA in historical parchments - identifying a procedure for extraction and amplification of genetic material.

PubMed

Lech, T

2016-05-06

Historical parchments in the form of documents, manuscripts, books, or letters, make up a large portion of cultural heritage collections. Their priceless historical value is associated with not only their content, but also the information hidden in the DNA deposited on them. Analyses of ancient DNA (aDNA) retrieved from parchments can be used in various investigations, including, but not limited to, studying their authentication, tracing the development of the culture, diplomacy, and technology, as well as obtaining information on the usage and domestication of animals. This article proposes and verifies a procedure for aDNA recovery from historical parchments and its appropriate preparation for further analyses. This study involved experimental selection of an aDNA extraction method with the highest efficiency and quality of extracted genetic material, from among the multi-stage phenol-chloroform extraction methods, and the modern, column-based techniques that use selective DNA-binding membranes. Moreover, current techniques to amplify entire genetic material were questioned, and the possibility of using mitochondrial DNA for species identification was analyzed. The usefulness of the proposed procedure was successfully confirmed in identification tests of historical parchments dating back to the 13-16th century AD.

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

USGS Publications Warehouse

Krynitsky, A.J.; Stafford, C.J.; Wiemeyer, Stanley N.

1988-01-01

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

Combining Follicular Unit Extraction and Scalp Micropigmentation for the Cosmetic Treatment of Alopecias

PubMed Central

Pak, Jae; Kim, Jino

2017-01-01

Two relatively new modalities, follicular unit extraction (FUE) and scalp micropigmentation have changed the treatment of hair loss, to reduce the number of procedures and the total costs of the hair restoration process. These 2 modalities augment each other when treating patients with thinning hair and balding. The explosion of FUE procedures (which reflected 52.6% of the hair transplant procedures performed in 2016, up from 48.5%) and the appearance of more and more new physicians offering hair restoration technologies employing FUE have caused a 20% annual growth in this industry over the past few years. This article reviews the use of FUE and scalp micropigmentation when used in combination. PMID:29263945

Speciation of antimony in airborne particulate matter using ultrasound probe fast extraction and analysis by HPLC-HG-AFS.

PubMed

Bellido-Martín, A; Gómez-Ariza, J L; Smichowsky, P; Sánchez-Rodas, D

2009-09-07

A fast extraction procedure has been developed for Sb(III) and Sb(V) oxoanions speciation in airborne particulate matter samples. Different extraction media (diammonium tartrate, hidroxilammonium clorhidrate, citric acid+ascorbic acid, phosphoric acid and citrate solutions) were tried, with assistance of an ultrasonic probe. The operation power and time of extraction were also optimized. The higher extraction recoveries were obtained with a 100 mmol L(-1) hidroxilammonium clorhidrate aqueous solution assisted by the ultrasound probe operated at 50 W during 3 min. The extracts were analyzed by HPLC-HG-AFS. The chromatographic separation of Sb(III) and Sb(V) was also optimized using diammonium tartrate and phthalic acid as mobile phases. The separation of both Sb species was performed in less than 3 min under isocratic conditions, using a 200 mmol L(-1) diammonium tartrate solution. The proposed extraction procedure and the HPLC-HG-AFS instrumental coupling have been successfully applied to airborne particulate matter samples, with high Sb content, collected in heavy traffic streets from Buenos Aires (Argentina). The results showed the presence of both Sb species at similar concentrations in the ng m(-3) level. The extraction yield was higher than 90% for all the analyzed samples.

Supercritical carbon dioxide extraction of 2,4-dichlorophenol from food crop tissues.

PubMed

Thomson, C A; Chesney, D J

1992-04-15

Supercritical fluid extraction with carbon dioxide has been found to be effective for the isolation of residue levels (0.1-1 ppm) of 2,4-dichlorophenol from selected plant tissues. The 2,4-dichlorophenol residues were incompletely extracted with supercritical CO2 alone, since a substantial fraction of the 2,4-dichlorophenol was covalently attached to the plant matrix. An acid pretreatment procedure was developed to partially hydrolyze the plant tissue prior to extraction, releasing the bound 2,4-dichlorophenol residues. Steam distillation showed higher residue levels for field-treated straw samples. This is attributed to the greater degree of hydrolysis inherent in the steam distillation procedure. Supercritical CO2 extraction of field-treated seed samples showed higher levels of 2,4-dichlorophenol residues than did steam distillation. The supercritical fluid extractant was able to solvate 2,4-dichlorophenol residues in the interior of the seed and transport them to the surface for collection. The aqueous medium used in steam distillation was unable to penetrate the hydrophobic seed matrix to the same degree. While the actual extraction time experienced in supercritical fluid extraction was far less than that of steam distillation (45 min vs 6 h, respectively), the total sample preparation time was similar in both methods.

Multivessel supercritical fluid extraction of food items in Total Diet Study.

PubMed

Hopper, M L; King, J W; Johnson, J H; Serino, A A; Butler, R J

1995-01-01

An off-line, large capacity, multivessel supercritical fluid extractor (SFE) was designed and constructed for extraction of large samples. The extractor can simultaneously process 1-6 samples (15-25 g) by using supercritical carbon dioxide (SC-CO2), which is relatively nontoxic and nonflammable, as the solvent extraction medium. Lipid recoveries for the SFE system were comparable to those obtained by blending or Soxhlet extraction procedures. Extractions at 10,000 psi, 80 degrees C, expanded gaseous CO2 flow rates of 4-5 L/min (35 degrees C), and 1-3 h extraction times gave reproducible lipid recoveries for pork sausage (relative standard deviation [RSD], 1.32%), corn chips (RSD, 0.46%), cheddar cheese (RSD, 1.14%), and peanut butter (RSD, 0.44%). In addition, this SFE system gave reproducible recoveries (> 93%) for butter fortified with cis-chlordane and malathion at the 100 ppm and 0.1 ppm levels. Six portions each of cheddar cheese, saltine crackers, sandwich cookies, and ground hamburger also were simultaneously extracted with SC-CO2 and analyzed for incurred pesticide residues. Results obtained with this SFE system were reproducible and comparable with results from organic-solvent extraction procedures currently used in the Total Diet Study; therefore, use and disposal of large quantities of organic solvents can be eliminated.

Focused microwave-assisted extraction combined with solid-phase microextraction and gas chromatography-mass spectrometry for the selective analysis of cocaine from coca leaves.

PubMed

Bieri, Stefan; Ilias, Yara; Bicchi, Carlo; Veuthey, Jean-Luc; Christen, Philippe

2006-04-21

An effective combination of focused microwave-assisted extraction (FMAE) with solid-phase microextraction (SPME) prior to gas chromatography (GC) is described for the selective extraction and quantitative analysis of cocaine from coca leaves (Erythroxylum coca). This approach required switching from an organic extraction solvent to an aqueous medium more compatible with SPME liquid sampling. SPME was performed in the direct immersion mode with a universal 100 microm polydimethylsiloxane (PDMS) coated fibre. Parameters influencing this extraction step, such as solution pH, sampling time and temperature are discussed. Furthermore, the overall extraction process takes into account the stability of cocaine in alkaline aqueous solutions at different temperatures. Cocaine degradation rate was determined by capillary electrophoresis using the short end injection procedure. In the selected extraction conditions, less than 5% of cocaine was degraded after 60 min. From a qualitative point of view, a significant gain in selectivity was obtained with the incorporation of SPME in the extraction procedure. As a consequence of SPME clean-up, shorter columns could be used and analysis time was reduced to 6 min compared to 35 min with conventional GC. Quantitative results led to a cocaine content of 0.70 +/- 0.04% in dry leaves (RSD <5%) which agreed with previous investigations.

Tricuspid insufficiency after laser lead extraction.

PubMed

Rodriguez, Yasser; Mesa, Julian; Arguelles, Eric; Carrillo, Roger G

2013-08-01

The use of laser lead extraction (LLE) to remove pacemaker and implantable cardiac defibrillator leads has become more prevalent in the past decade. Though the procedure is associated with a low rate of complications, LLE still poses some risks to patients. Some reports have suggested an increase in tricuspid insufficiency (TI) associated with LLE. We present a series of patients who underwent both LLE and complete evaluation for TI with echocardiographic techniques. From August 2008 to January 2010, 173 prospective, consecutive patients underwent LLE in a single center. All patients had transesophageal echocardiograms (TEE) during the extraction. Fifty-three patients had tricuspid valve function evaluated a day before the procedure with a transthoracic echocardiogram (TTE), during the procedure with a TEE and 2 days postoperatively with a TTE. All 173 patients experienced no change in tricuspid valve function during the procedure with TEE. Of the 53 patients who underwent a complete TI evaluation, 38 were males (72%) and 15 females (38%), with a mean age of 69.45 ± 14.08. Mean ejection fraction was 35.82 ± 14.72. Three (6%) patients experienced TI after the procedure (two mild and one severe, all with tricuspid valve endocarditis); 16 (30%) patients were found to have TI before LLE that returned to normal valve function during or after the procedure. Thirty-four (64%) patients did not experience any significant change of the tricuspid valve performance after LLE. LLE was not associated with increased TI. ©2013, The Authors. Journal compilation ©2013 Wiley Periodicals, Inc.

Microwave-Assisted Extraction of Fucoidan from Marine Algae.

PubMed

Mussatto, Solange I

2015-01-01

Microwave-assisted extraction (MAE) is a technique that can be applied to extract compounds from different natural resources. In this chapter, the use of this technique to extract fucoidan from marine algae is described. The method involves a closed MAE system, ultrapure water as extraction solvent, and suitable conditions of time, pressure, and algal biomass/water ratio. By using this procedure under the specified conditions, the penetration of the electromagnetic waves into the material structure occurs in an efficient manner, generating a distributed heat source that promotes the fucoidan extraction from the algal biomass.

Ultrasonication followed by single-drop microextraction combined with GC/MS for rapid determination of organochlorine pesticides from fish.

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2008-02-01

A novel, rapid and simple sample pretreatment technique termed ultrasonication followed by single-drop micro-extraction (U-SDME) has been developed and combined with GC/MS for the determination of organochlorine pesticides (OCPs) in fish. In the present work, the lengthy procedures generally used in the conventional methods like, Soxhlet extraction, supercritical fluid extraction, pressurized liquid extraction and microwave assisted solvent extraction for extraction of OCPs from fish tissues are minimized by the use of two simple extraction procedures. Firstly, OCPs from fish were extracted in organic solvent with ultrasonication and then subsequently preconcentrated by single-drop micro-extraction (SDME). Extraction parameters of ultrasonication and SDME were optimized in spiked sample solution in order to obtain efficient extraction of OCPs from fish tissues. The calibration curves for OCPs were found to be linear between 10-1000 ng/g with correlation of estimations in the range 0.990-0.994. The recoveries obtained in blank fish tissues were ranged from 82.1 to 95.3%. The LOD and RSD for determination of OCPs in fish were 0.5 ng/g and 9.4-10.0%, respectively. The proposed method was applied for the determination of bioconcentration factor in fish after exposure to different concentrations of OCPs in cultured water. The present method avoids the co-extraction of lipids, long extraction steps (>12 h) and large amount of organic solvent for the separation of OCPs. The main advantages of the present method are rapid, selective, sensitive and low cost for the determination of OCPs in fish.

Novel approach to microwave-assisted extraction and micro-solid-phase extraction from soil using graphite fibers as sorbent.

PubMed

Xu, Li; Lee, Hian Kee

2008-05-30

A single-step extraction-cleanup procedure involving microwave-assisted extraction (MAE) and micro-solid-phase extraction (micro-SPE) has been developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) from soil samples. Micro-SPE is a relatively new extraction procedure that makes use of a sorbent enclosed within a sealed polypropylene membrane envelope. In the present work, for the first time, graphite fiber was used as a sorbent material for extraction. MAE-micro-SPE was used to cleanup sediment samples and to extract and preconcentrate five PAHs in sediment samples prepared as slurries with addition of water. The best extraction conditions comprised of microwave heating at 50 degrees C for a duration of 20 min, and an elution (desorption) time of 5 min using acetonitrile with sonication. Using gas chromatography (GC)-flame ionization detection (FID), the limits of detection (LODs) of the PAHs ranged between 2.2 and 3.6 ng/g. With GC-mass spectrometry (MS), LODs were between 0.0017 and 0.0057 ng/g. The linear ranges were between 0.1 and 50 or 100 microg/g for GC-FID analysis, and 1 and 500 or 1000 ng/g for GC-MS analysis. Granular activated carbon was also used for the micro-SPE device but was found to be not as efficient in the PAH extraction. The MAE-micro-SPE method was successfully used for the extraction of PAHs in river and marine sediments, demonstrating its applicability to real environmental solid matrixes.

Pleurodesis Using Mistletoe Extract Delivered via a Spray Catheter during Semirigid Pleuroscopy for Managing Symptomatic Malignant Pleural Effusion.

PubMed

Eom, Jung Seop; Ahn, Hyo Yeong; Mok, Jeong Ha; Lee, Geewon; Jo, Eun-Jung; Kim, Mi-Hyun; Lee, Kwangha; Kim, Ki Uk; Park, Hye-Kyung; Lee, Min Ki

Talc poudrage during thoracoscopy is considered the standard procedure for patients with symptomatic malignant pleural effusion (MPE). Until now, no alternative technique other than talc poudrage for pleurodesis during medical thoracoscopy has been proposed. Liquid sclerosants, such as mistletoe extract, have been sprayed evenly into the pleural cavity during semirigid pleuroscopy for chemical pleurodesis. We conducted a retrospective study using the database of semirigid pleuroscopy to identify the usefulness of pleurodesis using a mistletoe extract delivered via a spray catheter during semirigid pleuroscopy for symptomatic MPE. All consecutive patients with symptomatic MPE who underwent semirigid pleuroscopy from October 2015 to September 2016 were registered. The responses were evaluated using chest X- ray or computed tomography 4 weeks after pleurodesis. The study included 43 patients who underwent pleurodesis with mistletoe extract via a spray catheter during semirigid pleuroscopy. Complete and partial responses were seen in 21 (49%) and 19 (44%) patients, respectively. The median duration of chest tube placement after pleurod-esis was 7 days (range 6-8 days) in the 40 patients with complete or partial responses. No cases of severe hemorrhage, empyema formation, respiratory failure, or procedure-related mortality were observed in the subjects at 4 weeks after semirigid pleuroscopy. Pleurodesis with mistletoe extract delivered via a spray catheter during semirigid pleuroscopy is a safe and effective procedure for managing symptomatic MPE. © 2017 S. Karger AG, Basel.

Dispersive liquid-liquid microextraction for the determination of nitrophenols in soils by microvial insert large volume injection-gas chromatography-mass spectrometry.

PubMed

Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

2016-07-22

A rapid and sensitive procedure for the determination of six NPs in soils by gas chromatography and mass spectrometry (GC-MS) is proposed. Ultrasound assisted extraction (UAE) is used for NP extraction from soil matrices to an organic solvent, while the environmentally friendly technique dispersive liquid-liquid microextraction (DLLME) is used for the preconcentration of the resulting UAE extracts. NPs were derivatized by applying an "in-situ" acetylation procedure, before being injected into the GC-MS system using microvial insert large volume injection (LVI). Several parameters affecting UAE, DLLME, derivatization and injection steps were investigated. The optimized procedure provided recoveries of 86-111% from spiked samples. Precision values of the procedure (expressed as relative standard deviation, RSD) lower than 12%, and limits of quantification ranging from 1.3 to 2.6ngg(-1), depending on the compound, were obtained. Twenty soil samples, obtained from military, industrial and agricultural areas, were analyzed by the proposed method. Two of the analytes were quantified in two of the samples obtained from industrial areas, at concentrations in the 4.8-9.6ngg(-1) range. Copyright © 2016 Elsevier B.V. All rights reserved.

Characterization of soil phosphorus in a fire-affected forest Cambisol by chemical extractions and (31)P-NMR spectroscopy analysis.

PubMed

Turrion, María-Belén; Lafuente, Francisco; Aroca, María-José; López, Olga; Mulas, Rafael; Ruipérez, Cesar

2010-07-15

This study was conducted to investigate the long-term effects of fire on soil phosphorus (P) and to determine the efficiency of different procedures in extracting soil P forms. Different P forms were determined: labile forms (Olsen-P, Bray-P, and P extracted by anion exchange membranes: AEM-P); moderately labile inorganic and organic P, obtained by NaOH-EDTA extraction after removing the AEM-P fraction; and total organic and inorganic soil P. (31)P-NMR spectroscopy was used to characterize the structure of alkali-soluble P forms (orthophosphate, monoester, pyrophosphate, and DNA). The studied area was a Pinus pinaster forest located at Arenas de San Pedro (southern Avila, Spain). The soils were Dystric Cambisols over granites. Soil samples were collected at 0-2 cm, 2-5 cm, and 10-15 cm depths, two years after a fire in the burned area and in an adjacent unburned forest area. Fire increased the total N, organic C, total P, and organic and inorganic P content in the surface soil layer. In burned soil, the P extracted by the sequential procedure (AEM and NaOH+EDTA) was about 95% of the total P. Bray extraction revealed a fire-induced increase in the sorption surfaces. Analysis by chemical methods overestimated the organic P fraction in the EDTA-NaOH extract in comparison with the determination by ignition procedure. This overestimation was more important in the burned than unburned soil samples, probably due to humification promoted by burning, which increased P sorption by soil particles. The fire-induced changes on the structure of alkali-soluble P were an increase in orthophosphate-P and a decrease in monoester-P and DNA-P. Copyright 2010 Elsevier B.V. All rights reserved.

Simultaneous determination of the endocrine disrupting compounds nonylphenol, nonylphenol ethoxylates, triclosan and bisphenol A in wastewater and sewage sludge by gas chromatography-mass spectrometry.

PubMed

Gatidou, Georgia; Thomaidis, Nikolaos S; Stasinakis, Athanasios S; Lekkas, Themistokles D

2007-01-05

An integrated analytical method for the simultaneous determination of 4-n-nonylphenol (4-n-NP), nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), bisphenol A (BPA) and triclosan (TCS) in wastewater (dissolved and particulate phase) and sewage sludge was developed based on gas chromatography-mass spectrometry. Chromatographic analysis was achieved after derivatization with bis(trimethylsilyl)trifluoroacetamide (BSTFA). Extraction from water samples was performed by solid-phase extraction (SPE). The optimization of SPE procedure included the type of sorbent and the type of the organic solvent used for the elution. Referred to solid samples, the target compounds were extracted by sonication. In this case the optimization of the extraction procedure included the variation of the amount of the extracted biomass, the duration and the temperature of sonication and the type of the extraction organic solvent. The developed extraction procedures resulted in good repeatability and reproducibility with relative standard deviations (RSDs) less than 13% for all the tested compounds for both types of samples. Satisfactory recoveries were obtained (>60%) for all the compounds in both liquid and solid samples, except for 4-n-NP, which gave recoveries up to 35% in wastewater samples and up to 63% in sludge samples. The limits of detection (LODs) of the target compounds varied from 0.03 (4-n-NP) to 0.41 microg l(-1) (NP2EO) and from 0.04 (4-n-NP) to 0.96 microg kg(-1) (NP2EO) for liquid and solid samples, respectively. The developed methods were successfully applied to the analysis of the target compounds in real samples.

Ionization Electron Signal Processing in Single Phase LArTPCs I. Algorithm Description and Quantitative Evaluation with MicroBooNE Simulation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Adams, C.; et al.

We describe the concept and procedure of drifted-charge extraction developed in the MicroBooNE experiment, a single-phase liquid argon time projection chamber (LArTPC). This technique converts the raw digitized TPC waveform to the number of ionization electrons passing through a wire plane at a given time. A robust recovery of the number of ionization electrons from both induction and collection anode wire planes will augment the 3D reconstruction, and is particularly important for tomographic reconstruction algorithms. A number of building blocks of the overall procedure are described. The performance of the signal processing is quantitatively evaluated by comparing extracted charge withmore » the true charge through a detailed TPC detector simulation taking into account position-dependent induced current inside a single wire region and across multiple wires. Some areas for further improvement of the performance of the charge extraction procedure are also discussed.« less

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and alpha-spectrometry.

PubMed

Goldstein, S J; Hensley, C A; Armenta, C E; Peters, R J

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for alpha-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of "real" environmental and bioassay samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of approximately 2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously.

Determination of 105 antibiotic, anti-inflammatory, antiparasitic agents and tranquilizers by LC-MS/MS based on an acidic QuEChERS-like extraction.

PubMed

Desmarchelier, Aurélien; Fan, Kaïli; Minh Tien, Mai; Savoy, Marie-Claude; Tarres, Adrienne; Fuger, Denis; Goyon, Alexandre; Bessaire, Thomas; Mottier, Pascal

2018-04-01

A procedure for screening 105 veterinary drugs in foods by liquid chromatography tandem mass-spectrometry (LC-MS/MS) is presented. Its scope encompasses raw materials of animal origin (milk, meat, fish, egg and fat) but also related processed ingredients and finished products commonly used and manufactured by food business operators. Due to the complexity of the matrices considered and to efficiently deal with losses during extraction and matrix effects during MS source ionisation, each sample was analysed twice, that is 'unspiked' and 'spiked at the screening target concentration' using a QuEChERS-like extraction. The entire procedure was validated according to the European Community Reference Laboratories Residues Guidelines. False-negative and false-positive rates were below 5% for all veterinary drugs whatever the food matrix. Effectiveness of the procedure was further demonstrated through participation to five proficiency tests and its ruggedness demonstrated in quality control operations by a second laboratory.

Extracting a Purely Non-rigid Deformation Field of a Single Structure

NASA Astrophysics Data System (ADS)

Demirci, Stefanie; Manstad-Hulaas, Frode; Navab, Nassir

During endovascular aortic repair (EVAR) treatment, the aortic shape is subject to severe deformation that is imposed by medical instruments such as guide wires, catheters, and the stent graft. The problem definition of deformable registration of images covering the entire abdominal region, however, is highly ill-posed. We present a new method for extracting the deformation of an aneurysmatic aorta. The outline of the procedure includes initial rigid alignment of two abdominal scans, segmentation of abdominal vessel trees, and automatic reduction of their centerline structures to one specified region of interest around the aorta. Our non-rigid registration procedure then only computes local non-rigid deformation and leaves out all remaining global rigid transformations. In order to evaluate our method, experiments for the extraction of aortic deformation fields are conducted on 15 patient datasets from endovascular aortic repair (EVAR) treatment. A visual assessment of the registration results were performed by two vascular surgeons and one interventional radiologist who are all experts in EVAR procedures.

An enhanced procedure for measuring organic acids and methyl esters in PM2.5

NASA Astrophysics Data System (ADS)

Liu, F.; Duan, F. K.; He, K. B.; Ma, Y. L.; Rahn, K. A.; Zhang, Q.

2015-11-01

A solid-phase extraction (SPE) pretreatment procedure allowing organic acids to be separated from methyl esters in fine aerosol has been developed. The procedure first separates the organic acids from fatty acid methyl esters (FAMEs) and other nonacid organic compounds by aminopropyl-based SPE cartridge and then quantifies them by gas chromatography/mass spectrometry. The procedure prevents the fatty acids and dimethyl phthalate from being overestimated, and so allows us to accurately quantify the C4-C11 dicarboxylic acids (DCAs) and the C8-C30 monocarboxylic acids (MCAs). Results for the extraction of DCAs, MCAs, and AMAs in eluate and FAMEs in effluate by SAX and NH2 SPE cartridges exhibited that the NH2 SPE cartridge gave higher extraction efficiency than the SAX cartridge. The recoveries of analytes ranged from 67.5 to 111.3 %, and the RSD ranged from 0.7 to 10.9 %. The resulting correlations between the aliphatic acids and FAMEs suggest that the FAMEs had sources similar to those of the carboxylic acids, or were formed by esterifying carboxylic acids, or that aliphatic acids were formed by hydrolyzing FAMEs. Through extraction and cleanup using this procedure, 17 aromatic acids in eluate were identified and quantified by gas chromatography/tandem mass spectrometry, including five polycyclic aromatic hydrocarbon (PAH): acids 2-naphthoic, biphenyl-4-carboxylic, 9-oxo-9H-fluorene-1-carboxylic, biphenyl-4,4´-dicarboxylic, and phenanthrene-1-carboxylic acid, plus 1,8-naphthalic anhydride. Correlations between the PAH acids and the dicarboxylic and aromatic acids suggested that the first three acids and 1,8-naphthalic anhydride were secondary atmospheric photochemistry products and the last two mainly primary.

On-line lab-in-syringe cloud point extraction for the spectrophotometric determination of antimony.

PubMed

Frizzarin, Rejane M; Portugal, Lindomar A; Estela, José M; Rocha, Fábio R P; Cerdà, Victor

2016-02-01

Most of the procedures for antimony determination require time-consuming sample preparation (e.g. liquid-liquid extraction with organic solvents), which are harmful to the environment. Because of the high antimony toxicity, a rapid, sensitive and greener procedure for its determination becomes necessary. The goal of this work was to develop an analytical procedure exploiting for the first time the cloud point extraction on a lab-in-syringe flow system aiming at the spectrophotometric determination of antimony. The procedure was based on formation of an ion-pair between the antimony-iodide complex and H(+) followed by extraction with Triton X-114. The factorial design showed that the concentrations of ascorbic acid, H2SO4 and Triton X-114, as well as second and third order interactions were significant at the 95% confidence level. A Box-Behnken design was applied to obtain the response surfaces and to identify the critical values. System is robust at the 95% confidence level. A linear response was observed from 5 to 50 µg L(-1), described by the equation A=0.137+0.050C(Sb) (r=0.998). The detection limit (99.7% confidence level), the coefficient of variation (n=5; 15 µg L(-1)) and the sampling rate was estimated at 1.8 µg L(-1), 1.6% and 16 h(-1), respectively. The procedure allows quantification of antimony in the concentrations established by environmental legislation (6 µg L(-1)) and it was successfully applied to the determination of antimony in freshwater samples and antileishmanial drugs, yielding results in agreement with those obtained by HGFAAS at the 95% confidence level. Copyright © 2015 Elsevier B.V. All rights reserved.

Recent Developments in Australian Gold Extraction.

ERIC Educational Resources Information Center

Thiele, Rodney B.

1995-01-01

Describes new technologies that have greatly improved the extraction efficiency of gold ore, including: altering plant layout to promote efficiency, engaging Filiblast forced oxidation and bioxidation systems, and updating the electrowinning procedure at the gold recovery stage. (JRH)

Assessment of Pb, Cd, Cr and Ag leaching from electronics waste using four extraction methods.

PubMed

Keith, Ashley; Keesling, Kara; Fitzwater, Kendra K; Pichtel, John; Houy, Denise

2008-12-01

Heavy metals present in electronic components may leach upon disposal and therefore pose significant environmental hazards. The potential leaching of Pb, Cd, Cr and Ag from PC cathode ray tubes, printed circuit boards (PCBs), PC mice, TV remote controls, and mobile phones was assessed. After controlled crushing, each component was extracted using the Toxicity Characteristic Leaching Procedure (TCLP), EPA Method 1312 (SPLP), NEN 7371 (Dutch Environmental Agency), and DIN S4 (Germany). The TCLP consistently leached the greatest amounts of Pb from all components. The SPLP, NEN 7371 and DIN S4 extracted relatively small amounts of metals compared with the TCLP and were not considered effective as leaching tests for e-waste. The smallest size fraction (< 2 mm) of CRT glass and PCBs leached significantly (p < 0.05) highest Pb via the TCLP. A modified TCLP removed 50.9% more extractable Pb compared with the conventional procedure.

A simple protocol for protein extraction of recalcitrant fruit tissues suitable for 2-DE and MS analysis.

PubMed

Song, Jun; Braun, Gordon; Bevis, Eric; Doncaster, Kristen

2006-08-01

Fruit tissues are considered recalcitrant plant tissue for proteomic analysis. Three phenol-free protein extraction procedures for 2-DE were compared and evaluated on apple fruit proteins. Incorporation of hot SDS buffer, extraction with TCA/acetone precipitation was found to be the most effective protocol. The results from SDS-PAGE and 2-DE analysis showed high quality proteins. More than 500 apple polypeptides were separated on a small scale 2-DE gel. The successful protocol was further tested on banana fruit, in which 504 and 386 proteins were detected in peel and flesh tissues, respectively. To demonstrate the quality of the extracted proteins, several protein spots from apple and banana peels were cut from 2-DE gels, analyzed by MS and have been tentatively identified. The protocol described in this study is a simple procedure which could be routinely used in proteomic studies of many types of recalcitrant fruit tissues.

Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

PubMed

Sklerov, J H; Kalasinsky, K S; Ehorn, C A

1999-10-01

A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were < 6% and < 13%, respectively. This procedure has been applied to quality-control specimens and LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DUST AND SOIL SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.15)

EPA Science Inventory

The method for extracting and preparing a dust or soil sample for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the extraction, concentration, and derivatization of samples that are to be analyzed by gas chromatography/mass spectrometry.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING URINE SAMPLES FOR ANALYSIS OF HYDROXY POLYCYCLIC AROMATIC HYDROCARBONS, PENTACHLOROPHENOL AND 2,4-D (SOP-5.21)

EPA Science Inventory

The method for extracting and preparing urine samples for analysis of hydroxy-polycyclic aromatic hydrocarbons, pentachlorophenol and 2,4-D is summarized in this SOP. It covers the extraction, concentration and methylation of samples that are to be analyzed by gas chromatography/...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.12)

EPA Science Inventory

The method is for extracting an indoor and outdoor air sample consisting of a quartz fiber filter and an XAD-2 cartridge for analysis of neutral persistent organic pollutants. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SURFACE WIPE FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.17)

EPA Science Inventory

This SOP summarizes the method for extracting and preparing a hard floor surface wipe or food preparation surface wipe sample for analysis of neutral persistent organic. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass spect...

Separation and structural analysis of saponins in a bark extract from Quillaja saponaria Molina.

PubMed

Nord, L I; Kenne, L

1999-07-20

Six major saponins were isolated from a bark extract from Quillaja saponaria Molina. Solid-phase extraction, followed by a two-step reversed-phase HPLC separation procedure with phosphate and ammonium acetate buffers of different pH values, was used. The compounds were characterised using NMR spectroscopy, mass spectrometry and chemical methods.

Occurrence of pneumomediastinum due to dental procedures.

PubMed

Aslaner, Mehmet Ali; Kasap, Gül Nihal; Demir, Cihat; Akkaş, Meltem; Aksu, Nalan M

2015-01-01

The occurrence of pneumomediastinum and massive subcutaneous emphysema due to dental procedures is quite rare. We present a case of pneumomediastinum and massive subcutaneous emphysema that occurred during third molar tooth extraction with air-turbine handpiece.

Use of gas chromatography-mass spectrometry for the assessment of the contamination caused by small concentrations of nitrophenols in soils and sediments

NASA Astrophysics Data System (ADS)

Cacho, Juan-Ignacio; Campillo, Natalia; Viñas, Pilar; Hernandez-Cordoba, Manuel

2015-04-01

Nitrophenols (NPs) are widely distributed environmental contaminants that can be present in soils and sediments due to the degradation of some pesticides (parathion and fenitrothion) or by accidental spilling in ammunition plants or storage places. This communication reports a rapid and sensitive procedure for the determination of the most common NPs in soils by using gas chromatography coupled to mass spectrometry (GC-MS) as the analytical technique. Ultrasound assisted extraction (UAE) was employed for the extraction of the NPs from the soil samples to an organic solvent. Next, the resulting UAE extracts were submitted to dispersive liquid-liquid microextraction (DLLME) for achieving an effective preconcentration. DLLME is an easy-to-carry out, environmentally friendly separation technique involving minimal amounts of organic solvents. Since the volatility of NPs is low, as a previous stage to the GC-MS measurement the compounds were derivatized using a simple "in-situ" acetylation procedure. The main parameters affecting the UAE stage, as well as the DLLME and derivatization steps, were investigated looking for maximum analytical signals. The optimized procedure provided extraction recoveries in the 72-86% range, with precision values (expressed as relative standard deviation, RSD) ≤ 12%, and detection limits ranging from 1.3 and 3.3 ng g-1, depending on the compound. 20 soil and sediment samples, from military, industrial and agricultural areas were analyzed by the studied procedure in order to check its applicability.

A procedure for quantitation of total oxidized uranium for bioremediation studies

USGS Publications Warehouse

Elias, Dwayne A.; Senko, John M.; Krumholz, Lee R.

2003-01-01

A procedure was developed for the quantitation of complexed U(VI) during studies on U(VI) bioremediation. These studies typically involve conversion of soluble or complexed U(VI) (oxidized) to U(IV) (the reduced form which is much less soluble). Since U(VI) freely exchanges between material adsorbed to the solid phase and the dissolved phase, uranium bioremediation experiments require a mass balance of U in both its soluble and adsorbed forms as well as in the reduced sediment bound phase. We set out to optimize a procedure for extraction and quantitation of sediment bound U(VI). Various extractant volumes to sediment ratios were tested and it was found that between 1:1 to 8:1 ratios (v/w) there was a steady increase in U(VI) recovered, but no change with further increases in v/w ratio.Various strengths of NaHCO3, Na-EDTA, and Na-citrate were used to evaluate complexed U(VI) recovery, while the efficiency of a single versus repeated extraction steps was compared with synthesized uranyl-phosphate and uranyl-hydroxide. Total recovery with 1 M NaHCO3 was 95.7% and 97.9% from uranyl-phosphate and uranyl-hydroxide, respectively, compared to 80.7% and 89.9% using 450 mM NaHCO3. Performing the procedure once yielded an efficiency of 81.1% and 92.3% for uranyl-phosphate and uranyl-hydroxide, respectively, as compared to three times. All other extractants yielded 7.9–82.0% in both experiments.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR ARCHIVE PROCEDURE FOR STUDY SAMPLES (UA-G-4.0)

EPA Science Inventory

The purpose of this SOP is to outline the archive/custody guidelines used by the NHEXAS Arizona research project. This procedure was followed to maintain and locate samples, extracts, tracings and hard copy results after laboratory analysis during the Arizona NHEXAS project and ...

40 CFR 53.63 - Test procedure: Wind tunnel inlet aspiration test.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 5 2011-07-01 2011-07-01 false Test procedure: Wind tunnel inlet... Testing Performance Characteristics of Class II Equivalent Methods for PM2.5 § 53.63 Test procedure: Wind... extracts an ambient aerosol at elevated wind speeds. This wind tunnel test uses a single-sized, liquid...

Plastic freezer bags: a cost-effective method to protect extraction sites in laparoscopic colorectal procedures?

PubMed

Huynh, Hai P; Musselman, Reilly P; Trottier, Daniel C; Soto, Claudia M; Poulin, Eric C; Mamazza, Joseph; Boushey, Robin P; Auer, Rebecca C; Moloo, Husein

2013-10-01

To review surgical-site infection (SSI) and retrieval-site tumor recurrence rates in laparoscopic colorectal procedures when using a plastic freezer bag as a wound protector. Laparoscopic colorectal procedures where a plastic freezer bag used as a wound protector at the extraction site were reviewed between 1991 and 2008 from a prospectively collected database. χ test was used to compare SSI and tumor recurrence rates between groups. Costing data were obtained from the operating room supplies department. A total of 936 cases with 51 (5.45%) surgical-site infections were identified. SSI rates did not differ when comparing groups based on demographic factors, diagnosis, or location of procedure. Retrieval-site tumor recurrence rate was 0.21% (1/474). Cost of plastic freezer bags including sterilization ranged from $0.25 to $3. Plastic freezer bags as wound protectors in laparoscopic colorectal procedures are cost effective and have SSI and retrieval-site tumor recurrence rates that compare favorably to published data.

Synthesis and application of a new thiazolylazo reagent for cloud point extraction and determination of cobalt in pharmaceutical preparations.

PubMed

Yamaki, Regina Terumi; Nunes, Luana Sena; de Oliveira, Hygor Rodrigues; Araújo, André S; Bezerra, Marcos Almeida; Lemos, Valfredo Azevedo

2011-01-01

The synthesis and characterization of the reagent 2-(5-bromothiazolylazo)-4-chlorophenol and its application in the development of a preconcentration procedure for cobalt determination using flame atomic absorption spectrometry after cloud point extraction is presented. This procedure is based on cobalt complexing and entrapment of the metal chelates into micelles of a surfactant-rich phase of Triton X-114. The preconcentration procedure was optimized by using a response surface methodology through the application of the Box-Behnken matrix. Under optimum conditions, the procedure determined the presence of cobalt with an LOD of 2.8 microg/L and LOQ of 9.3 microg/L. The enrichment factor obtained was 25. The precision was evaluated as the RSD, which was 5.5% for 10 microg/L cobalt and 6.9% for 30 microg/L. The accuracy of the procedure was assessed by comparing the results with those found using inductively coupled plasma-optical emission spectrometry. After validation, the procedure was applied to the determination of cobalt in pharmaceutical preparation samples containing cobalamin (vitamin B12).

Saffron Samples of Different Origin: An NMR Study of Microwave-Assisted Extracts

PubMed Central

Sobolev, Anatoly P.; Carradori, Simone; Capitani, Donatella; Vista, Silvia; Trella, Agata; Marini, Federico; Mannina, Luisa

2014-01-01

An NMR analytical protocol is proposed to characterize saffron samples of different geographical origin (Greece, Spain, Hungary, Turkey and Italy). A microwave-assisted extraction procedure was developed to obtain a comparable recovery of metabolites with respect to the ISO specifications, reducing the solvent volume and the extraction time needed. Metabolite profiles of geographically different saffron extracts were compared showing significant differences in the content of some metabolites. PMID:28234327

Optimisation of the microplate resazurin assay for screening and bioassay-guided fractionation of phytochemical extracts against Mycobacterium tuberculosis.

PubMed

O'Neill, Taryn E; Li, Haoxin; Colquhoun, Caitlyn D; Johnson, John A; Webster, Duncan; Gray, Christopher A

2014-01-01

Because of increased resistance to current drugs, there is an urgent need to discover new anti-mycobacterial compounds for the development of novel anti-tuberculosis drugs. The microplate resazurin assay (MRA) is commonly used to evaluate natural products and synthetic compounds for anti-mycobacterial activity. However, the assay can be problematic and unreliable when screening methanolic phytochemical extracts. To optimise the MRA for the screening and bioassay-guided fractionation of phytochemical extracts using Mycobacterium tuberculosis H37Ra. The effects of varying assay duration, resazurin solution composition, solvent (dimethyl sulphoxide - DMSO) concentration and type of microtitre plate used on the results and reliability of the MRA were investigated. The optimal bioassay protocol was applied to methanolic extracts of medicinal plants that have been reported to possess anti-mycobacterial activity. The variables investigated were found to have significant effects on the results obtained with the MRA. A standardised procedure that can reliably quantify anti-mycobacterial activity of phytochemical extracts in as little as 48 h was identified. The optimised MRA uses 2% aqueous DMSO, with an indicator solution of 62.5 µg/mL resazurin in 5% aqueous Tween 80 over 96 h incubation. The study has identified an optimal procedure for the MRA when used with M. tuberculosis H37Ra that gives rapid, reliable and consistent results. The assay procedure has been used successfully for the screening and bioassay-guided fractionation of anti-mycobacterial compounds from methanol extracts of Canadian medicinal plants. Copyright © 2014 John Wiley & Sons, Ltd.

Evaluation of Superparamagnetic Silica Nanoparticles for Extraction of Triazines in Magnetic in-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography

PubMed Central

González-Fuenzalida, R. A.; Moliner-Martínez, Y.; Prima-Garcia, Helena; Ribera, Antonio; Campins-Falcó, P.; Zaragozá, Ramon J.

2014-01-01

The use of magnetic nanomaterials for analytical applications has increased in the recent years. In particular, magnetic nanomaterials have shown great potential as adsorbent phase in several extraction procedures due to the significant advantages over the conventional methods. In the present work, the influence of magnetic forces over the extraction efficiency of triazines using superparamagnetic silica nanoparticles (NPs) in magnetic in tube solid phase microextraction (Magnetic-IT-SPME) coupled to CapLC has been evaluated. Atrazine, terbutylazine and simazine has been selected as target analytes. The superparamagnetic silica nanomaterial (SiO2-Fe3O4) deposited onto the surface of a capillary column gave rise to a magnetic extraction phase for IT-SPME that provided a enhancemment of the extraction efficiency for triazines. This improvement is based on two phenomena, the superparamegnetic behavior of Fe3O4 NPs and the diamagnetic repulsions that take place in a microfluidic device such a capillary column. A systematic study of analytes adsorption and desorption was conducted as function of the magnetic field and the relationship with triazines magnetic susceptibility. The positive influence of magnetism on the extraction procedure was demonstrated. The analytical characteristics of the optimized procedure were established and the method was applied to the determination of the target analytes in water samples with satisfactory results. When coupling Magnetic-IT-SPME with CapLC, improved adsorption efficiencies (60%–63%) were achieved compared with conventional adsorption materials (0.8%–3%). PMID:28344221

Simple and fast analysis of tetrabromobisphenol A, hexabromocyclododecane isomers, and polybrominated diphenyl ethers in serum using solid-phase extraction or QuEChERS extraction followed by tandem mass spectrometry coupled to HPLC and GC.

PubMed

Li, Jian; Chen, Tian; Wang, Yuwei; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei; Wang, Dejun; Wu, Yongning

2017-02-01

Two simplified sample preparation procedures for simultaneous extraction and clean-up of tetrabromobisphenol A, α-, β-, and γ-hexabromocyclododecane and polybrominated diphenyl ethers in human serum were developed and validated. The first procedure was based on solid-phase extraction. Sample extraction, purification, and lipid removal were carried out directly on an Oasis HLB cartridge. The second procedure was a quick, easy, cheap, effective, rugged, and safe-based approach using octadecyl-modified silica particles as a sorbent. After sample extraction and cleanup, tetrabromobisphenol A/hexabromocyclododecane was separated from polybrominated diphenyl ethers by using a Si-based cartridge. Tetrabromobisphenol A and hexabromocyclododecane were then detected by high-performance liquid chromatography coupled to tandem mass spectrometry, while polybrominated diphenyl ethers were detected by gas chromatography coupled to tandem mass spectrometry. The results of the spike recovery test using fetal bovine serum showed that the average recoveries of the analytes ranged from 87.3 to 115.3% with relative standard deviations equal to or lower than 13.4 %. Limits of detection of the analytes were in the range of 0.4-19 pg/mL except for decabromodiphenyl ether. The developed method was successfully applied to routine analysis of human serum samples from occupational workers and the general population. Extremely high serum polybrominated diphenyl ethers levels up to 3.32 × 10 4 ng/g lipid weight were found in occupational workers. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of microalgae derived lipids with supercritical carbon dioxide in an industrial relevant pilot plant.

PubMed

Lorenzen, Jan; Igl, Nadine; Tippelt, Marlene; Stege, Andrea; Qoura, Farah; Sohling, Ulrich; Brück, Thomas

2017-06-01

Microalgae are capable of producing up to 70% w/w triglycerides with respect to their dry cell weight. Since microalgae utilize the greenhouse gas CO 2 , they can be cultivated on marginal lands and grow up to ten times faster than terrestrial plants, the generation of algae oils is a promising option for the development of sustainable bioprocesses, that are of interest for the chemical lubricant, cosmetic and food industry. For the first time we have carried out the optimization of supercritical carbon dioxide (SCCO 2 ) mediated lipid extraction from biomass of the microalgae Scenedesmus obliquus and Scenedesmus obtusiusculus under industrrially relevant conditions. All experiments were carried out in an industrial pilot plant setting, according to current ATEX directives, with batch sizes up to 1.3 kg. Different combinations of pressure (7-80 MPa), temperature (20-200 °C) and CO 2 to biomass ratio (20-200) have been tested on the dried biomass. The most efficient conditions were found to be 12 MPa pressure, a temperature of 20 °C and a CO 2 to biomass ratio of 100, resulting in a high extraction efficiency of up to 92%. Since the optimized CO 2 extraction still yields a crude triglyceride product that contains various algae derived contaminants, such as chlorophyll and carotenoids, a very effective and scalable purification procedure, based on cost efficient bentonite based adsorbers, was devised. In addition to the sequential extraction and purification procedure, we present a consolidated online-bleaching procedure for algae derived oils that is realized within the supercritical CO 2 extraction plant.

Extracting natural dyes from wool--an evaluation of extraction methods.

PubMed

Manhita, Ana; Ferreira, Teresa; Candeias, António; Dias, Cristina Barrocas

2011-05-01

The efficiency of eight different procedures used for the extraction of natural dyes was evaluated using contemporary wool samples dyed with cochineal, madder, woad, weld, brazilwood and logwood. Comparison was made based on the LC-DAD peak areas of the natural dye's main components which had been extracted from the wool samples. Among the tested methods, an extraction procedure with Na(2)EDTA in water/DMF (1:1, v/v) proved to be the most suitable for the extraction of the studied dyes, which presented a wide range of chemical structures. The identification of the natural dyes used in the making of an eighteenth century Arraiolos carpet was possible using the Na(2)EDTA/DMF extraction of the wool embroidery samples and an LC-DAD-MS methodology. The effectiveness of the Na(2)EDTA/DMF extraction method was particularly observed in the extraction of weld dye components. Nine flavone derivatives previously identified in weld extracts could be identified in a single historical sample, confirming the use of this natural dye in the making of Arraiolos carpets. Indigo and brazilwood were also identified in the samples, and despite the fact that these natural dyes were referred in the historical recipes of Arraiolos dyeing, it is the first time that the use of brazilwood is confirmed. Mordant analysis by ICP-MS identified the widespread use of alum in the dyeing process, but in some samples with darker hues, high amounts of iron were found instead.

Displacement imprinted polymer receptor analysis (DIPRA) for chlorophenolic contaminants in drinking water and packaging materials.

PubMed

Nicholls, C; Karim, K; Piletsky, S; Saini, S; Setford, S

2006-01-15

The preparation of a molecularly imprinted polymer (MIP) for pentachlorophenol is described together with two alternative reporter derivatives for use in a displacement imprinted polymer receptor analysis (DIPRA) format procedure. In this procedure, alternative reporter molecules were rebound to the synthetic receptor sites and their displacement by the target analyte was employed as the basis of a simple procedure for the measurement of chlorophenols in water and packaging material samples. Water samples were extracted using the standard procedure (EPA 528) and a detection limit of 0.5 microg l(-1) was achieved using the DIPRA detection method, with good agreement between the displacement technique and GC-ECD analysis. A variety of packaging materials, extracted using a buffered detergent solution were also analysed using the DIPRA procedure and showed good agreement with GC results. In addition, investigation of the cross-reactivity of a range of pesticides and materials commonly encountered in environmental analysis indicated the procedure gave good discrimination between pesticides bearing a chlorophenolic moiety and other materials. The procedure is considered highly suitable for use as a rapid field-test method or for incorporation into a test kit device.

Hair Transplantation Controversies.

PubMed

Avram, Marc R; Finney, Robert; Rogers, Nicole

2017-11-01

Hair transplant surgery creates consistently natural appearing transplanted hair for men. It is increasingly popular procedure to restore natural growing hair for men with hair loss. To review some current controversies in hair transplant surgery. Review of the English PubMed literature and specialty literature in hair transplant surgery. Some of the controversies in hair transplant surgery include appropriate donor harvesting technique including elliptical donor harvesting versus follicular unit extraction whether manual versus robotic, the role of platelet-rich plasma and low-level light surgery in hair transplant surgery. Hair transplant surgery creates consistently natural appearing hair. As with all techniques, there are controversies regarding the optimal method for performing the procedure. Some of the current controversies in hair transplant surgery include optimal donor harvesting techniques, elliptical donor harvesting versus follicular unit extraction, the role of low-level light therapy and the platelet-rich plasma therapy in the procedure. Future studies will further clarify their role in the procedure.

Pesticide-sampling equipment, sample-collection and processing procedures, and water-quality data at Chicod Creek, North Carolina, 1992

USGS Publications Warehouse

Manning, T.K.; Smith, K.E.; Wood, C.D.; Williams, J.B.

1994-01-01

Water-quality samples were collected from Chicod Creek in the Coastal Plain Province of North Carolina during the summer of 1992 as part of the U.S. Geological Survey's National Water-Quality Assessment Program. Chicod Creek is in the Albemarle-Pamlico drainage area, one of four study units designated to test equipment and procedures for collecting and processing samples for the solid-phase extraction of selected pesticides, The equipment and procedures were used to isolate 47 pesticides, including organonitrogen, carbamate, organochlorine, organophosphate, and other compounds, targeted to be analyzed by gas chromatography/mass spectrometry. Sample-collection and processing equipment equipment cleaning and set-up procedures, methods pertaining to collecting, splitting, and solid-phase extraction of samples, and water-quality data resulting from the field test are presented in this report Most problems encountered during this intensive sampling exercise were operational difficulties relating to equipment used to process samples.

Terpenes as green solvents for extraction of oil from microalgae.

PubMed

Dejoye Tanzi, Celine; Abert Vian, Maryline; Ginies, Christian; Elmaataoui, Mohamed; Chemat, Farid

2012-07-09

Herein is described a green and original alternative procedure for the extraction of oil from microalgae. Extractions were carried out using terpenes obtained from renewable feedstocks as alternative solvents instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using Soxhlet extraction followed by the elimination of the solvent from the medium using Clevenger distillation in the second step. Oils extracted from microalgae were compared in terms of qualitative and quantitative determination. No significant difference was obtained between each extract, allowing us to conclude that the proposed method is green, clean and efficient.

OPTIMIZED DETERMINATION OF TRACE JET FUEL VOLATILE ORGANIC COMPOUNDS IN HUMAN BLOOD USING IN-FIELD LIQUID-LIQUID EXTRACTION WITH SUBSEQUENT LABORATORY GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS AND ON-COLUMN LARGE VOLUME INJECTION

EPA Science Inventory

A practical and sensitive method to assess volatile organic compounds (VOCs) from JP-8 jet fuel in human whole blood was developed by modifying previously established liquid-liquid extraction procedures, optimizing extraction times, solvent volume, specific sample processing te...

Displacement-dispersive liquid-liquid microextraction based on solidification of floating organic drop of trace amounts of palladium in water and road dust samples prior to graphite furnace atomic absorption spectrometry determination.

PubMed

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

2013-01-01

A new displacement-dispersive liquid-liquid microextraction method based on the solidification of floating organic drop was developed for separation and preconcentration of Pd(ll) in road dust and aqueous samples. This method involves two steps of dispersive liquid-liquid microextraction based on solidification. In Step 1, Cu ions react with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which is extracted by dispersive liquid-liquid microextraction based on a solidification procedure using 1-undecanol (extraction solvent) and ethanol (dispersive solvent). In Step 2, the extracted complex is first dispersed using ethanol in a sample solution containing Pd ions, then a dispersive liquid-liquid microextraction based on a solidification procedure is performed creating an organic drop. In this step, Pd(ll) replaces Cu(ll) from the pre-extracted Cu-DDTC complex and goes into the extraction solvent phase. Finally, the Pd(ll)-containing drop is introduced into a graphite furnace using a microsyringe, and Pd(ll) is determined using atomic absorption spectrometry. Several factors that influence the extraction efficiency of Pd and its subsequent determination, such as extraction and dispersive solvent type and volume, pH of sample solution, centrifugation time, and concentration of DDTC, are optimized.

Magnetic dispersive solid-phase extraction based on modified magnetic nanoparticles for the detection of cocaine and cocaine metabolites in human urine by high-performance liquid chromatography-mass spectrometry.

PubMed

Yang, Feiyu; Zou, Yun; Ni, Chunfang; Wang, Rong; Wu, Min; Liang, Chen; Zhang, Jiabin; Yuan, Xiaoliang; Liu, Wenbin

2017-11-01

An easy-to-handle magnetic dispersive solid-phase extraction procedure was developed for preconcentration and extraction of cocaine and cocaine metabolites in human urine. Divinyl benzene and vinyl pyrrolidone functionalized silanized Fe 3 O 4 nanoparticles were synthesized and used as adsorbents in this procedure. Scanning electron microscopy, vibrating sample magnetometry, and infrared spectroscopy were employed to characterize the modified adsorbents. A high-performance liquid chromatography with mass spectrometry method for determination of cocaine and its metabolites in human urine sample has been developed with pretreatment of the samples by magnetic dispersive solid-phase extraction. The obtained results demonstrated the higher extraction capacity of the prepared nanoparticles with recoveries between 75.1 to 105.7% and correlation coefficients higher than 0.9971. The limits of detection for the cocaine and cocaine metabolites were 0.09-1.10 ng/mL. The proposed magnetic dispersive solid-phase extraction method provided a rapid, environmentally friendly and magnetic stuff recyclable approach and it was confirmed that the prepared adsorbents material was a kind of highly effective extraction materials for the trace cocaine and cocaine metabolites analyses in human urine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Specific extraction of chromium as tetrabutylammonium-chromate and spectrophotometric determination by diphenylcarbazide: speciation of chromium in effluent streams.

PubMed

Noroozifar, M; Khorasani-Motlagh, M

2003-05-01

A very specific, selective, simple, and inexpensive procedure was developed for the speciation of CrVI and CrIII. This method is based on the quantitative extraction of chromate and CrIII (previously oxidized to CrVI) as a tetrabutylammonium-chromate ion-pair in methyl isobutyl ketone (MIBK), and then back extraction and preconcentration with an acidic diphenylcarbazide (DPC) solution. Back extraction was applied to achieve further preconcentration by a final factor of 20. The CrVI-DPC complex was determined in back-extract by a spectrophotometer at 548 nm. Under these extraction conditions, most of the probable concomitant cations and anions remained in the first inorganic phase. The calibration curve was linear up to 0.14 microg L(-1) of CrVI with a detection limit of 2.22 ng L(-1). The developed procedure was found to be suitable for the determination of the CrVI and CrIII species in various natural water samples with a relative standard deviation of better than 1.6%. The method was successfully applied to the speciation of chromium in spiked natural water samples, and also samples of effluent from a leather treatment plant.

Assessment of a geochemical extraction procedure to determine the solid phase fractionation and bioaccessibility of potentially harmful elements in soils: a case study using the NIST 2710 reference soil.

PubMed

Wragg, Joanna; Cave, Mark

2012-04-13

Three mineral acid sequential extraction regimes (HNO(3) only, HNO(3) followed by HCl and aqua regia) were applied to the NIST 2710 contaminated reference soil. The major and trace element chemical analysis data from the extractions were subjected to a chemometric self-modelling mixture resolution procedure which identified that 12 distinct physico-chemical components were extracted. The fractionation of As, Cd, Ni and Pb between these components were determined. Tentative assignments of the mineralogical sources of the components were made. The human ingestion bioaccessible fraction of As, Cd and Pb were determined using the in vitro BARGE UBM bioaccessibility test and were found to be 51.6%, 68.0% and 68.4% respectively. The relationship between the lability of the physico-chemical components and the bioaccessible fraction of the soils was investigated and the bioaccessible fractions were assigned to specific components. The extraction scheme using aqua regia was found to be the most suitable as it was the only one which extracted the iron sulphide phase in the soil. Copyright © 2012 Elsevier B.V. All rights reserved.

An improved filter elution and cell culture assay procedure for evaluating public groundwater systems for culturable enteroviruses.

PubMed

Dahling, Daniel R

2002-01-01

Large-scale virus studies of groundwater systems require practical and sensitive procedures for both sample processing and viral assay. Filter adsorption-elution procedures have traditionally been used to process large-volume water samples for viruses. In this study, five filter elution procedures using cartridge filters were evaluated for their effectiveness in processing samples. Of the five procedures tested, the third method, which incorporated two separate beef extract elutions (one being an overnight filter immersion in beef extract), recovered 95% of seeded poliovirus compared with recoveries of 36 to 70% for the other methods. For viral enumeration, an expanded roller bottle quantal assay was evaluated using seeded poliovirus. This cytopathic-based method was considerably more sensitive than the standard plaque assay method. The roller bottle system was more economical than the plaque assay for the evaluation of comparable samples. Using roller bottles required less time and manipulation than the plaque procedure and greatly facilitated the examination of large numbers of samples. The combination of the improved filter elution procedure and the roller bottle assay for viral analysis makes large-scale virus studies of groundwater systems practical. This procedure was subsequently field tested during a groundwater study in which large-volume samples (exceeding 800 L) were processed through the filters.

PHYSIOLOGICALLY BASED EXTRACTION PROCEDURE: COMPARISON OF FIVE FLUIDS

EPA Science Inventory

Traditionally, the performance of soil remediation technologies has been evaluated based on the total amount of extractable contaminants. However, some have argued that remedial treatments may alter the bioavailability as well as the mass of contaminants. For example, it has been...

19 CFR 191.102 - Procedure.

Code of Federal Regulations, 2010 CFR

2010-04-01

... (CONTINUED) DRAWBACK Internal Revenue Tax on Flavoring Extracts and Medicinal or Toilet Preparations... medicinal or toilet preparations on which drawback is claimed shall record the products manufactured, the... than 5 percent. If the percentage of alcohol contained in a medicinal preparation, flavoring extract or...

Minimally Invasive Catheter Procedures to Assist Complicated Pacemaker Lead Extraction and Implantation in the Operating Room

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kroepil, Patric; Lanzman, Rotem S., E-mail: rotemshlomo@yahoo.de; Miese, Falk R.

2011-04-15

We report on percutaneous catheter procedures in the operating room (OR) to assist complicated manual extraction or insertion of pacemaker (PM) and implantable cardioverter defibrillator leads. We retrospectively reviewed complicated PM revisions and implantations performed between 2004 and 2009 that required percutaneous catheter procedures performed in the OR. The type of interventional procedure, catheter and retrieval system used, venous access, success rates, and procedural complications were analyzed. In 41 (12 female and 29 male [mean age 62 {+-} 17 years]) of 3021 (1.4%) patients, standard manual retrieval of old leads or insertion of new leads was not achievable and thusmore » required percutaneous catheter intervention for retrieval of misplaced leads and/or recanalisation of occluded central veins. Thirteen of 18 (72.2%) catheter-guided retrieval procedures for misplaced (right atrium [RA] or ventricle [RV; n = 3], superior vena cava [n = 2], brachiocephalic vein [n = 5], and subclavian vein [n = 3]) lead fragments in 16 patients were successful. Percutaneous catheter retrieval failed in five patients because there were extremely fixed or adhered lead fragments. Percutaneous transluminal angiography (PTA) of central veins for occlusion or high-grade stenosis was performed in 25 patients. In 22 of 25 patients (88%), recanalization of central veins was successful, thus enabling subsequent lead replacement. Major periprocedural complications were not observed. In the case of complicated manual PM lead implantation or revision, percutaneous catheter-guided extraction of misplaced lead fragments or recanalisation of central veins can be performed safely in the OR, thus enabling subsequent implantation or revision of PM systems in the majority of patients.« less

Microwave-assisted extraction of coumarin and related compounds from Melilotus officinalis (L.) Pallas as an alternative to Soxhlet and ultrasound-assisted extraction.

PubMed

Martino, Emanuela; Ramaiola, Ilaria; Urbano, Mariangela; Bracco, Francesco; Collina, Simona

2006-09-01

Soxhlet extraction, ultrasound-assisted extraction (USAE) and microwaves-assisted extraction (MAE) in closed system have been investigated to determine the content of coumarin, o-coumaric and melilotic acids in flowering tops of Melilotus officinalis. The extracts were analyzed with an appropriate HPLC procedure. The reproducibility of extraction and of chromatographic analysis was proved. Taking into account the extraction yield, the cost and the time, we studied the effects of extraction variables on the yield of the above-mentioned compounds. Better results were obtained with MAE (50% v/v aqueous ethanol, two heating cycles of 5 min, 50 degrees C). On the basis of the ratio extraction yield/extraction time, we therefore propose MAE as the most efficient method.

Determination of parabens and endocrine-disrupting alkylphenols in soil by gas chromatography-mass spectrometry following matrix solid-phase dispersion or in-column microwave-assisted extraction: a comparative study.

PubMed

Pérez, R A; Albero, B; Miguel, E; Sánchez-Brunete, C

2012-03-01

Two rapid methods were evaluated for the simultaneous extraction of seven parabens and two alkylphenols from soil based on matrix solid-phase dispersion (MSPD) and microwave-assisted extraction (MAE). Soil extracts were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide and analyzed by gas chromatography with mass spectrometry. Extraction and clean-up of samples were carried out by both methods in a single step. A glass sample holder, inside the microwave cell, was used in MAE to allow the simultaneous extraction and clean-up of samples and shorten the MAE procedure. The detection limits achieved by MSPD were lower than those obtained by MAE because the presence of matrix interferences increased with this extraction method. The extraction yields obtained by MSPD and MAE for three different types of soils were compared. Both procedures showed good recoveries and sensitivity for the determination of parabens and alkylphenols in two of the soils assayed, however, only MSPD yielded good recoveries with the other soil. Finally, MSPD was applied to the analysis of soils collected in different sites of Spain. In most of the samples analyzed, methylparaben and butylparaben were detected at levels ranging from 1.21 to 8.04 ng g(-1) dry weight and 0.48 to 1.02 ng g(-1) dry weight, respectively.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR ARCHIVE PROCEDURE FOR STUDY SAMPLES (UA-G-4.0)

EPA Science Inventory

The purpose of this SOP is to outline the archive/custody guidelines used by the Arizona Border Study. This procedure was followed to maintain and locate samples, extracts, tracings and hard copy results after laboratory analysis during the Arizona NHEXAS project and the Border ...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR ANALYSIS OF VOLATILE ORGANIC COMPOUNDS COLLECTED WITH A PASSIVE SAMPLER (BCO-L-17.1)

EPA Science Inventory

The purpose of this SOP is to describe the methodology used for the analysis of the 3M OVM 3500 Organic Vapor Monitors for volatile organic compounds (VOCs), using solvent extraction and standard gas chromatography/mass spectrometry (GC/MS) analysis procedures. This procedure was...

Comparison of Astigmatic Correction after Femtosecond Lenticule Extraction and Small-Incision Lenticule Extraction for Myopic Astigmatism

PubMed Central

Kobashi, Hidenaga; Kamiya, Kazutaka; Ali, Mohamed A.; Igarashi, Akihito; Elewa, Mohamed Ehab M.; Shimizu, Kimiya

2015-01-01

Purpose To compare postoperative astigmatic correction between femtosecond lenticule extraction (FLEx) and small-incision lenticule extraction (SMILE) in eyes with myopic astigmatism. Methods We examined 26 eyes of 26 patients undergoing FLEx and 26 eyes of 26 patients undergoing SMILE to correct myopic astigmatism (manifest astigmatism of 1 diopter (D) or more). Visual acuity, cylindrical refraction, the predictability of the astigmatic correction, and the astigmatic vector components using Alpin’s method, were compared between the two groups 3 months postoperatively. Results We found no statistically significant difference in manifest cylindrical refraction (p=0.74) or in the percentage of eyes within ± 0.50 D of their refraction (p=0.47) after the two surgical procedures. Moreover, no statistically significant difference was detected between the groups in astigmatic vector components, namely, surgically induced astigmatism (0.80), target induced astigmatism (p=0.87), astigmatic correction index (p=0.77), angle of error (p=0.24), difference vector (p=0.76), index of success (p=0.91), flattening effect (p=0.79), and flattening index (p=0.84). Conclusions Both FLEx and SMILE procedures are essentially equivalent in correcting myopic astigmatism using vector analysis, suggesting that the lifting or non-lifting of the flap does not significantly affect astigmatic outcomes after these surgical procedures. PMID:25849381

Rapid virus detection procedure for molecular tracing of shellfish associated with disease outbreaks.

PubMed

de Roda Husman, Ana Maria; Lodder-Verschoor, Froukje; van den Berg, Harold H J L; Le Guyader, Françoise S; van Pelt, Hilde; van der Poel, Wim H M; Rutjes, Saskia A

2007-04-01

Detection of pathogenic viruses in oysters implicated in gastroenteritis outbreaks is often hampered by time-consuming, specialist virus extraction methods. Five virus RNA extraction methods were evaluated with respect to performance characteristics and sensitivity on artificially contaminated oyster digestive glands. The two most promising procedures were further evaluated on bioaccumulated and naturally contaminated oysters. The most efficient method was used to trace the source in an outbreak situation. Out of five RNA extraction protocols, PEG precipitation and the RNeasy Kit performed best with norovirus genogroup III-spiked digestive glands. Analyzing 24-h bioaccumulated oysters revealed a slightly better sensitivity with PEG precipitation, but the RNeasy Kit was less prone to concentrate inhibitors. The latter procedure demonstrated the presence of human noroviruses in naturally contaminated oysters and oysters implicated in an outbreak. In this outbreak, in four out of nine individually analyzed digestive glands, norovirus was detected. In one of the oysters and in one of the fecal samples of the clinical cases, identical norovirus strains were detected. A standard and rapid virus extraction method using the RNeasy Kit appeared to be most useful in tracing shellfish as the source in gastroenteritis outbreaks, and to be able to make effective and timely risk management decisions.

Assessing Metal Mobilization from Industrially Lead-Contaminated Soils Located at an Urban Site

EPA Science Inventory

A series of leaching and partitioning tests (Toxicity Characteristic Leaching Procedure (TCLP), Synthetic Precipitation Leaching Procedure (SPLP), Controlled Acidity Leaching Protocol (CALP), Acid Neutralization Capacity (ANC), and sequential extraction) were applied to three dif...

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

PubMed Central

Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

2018-01-01

Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

The loss of essential oil components induced by the Purge Time in the Pressurized Liquid Extraction (PLE) procedure of Cupressus sempervirens.

PubMed

Dawidowicz, Andrzej L; Czapczyńska, Natalia B; Wianowska, Dorota

2012-05-30

The influence of different Purge Times on the effectiveness of Pressurized Liquid Extraction (PLE) of volatile oil components from cypress plant matrix (Cupressus sempervirens) was investigated, applying solvents of diverse extraction efficiencies. The obtained results show the decrease of the mass yields of essential oil components as a result of increased Purge Time. The loss of extracted components depends on the extrahent type - the greatest mass yield loss occurred in the case of non-polar solvents, whereas the smallest was found in polar extracts. Comparisons of the PLE method with Sea Sand Disruption Method (SSDM), Matrix Solid-Phase Dispersion Method (MSPD) and Steam Distillation (SD) were performed to assess the method's accuracy. Independent of the solvent and Purge Time applied in the PLE process, the total mass yield was lower than the one obtained for simple, short and relatively cheap low-temperature matrix disruption procedures - MSPD and SSDM. Thus, in the case of volatile oils analysis, the application of these methods is advisable. Copyright © 2012 Elsevier B.V. All rights reserved.

Percutaneous Lead Extraction in Infection of Cardiac Implantable Electronic Devices: a Systematic Review

PubMed Central

Menezes Júnior, Antônio da Silva; Magalhães, Thaís Rodrigues; Morais, Alana de Oliveira Alarcão

2018-01-01

Introduction In the last two decades, the increased number of implants of cardiac implantable electronic devices has been accompanied by an increase in complications, especially infection. Current recommendations for the appropriate treatment of cardiac implantable electronic devices-related infections consist of prolonged antibiotic therapy associated with complete device extraction. The purpose of this study was to analyze the importance of percutaneous extraction in the treatment of these devices infections. Methods A systematic review search was performed in the PubMed, BVS, Cochrane CENTRAL, CAPES, SciELO and ScienceDirect databases. A total of 1,717 studies were identified and subsequently selected according to the eligibility criteria defined by relevance tests by two authors working independently. Results Sixteen studies, describing a total of 3,354 patients, were selected. Percutaneous extraction was performed in 3,081 patients. The average success rate for the complete percutaneous removal of infected devices was 92.4%. Regarding the procedure, the incidence of major complications was 2.9%, and the incidence of minor complications was 8.4%. The average in-hospital mortality of the patients was 5.4%, and the mortality related to the procedure ranged from 0.4 to 3.6%. The mean mortality was 20% after 6 months and 14% after a one-year follow-up. Conclusion Percutaneous extraction is the main technique for the removal of infected cardiac implantable electronic devices, and it presents low rates of complications and mortality related to the procedure.

Xanthium strumarium extract inhibits mammalian cell proliferation through mitotic spindle disruption mediated by xanthatin.

PubMed

Sánchez-Lamar, Angel; Piloto-Ferrer, Janet; Fiore, Mario; Stano, Pasquale; Cozzi, Renata; Tofani, Daniela; Cundari, Enrico; Francisco, Marbelis; Romero, Aylema; González, Maria L; Degrassi, Francesca

2016-12-24

Xanthium strumarium L. is a member of the Asteraceae family popularly used with multiple therapeutic purposes. Whole extracts of this plant have shown anti-mitotic activity in vitro suggesting that some components could induce mitotic arrest in proliferating cells. Aim of the present work was to characterize the anti-mitotic properties of the X. strumarium whole extract and to isolate and purify active molecule(s). The capacity of the whole extract to inhibit mitotic progression in mammalian cultured cells was investigated to identify its anti-mitotic activity. Isolation of active component(s) was performed using a bioassay-guided multistep separation procedure in which whole extract was submitted to a progressive process of fractionation and fractions were challenged for their anti-mitotic activity. Our results show for the first time that X. strumarium whole extract inhibits assembly of the mitotic spindle and spindle-pole separation, thereby heavily affecting mitosis, impairing the metaphase to anaphase transition and inducing apoptosis. The purification procedure led to a fraction with an anti-mitotic activity comparable to that of the whole extract. Chemical analysis of this fraction showed that its major component was xanthatin. The present work shows a new activity of X. strumarium extract, i.e. the alteration of the mitotic apparatus in cultured cells that may be responsible for the anti-proliferative activity of the extract. Anti-mitotic activity is shown to be mainly exerted by xanthatin. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Comparative study between extraction techniques and column separation for the quantification of sinigrin and total isothiocyanates in mustard seed.

PubMed

Cools, Katherine; Terry, Leon A

2012-07-15

Glucosinolates are β-thioglycosides which are found naturally in Cruciferae including the genus Brassica. When enzymatically hydrolysed, glucosinolates yield isothiocyanates and give a pungent taste. Both glucosinolates and isothiocyanates have been linked with anticancer activity as well as antifungal and antibacterial properties and therefore the quantification of these compounds is scientifically important. A wide range of literature exists on glucosinolates, however the extraction and quantification procedures differ greatly resulting in discrepancies between studies. The aim of this study was therefore to compare the most popular extraction procedures to identify the most efficacious method and whether each extraction can also be used for the quantification of total isothiocyanates. Four extraction techniques were compared for the quantification of sinigrin from mustard cv. Centennial (Brassica juncea L.) seed; boiling water, boiling 50% (v/v) aqueous acetonitrile, boiling 100% methanol and 70% (v/v) aqueous methanol at 70 °C. Prior to injection into the HPLC, the extractions which involved solvents (acetonitrile or methanol) were freeze-dried and resuspended in water. To identify whether the same extract could be used to measure total isothiocyanates, a dichloromethane extraction was carried out on the sinigrin extracts. For the quantification of sinigrin alone, boiling 50% (v/v) acetonitrile was found to be the most efficacious extraction solvent of the four tested yielding 15% more sinigrin than the water extraction. However, the removal of the acetonitrile by freeze-drying had a negative impact on the isothiocyanate content. Quantification of both sinigrin and total isothiocyanates was possible when the sinigrin was extracted using boiling water. Two columns were compared for the quantification of sinigrin revealing the Zorbax Eclipse to be the best column using this particular method. Copyright © 2012 Elsevier B.V. All rights reserved.

Automatic digital surface model (DSM) generation from aerial imagery data

NASA Astrophysics Data System (ADS)

Zhou, Nan; Cao, Shixiang; He, Hongyan; Xing, Kun; Yue, Chunyu

2018-04-01

Aerial sensors are widely used to acquire imagery for photogrammetric and remote sensing application. In general, the images have large overlapped region, which provide a lot of redundant geometry and radiation information for matching. This paper presents a POS supported dense matching procedure for automatic DSM generation from aerial imagery data. The method uses a coarse-to-fine hierarchical strategy with an effective combination of several image matching algorithms: image radiation pre-processing, image pyramid generation, feature point extraction and grid point generation, multi-image geometrically constraint cross-correlation (MIG3C), global relaxation optimization, multi-image geometrically constrained least squares matching (MIGCLSM), TIN generation and point cloud filtering. The image radiation pre-processing is used in order to reduce the effects of the inherent radiometric problems and optimize the images. The presented approach essentially consists of 3 components: feature point extraction and matching procedure, grid point matching procedure and relational matching procedure. The MIGCLSM method is used to achieve potentially sub-pixel accuracy matches and identify some inaccurate and possibly false matches. The feasibility of the method has been tested on different aerial scale images with different landcover types. The accuracy evaluation is based on the comparison between the automatic extracted DSMs derived from the precise exterior orientation parameters (EOPs) and the POS.

Incidence and Characteristics of Cataract Surgery in Poland, during 2010-2015.

PubMed

Nowak, Michał S; Grabska-Liberek, Iwona; Michalska-Małecka, Katarzyna; Grzybowski, Andrzej; Kozioł, Milena; Niemczyk, Wojciech; Więckowska, Barbara; Szaflik, Jacek P

2018-03-02

Background: To assess the incidence and characteristic of cataract surgery in Poland from 2010 to 2015 and to interpret these findings. Patients and methods: Data from all patients who underwent cataract surgery alone or in combined procedures in Poland between January 2010 and December 2015 were evaluated. Patient data were from the national database of hospitalizations maintained by National Health Fund. Data on the population of Poland were obtained from Central Statistical Office of Poland. Results: In total, 1,218,777 cataract extractions (alone or combined with other procedures) were performed in 1,081,345 patients during 2010-2015. Overall, the incidence of cataract surgery increased from 5.22/1000 person-years in 2010 to 6.17/1000 person-years in 2015. Phacoemulsification was performed in 97.46% of cataract extractions, and 3.02% of cataract extractions were combined procedures. The rate of one-day procedures increased from 28.3% in 2010 to 43.1% in 2015. The probability of second-eye surgery 12 months after the first-eye surgery increased from 44% in 2010 to 73% in 2015 (log-rank test p < 0.0001). Conclusion: In Poland, from 2010 to 2015, the total incidence of cataract surgery, the number of people who underwent surgery, and the number of one-day cataract surgeries increased significantly.

Loop-mediated isothermal amplification with the Procedure for Ultra Rapid Extraction kit for the diagnosis of pneumocystis pneumonia.

PubMed

Kawano, Shuichi; Maeda, Takuya; Suzuki, Takefumi; Abe, Tatsuhiro; Mikita, Kei; Hamakawa, Yusuke; Ono, Takeshi; Sonehara, Wataru; Miyahira, Yasushi; Kawana, Akihiko

2015-03-01

Loop-mediated isothermal amplification (LAMP) is an innovative molecular technique requiring only a heating device and isothermal conditions to amplify a specific target gene. The results of current microscopic diagnostic tools for pneumocystis pneumonia are not sufficiently consistent for detecting infection with a low-density of Pneumocystis jirovecii. Although polymerase chain reaction (PCR) is highly sensitive, it is not suitable for resource-limited facilities. LAMP is a potential diagnostic replacement for PCR in such settings but a critical disadvantage of DNA extraction was still remained. Therefore, we employed the Procedure for Ultra Rapid Extraction (PURE) kit, which uses a porous material, to isolate the DNA from clinical samples in a simple way in combination with previously reported LAMP procedure for diagnosing PCP. The detection limit of the PURE-LAMP method applied to artificial bronchoalveolar lavage fluid samples was 100 copies/tube, even with the use of massive blood-contaminated solutions. In addition, we concluded the diagnostic procedure within 1 h without the need for additional equipment. PURE-LAMP coupled with suitable primers for specific pathogens has good potential for diagnosing various infectious diseases. Copyright © 2014 Japanese Society of Chemotherapy and The Japanese Association for Infectious Diseases. Published by Elsevier Ltd. All rights reserved.

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2011 CFR

2011-07-01

... PROHIBITIONS Self-Implementing Alternative Extraction and Chemical Analysis Procedures for Non-liquid PCB Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a... of use in this chemical extraction and chemical analysis comparison study, a person may adjust PCB...

Biofabrication of Ag nanoparticles using Moringa oleifera leaf extract and their antimicrobial activity

PubMed Central

Prasad, TNVKV; Elumalai, EK

2011-01-01

Objective To formulate a simple rapid procedure for bioreduction of silver nanoparticles using aqueous leaves extract of Moringa oleifera (M. oleifera). Methods 10 mL of leaf extract was mixed to 90 mL of 1 mM aqueous of AgNO3 and was heated at 60 - 80 °C for 20 min. A change from brown to reddish color was observed. Characterization using UV-Vis spectrophotometry, Transmission Electron Microscopy (TEM) was performed. Results TEM showed the formation of silver nanoparticles with an average size of 57 nm. Conclusions M. oleifera demonstrates strong potential for synthesis of silver nanoparticles by rapid reduction of silver ions (Ag+ to Ag0). Biological methods are good competents for the chemical procedures, which are eco-friendly and convenient. PMID:23569809

Is the HAS-BLED score useful in predicting post-extraction bleeding in patients taking warfarin? A retrospective cohort study

PubMed Central

Kataoka, Toshiyuki; Hoshi, Keika; Ando, Tomohiro

2016-01-01

Objective Unexpected post-extraction bleeding is often experienced in clinical practice. Therefore, determining the risk of post-extraction bleeding in patients receiving anticoagulant therapy prior to surgery is beneficial. This study aimed to verify whether the HAS-BLED score was useful in predicting post-extraction bleeding in patients taking warfarin. Design Retrospective cohort study. Setting Department of Oral and Maxillofacial Surgery, Tokyo Women's Medical University. Participants Participants included 258 sequential cases (462 teeth) who had undergone tooth extraction between 1 January 2010 and 31 December 2012 while continuing warfarin therapy. Main outcome measure Post-extraction risk factors for bleeding. The following data were collected as the predicting variables for multivariate logistic analysis: the HAS-BLED score, extraction site, tooth type, stability of teeth, extraction procedure, prothrombin time-international normalised ratio value, platelet count and the use of concomitant antiplatelet agents. Results Post-extraction bleeding was noted in 21 (8.1%) of the 258 cases. Haemostasis was achieved with localised haemostatic procedures in all the cases of post-extraction bleeding. The HAS-BLED score was found to be insufficient in predicting post-extraction bleeding (area under the curve=0.548, p=0.867, multivariate analysis). The risk of post-extraction bleeding was approximately three times greater in patients taking concomitant oral antiplatelet agents (risk ratio=2.881, p=0.035, multivariate analysis). Conclusions The HAS-BLED score alone could not predict post-extraction bleeding. The concomitant use of oral antiplatelet agents was a risk factor for post-extraction bleeding. No episodes of post-extraction bleeding required more than local measures for haemostasis. However, because this was a retrospective study conducted at a single institution, large-scale prospective cohort studies, which include cases of outpatient tooth extraction, will be necessary in the future. PMID:26936909

Performance of different mono- and multiplex nucleic acid amplification tests on a multipathogen external quality assessment panel.

PubMed

Loens, K; van Loon, A M; Coenjaerts, F; van Aarle, Y; Goossens, H; Wallace, P; Claas, E J C; Ieven, M

2012-03-01

An external quality assessment (EQA) panel consisting of a total of 48 samples in bronchoalveolar lavage (BAL) fluid or transport medium was prepared in collaboration with Quality Control for Molecular Diagnostics (QCMD) (www.qcmd.org). The panel was used to assess the proficiency of the three laboratories that would be responsible for examining the 6,000 samples to be collected in the GRACE Network of Excellence (www.grace-lrti.org). The main objective was to decide on the best-performing testing approach for the detection of influenza viruses A and B, parainfluenza virus types 1 to 3, respiratory syncytial virus (RSV), human metapneumovirus, coronavirus, rhinovirus, adenovirus, Chlamydophila pneumoniae, Mycoplasma pneumoniae, and Legionella pneumophila by nucleic acid amplification techniques (NAATs). Two approaches were chosen: (i) laboratories testing samples using their in-house procedures for extraction and amplification and (ii) laboratories using their in-house amplification procedures on centrally extracted samples. Furthermore, three commercially available multiplex NAAT tests-the ResPlex (Qiagen GmbH, Hilden, Germany), RespiFinder plus (PathoFinder, Maastricht, The Netherlands), and RespiFinder Smart 21 (PathoFinder) tests-were evaluated by examination of the same EQA panel by the manufacturer. No large differences among the 3 laboratories were noticed when the performances of the assays developed in-house in combination with the in-house extraction procedures were compared. Also, the extraction procedure (central versus local) had little effect on performance. However, large differences in amplification efficacy were found between the commercially available tests; acceptable results were obtained by using the PathoFinder assays.

A multiplexed microfluidic toolbox for the rapid optimization of affinity-driven partition in aqueous two phase systems.

PubMed

Bras, Eduardo J S; Soares, Ruben R G; Azevedo, Ana M; Fernandes, Pedro; Arévalo-Rodríguez, Miguel; Chu, Virginia; Conde, João P; Aires-Barros, M Raquel

2017-09-15

Antibodies and other protein products such as interferons and cytokines are biopharmaceuticals of critical importance which, in order to be safely administered, have to be thoroughly purified in a cost effective and efficient manner. The use of aqueous two-phase extraction (ATPE) is a viable option for this purification, but these systems are difficult to model and optimization procedures require lengthy and expensive screening processes. Here, a methodology for the rapid screening of antibody extraction conditions using a microfluidic channel-based toolbox is presented. A first microfluidic structure allows a simple negative-pressure driven rapid screening of up to 8 extraction conditions simultaneously, using less than 20μL of each phase-forming solution per experiment, while a second microfluidic structure allows the integration of multi-step extraction protocols based on the results obtained with the first device. In this paper, this microfluidic toolbox was used to demonstrate the potential of LYTAG fusion proteins used as affinity tags to optimize the partitioning of antibodies in ATPE processes, where a maximum partition coefficient (K) of 9.2 in a PEG 3350/phosphate system was obtained for the antibody extraction in the presence of the LYTAG-Z dual ligand. This represents an increase of approx. 3.7 fold when compared with the same conditions without the affinity molecule (K=2.5). Overall, this miniaturized and versatile approach allowed the rapid optimization of molecule partition followed by a proof-of-concept demonstration of an integrated back extraction procedure, both of which are critical procedures towards obtaining high purity biopharmaceuticals using ATPE. Copyright © 2017 Elsevier B.V. All rights reserved.

Situation Tracking in Large Data Streams

DTIC Science & Technology

2015-02-01

Pike, R. 1989: Different Ways to Cue a Coherent Memory System: A Theory for Episodic , Semantic , and Procedural Tasks. Psychological Review, 96(2), 208...to extract general concept models, such as Latent Semantic Indexing. This technique generally extracts a single topic model, and does not extract a...2001. Semantic leaps: frame-shifting and conceptual blending in meaning construction. Cambridge University Press. Humphreys, M. S, Bain, J. D

A rapid and reliable procedure for extraction of cellular polyamines and inorganic ions from plant tissues

Treesearch

Rakesh Minocha; Walter C. Shortle; Stephanie L. Long; Subhash C. Minocha

1994-01-01

A fast and reliable method for the extraction of cellular polyamines and major inorganic ions (Ca, Mg, Mn, K, and P) from several plant tissues is described. The method involves repeated freezing and thawing of samples instead of homogenization. The efficiency of extraction of both the polyamines and inorganic ions by these two methods was compared for 10 different...

Creation of the sole regional laser lead extraction program serving Atlantic Canada: initial experience

PubMed Central

Williams, Kenneth J.; O’Keefe, Scott; Légaré, Jean-Francois

2016-01-01

Background An increasing need for laser lead extraction has grown in parallel with the increase of implantation of pacing and defibrillating devices. We reviewed the initial experience of a regional laser-assisted lead extraction program serving Atlantic Canada. Methods We retrospectively reviewed the cases of all consecutive patients who underwent laser lead extraction at the Maritime Heart Centre in Halifax, NS, between 2006 and 2015. We conducted univariate and Kaplan–Meier survivorship analyses. Results During the 9-year study period, 108 consecutive patients underwent laser lead extractions (218 leads extracted). The most common indication for extraction was infection (84.3%). Most patients were older than 60 years (73.1%) and had leads chronically implanted; the explanted leads were an average of 7.5 ± 6.8 years old. Procedural and clinical success (resolution of preoperative symptoms) rates and mortality were 96.8%, 97.2%, and 0.9%, respectively. Sternotomy procedures were performed in 3 instances: once for vascular repair due to perforation and twice to ensure that all infected lead material was removed. No minor complications required surgical intervention. Survival after discharge was 98.4% at 30 days and 94% at 12 months. Conclusion Atlantic Canada’s sole surgical extraction centre achieved high extraction success with a low complication rate. Lead extraction in an operative setting provides for immediate surgical intervention and is essential for the survival of patients with complicated cases. Surgeons must weigh the risks versus benefits in patients older than 60 years who have chronically implanted leads (> 1 yr) and infection. PMID:26999473

Microwave-assisted extraction and ultrasonic extraction to determine polycyclic aromatic hydrocarbons in needles and bark of Pinus pinaster Ait. and Pinus pinea L. by GC-MS.

PubMed

Ratola, Nuno; Lacorte, Sílvia; Barceló, Damià; Alves, Arminda

2009-01-15

Two different extraction strategies (microwave-assisted extraction (MAE) and ultrasonic extraction (USE)) were tested in the extraction of the 16 US Environmental Protection Agency (EPA) polycyclic aromatic hydrocarbons (PAHs) from pine trees. Extraction of needles and bark from two pine species common in the Iberian Peninsula (Pinus pinaster Ait. and Pinus pinea L.) was optimized using two amounts of sample (1g and 5 g) and two PAHs spiking levels (20 ng/g and 100 ng/g). In all cases, the clean-up procedure following extraction consisted in solid-phase extraction (SPE) with alumina cartridges. Quantification was done by gas chromatography (GC) with mass spectrometry (MS), using five deuterated PAH surrogate standards as internal standards. Limits of detection were globally below 0.2 ng/g. The method was robust for the matrices studied regardless of the extraction procedures. Recovery values between 70 and 130% were reached in most cases, except for high molecular weight PAHs (indeno[1,2,3-cd]pyrene, dibenzo[a,h]anthracene and benzo[ghi]perylene). A field study with naturally contaminated samples from eight sites (four in Portugal and four in Catalonia, Spain) showed that needles are more suitable biomonitors for PAHs, yielding concentrations from 2 to 17 times higher than those found in bark. The levels varied according to the sampling site, with the sum of the individual PAH concentrations between 213 and 1773 ng/g (dry weight). Phenanthrene was the most abundant PAH, followed by fluoranthene, naphthalene and pyrene.

Spectrophotometric determination of molybdenum in rocks with thiocyanate

USGS Publications Warehouse

Lillie, E.G.; Greenland, L.P.

1974-01-01

A rapid procedure for the determination of microgram amounts of molybdenum in rocks is described. After acid decomposition, molybdenum is extracted from a hydrochloric acid solution into xylene with tributyl phosphate. After back-extraction with water, molybdenum is extracted as the ??-benzoinoximate into chloroform, stripped into hydrochloric acid extracted as the thiocyanate into amyl alcohol, and determined spectrophotometrically. The molybdenum thiocyanate color produced is stable, sensitive, and reproducible. Results of analyses of several of the U.S. Geological Survey standard rocks are given. ?? 1974.

High-speed RNA microextraction technology using magnetic oligo-dT beads and lateral magnetophoresis.

PubMed

Lee, Hwanyong; Jung, Jinhee; Han, Song-I; Han, Ki-Ho

2010-10-21

This paper presents a high-speed RNA microextractor for the direct isolation of RNA from peripheral blood lysate using magnetic oligo-dT beads. The extraction is achieved through lateral magnetophoresis, generated by a ferromagnetic wire array inlaid on a glass substrate. This RNA microextractor separated more than 80% of magnetic beads with a flow rate up to 20 ml h(-1), and the overall extraction procedure was completed within 1 min. The absorbance ratio of RNA to protein (A(260)/A(280)) was >1.7, indicating that the extraction technology yielded nearly pure RNA. The feasibility of this technique was evaluated further for its applicability to reverse transcription polymerase chain reaction (RT-PCR) procedures by performing cDNA synthesis and PCR. The analysis verified that the RNA microextractor is a practical method for easy, rapid, and high-precision RT-PCR using minimal reagent volumes without requiring highly trained personnel. In addition, it can be readily incorporated into genetic analysis procedures for realizing automated on-chip genetic platforms in a micro format.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and {alpha}-Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Goldstein, S.J.; Hensley, C.A.; Armenta, C.E.

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for {alpha}-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of `real` environmental and bioassaymore » samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of {approx}2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously. 24 refs., 2 figs., 2 tabs.« less

Automatic Generation of Conditional Diagnostic Guidelines.

PubMed

Baldwin, Tyler; Guo, Yufan; Syeda-Mahmood, Tanveer

2016-01-01

The diagnostic workup for many diseases can be extraordinarily nuanced, and as such reference material text often contains extensive information regarding when it is appropriate to have a patient undergo a given procedure. In this work we employ a three task pipeline for the extraction of statements indicating the conditions under which a procedure should be performed, given a suspected diagnosis. First, we identify each instance in the text where a procedure is being recommended. Next we examine the context around these recommendations to extract conditional statements that dictate the conditions under which the recommendation holds. Finally, corefering recommendations across the document are linked to produce a full recommendation summary. Results indicate that each underlying task can be performed with above baseline performance, and the output can be used to produce concise recommendation summaries.

Assessment of simple colorimetric procedures to determine smoking status of diabetic subjects.

PubMed

Smith, R F; Mather, H M; Ellard, G A

1998-02-01

The performance of a simple colorimetric assay for urinary nicotine metabolites to assess smoking status in diabetic subjects (n = 251) was investigated. Several variations of the colorimetric assay and a qualitative extraction procedure were evaluated in comparison with a cotinine immunoassay as the "gold standard." Among these, the best overall performance was achieved with the qualitative test (sensitivity 95%; specificity 100%). The quantitative measurement of total nicotine metabolites performed less well (sensitivity 92%; specificity 97%) but could be improved by incorporating a blank extraction (sensitivity 98%; specificity 98%). Allowance for diuresis appeared to offer no advantage over the other methods. These results support previous findings regarding the use of these colorimetric procedures in nondiabetic subjects and, contrary to other recent observations, their performance was not impaired in diabetic patients.

An improved procedure for shipboard enumeration of faecal indicator bacteria in marine sediments from sewage sludge disposal areas.

PubMed

West, P A

1988-04-01

An improved membrane filtration procedure for use on board ship to enumerate Escherichia coli and Group D faecal streptococci in marine sediments is described. Ultrasonication extraction combined with resuscitation of sublethally-injured cells yielded significantly higher counts of E. coli than sediments shaken by hand. Counts of E. coli were also higher on mFC agar (without rosalic acid) after a period of resuscitation on tryptone-soy agar supplemented with 0.1% yeast extract than on a 4% Teepol-lactose medium. Ultrasonication of sediments made no significant difference to counts of Group D faecal streptococci on KF-streptococcus agar. These improved isolation procedures allowed better discrimination of the area affected by sewage sludge at a disposal site off the northeast coast of England.

Evaluating bis(2-ethylhexyl) methanediphosphonic acid (H 2DEH[MDP]) based polymer ligand film (PLF) for plutonium and uranium extraction

DOE PAGES

Rim, Jung H.; Armenta, Claudine E.; Gonzales, Edward R.; ...

2015-09-12

This paper describes a new analyte extraction medium called polymer ligand film (PLF) that was developed to rapidly extract radionuclides. PLF is a polymer medium with ligands incorporated in its matrix that selectively and quickly extracts analytes. The main focus of the new technique is to shorten and simplify the procedure for chemically isolating radionuclides for determination through alpha spectroscopy. The PLF system was effective for plutonium and uranium extraction. The PLF was capable of co-extracting or selectively extracting plutonium over uranium depending on the PLF composition. As a result, the PLF and electrodeposited samples had similar alpha spectra resolutions.

U.S. Geological Survey Noble Gas Laboratory’s standard operating procedures for the measurement of dissolved gas in water samples

USGS Publications Warehouse

Hunt, Andrew G.

2015-08-12

This report addresses the standard operating procedures used by the U.S. Geological Survey’s Noble Gas Laboratory in Denver, Colorado, U.S.A., for the measurement of dissolved gases (methane, nitrogen, oxygen, and carbon dioxide) and noble gas isotopes (helium-3, helium-4, neon-20, neon-21, neon-22, argon-36, argon-38, argon-40, kryton-84, krypton-86, xenon-103, and xenon-132) dissolved in water. A synopsis of the instrumentation used, procedures followed, calibration practices, standards used, and a quality assurance and quality control program is presented. The report outlines the day-to-day operation of the Residual Gas Analyzer Model 200, Mass Analyzer Products Model 215–50, and ultralow vacuum extraction line along with the sample handling procedures, noble gas extraction and purification, instrument measurement procedures, instrumental data acquisition, and calculations for the conversion of raw data from the mass spectrometer into noble gas concentrations per unit mass of water analyzed. Techniques for the preparation of artificial dissolved gas standards are detailed and coupled to a quality assurance and quality control program to present the accuracy of the procedures used in the laboratory.

Assessment of Supercritical Fluid Extraction Use in Whole Sediment Toxicity Identification Evaluations

EPA Science Inventory

In this investigation, supercritical fluid extraction (SFE) with pure CO2 was assessed as a confirmatory tool in Phase III of whole sediment toxicity identification evaluations (TIEs). The SFE procedure was assessed on two reference sediments and three contaminated sediments usi...

Application of FTA technology to extraction of sperm DNA from mixed body fluids containing semen.

PubMed

Fujita, Yoshihiko; Kubo, Shin-ichi

2006-01-01

FTA technology is a novel method designed to simplify the collection, shipment, archiving and purification of nucleic acids from a wide variety of biological sources. In this study, we report a rapid and simple method of extracting DNA from sperm when body fluids mixed with semen were collected using FTA cards. After proteinase K digestion of the sperm and body fluid mixture, the washed pellet suspension as the sperm fraction and the concentrated supernatant as the epithelial cell fraction were respectively applied to FTA cards containing DTT. The FTA cards were dried, then directly added to a polymerase chain reaction (PCR) mix and processed by PCR. The time required from separation of the mixed fluid into sperm and epithelial origin DNA extractions was only about 2.5-3h. Furthermore, the procedure was extremely simple. It is considered that our designed DNA extraction procedure using an FTA card is available for application to routine work.

A non-invasive technique for rapid extraction of DNA from fish scales.

PubMed

Kumar, Ravindra; Singh, Poonam Jayant; Nagpure, N S; Kushwaha, Basdeo; Srivastava, S K; Lakra, W S

2007-11-01

DNA markers are being increasingly used in studies related to population genetics and conservation biology of endangered species. DNA isolation for such studies requires a source of biological material that is easy to collect, non-bulky and reliable. Further, the sampling strategies based on non-invasive procedures are desirable, especially for the endangered fish species. In view of above, a rapid DNA extraction method from fish scales has been developed with the use of a modified lysis buffer that require about 2 hr duration. This methodology is non-invasive, less expensive and reproducible with high efficiency of DNA recovery. The DNA extracted by this technique, have been found suitable for performing restriction enzyme digestion and PCR amplification. Therefore, the present DNA extraction procedure can be used as an alternative technique in population genetic studies pertaining to endangered fish species. The technique was also found equally effective for DNA isolation from fresh, dried and ethanol preserved scales.

THE ANALYSIS OF URANIUM-ZIRCONIUM ALLOYS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Milner, G.W.C.; Skewies, A.F.

1953-03-01

A satisfactory procedure is described for the analysis of uranium-zirconium alloys containing up to 25% zirconium. It is based on the separation of the zirconium from the uranium by dissolving the cupferron complex of the former element into chloroform. After the evaporation of the solvent from the combined organic extracts, the residue is ignited to zirconium oxide. The latter is then re-dissolved and zirconium is separated from other elements co-extracted in the solvent extraction procedure by precipitation with mandelic acid. The zirconium mandelate is finally ignited to oxide at 960 deg C. The uranium is separated from the aqueous solutionmore » remaining from the cupferron extraction by precipitating with tannin at a pH of 8; the precipitate being removed by filtration and then ignited a t 800 deg C. The residue is dissolved in nitric acid and the uranium is finally determined by precipitating as ammonium diuranate and then igniting to U{sub 3}O{sub 8}. (auth)« less

Utilization of Sunlight into Methane Hydrate Production: Feasibility Study Based on Energy Balance Estimation

NASA Astrophysics Data System (ADS)

Shimada, J.; Shimada, M.; Tsunashima, K.; Aoyama, C.

2017-12-01

Methane hydrate is gaining remarkable attention as future natural gas resource. Collection procedures such as heating, depressurization, and chemical intrusion are being tested, but because of its high cost, they are still under development and not yet implemented. Cost reduction of the procedures cannot be expected as long as fossil fuel is used as power and heat source to extract methane gas from methane hydrate. In this regard, natural energy such as sunlight, wind, tidal, and wave powers should be implemented as energy resources as alternatives of fossil fuels. Using natural energy instead of fossil fuel will also help to prevent global warming. However, only a few proposals have been made regarding extraction methods to use clean natural energy effectively. In this study, authors will present a new extraction method using optical fibers to expose direct sunlight onto methane hydrate, and verify from various standpoints such as energy balance during extraction process and dependency of the environment.

Microdialysis as a New Technique for Extracting Phenolic Compounds from Extra Virgin Olive Oil.

PubMed

Bazzu, Gianfranco; Molinu, Maria Giovanna; Dore, Antonio; Serra, Pier Andrea

2017-03-01

The amount and composition of the phenolic components play a major role in determining the quality of olive oil. The traditional liquid-liquid extraction (LLE) method requires a time-consuming sample preparation to obtain the "phenolic profile" of extra virgin olive oil (EVOO). This study aimed to develop a microdialysis extraction (MDE) as an alternative to the LLE method to evaluate the phenolic components of EVOO. To this purpose, a microdialysis device and dialysis procedure were developed. "Dynamic-oil" microdialysis was performed using an extracting solution (80:20 methanol/water) flow rate of 2 μL min -1 and a constant EVOO stream of 4 μL min -1 . The results indicated a strong positive correlation between MDE and the LLE method, providing a very similar phenolic profile obtained with traditional LLE. In conclusion, the MDE approach, easier and quicker in comparison to LLE, provided a reliable procedure to determine the phenolic components used as a marker of the quality and traceability of EVOO.

Enantioselective extraction of (+)-(S)-citalopram and its main metabolites using a tailor-made stir bar chiral imprinted polymer for their LC-ESI-MS/MS quantitation in urine samples.

PubMed

Unceta, Nora; Gómez-Caballero, Alberto; García, Deiene; Díaz, Goretti; Guerreiro, Antonio; Piletsky, Sergey; Goicolea, M Aránzazu; Barrio, Ramón J

2013-11-15

This paper reports the application of a chiral imprinted polymer (CIP)-coated stir bar for the selective extraction of (+)-(S)-citalopram (SCIT) and its main metabolites, (+)-(S)-desmethylcitalopram (SDCIT) and (+)-(S)-didesmethylcitalopram (SDDCIT), from urine samples. The developed device has been demonstrated to be capable of selectively extracting the three target analytes from urine samples without saturating the imprinted sites. A CIP-coated stir bar sorptive extraction procedure (CIP-SBSE) is proposed for the isolation of SCIT, SDCIT and SDDCIT followed by their subsequent analysis using liquid chromatography ion trap mass spectrometry (LC-ITMS). Deuterated SCIT-d6 was used as an internal standard. The method was validated using a standard procedure, which revealed that a quantification of 5 ng mL(-1) was obtained in urine samples and that the accuracy and precision were within the established values while no matrix effect was observed. Copyright © 2013 Elsevier B.V. All rights reserved.

eCTG: an automatic procedure to extract digital cardiotocographic signals from digital images.

PubMed

Sbrollini, Agnese; Agostinelli, Angela; Marcantoni, Ilaria; Morettini, Micaela; Burattini, Luca; Di Nardo, Francesco; Fioretti, Sandro; Burattini, Laura

2018-03-01

Cardiotocography (CTG), consisting in the simultaneous recording of fetal heart rate (FHR) and maternal uterine contractions (UC), is a popular clinical test to assess fetal health status. Typically, CTG machines provide paper reports that are visually interpreted by clinicians. Consequently, visual CTG interpretation depends on clinician's experience and has a poor reproducibility. The lack of databases containing digital CTG signals has limited number and importance of retrospective studies finalized to set up procedures for automatic CTG analysis that could contrast visual CTG interpretation subjectivity. In order to help overcoming this problem, this study proposes an electronic procedure, termed eCTG, to extract digital CTG signals from digital CTG images, possibly obtainable by scanning paper CTG reports. eCTG was specifically designed to extract digital CTG signals from digital CTG images. It includes four main steps: pre-processing, Otsu's global thresholding, signal extraction and signal calibration. Its validation was performed by means of the "CTU-UHB Intrapartum Cardiotocography Database" by Physionet, that contains digital signals of 552 CTG recordings. Using MATLAB, each signal was plotted and saved as a digital image that was then submitted to eCTG. Digital CTG signals extracted by eCTG were eventually compared to corresponding signals directly available in the database. Comparison occurred in terms of signal similarity (evaluated by the correlation coefficient ρ, and the mean signal error MSE) and clinical features (including FHR baseline and variability; number, amplitude and duration of tachycardia, bradycardia, acceleration and deceleration episodes; number of early, variable, late and prolonged decelerations; and UC number, amplitude, duration and period). The value of ρ between eCTG and reference signals was 0.85 (P < 10 -560 ) for FHR and 0.97 (P < 10 -560 ) for UC. On average, MSE value was 0.00 for both FHR and UC. No CTG feature was found significantly different when measured in eCTG vs. reference signals. eCTG procedure is a promising useful tool to accurately extract digital FHR and UC signals from digital CTG images. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of cocaine in postmortem human liver exposed to overdose. Application of an innovative and efficient extraction/clean up procedure and gas chromatography-mass spectrometry analysis.

PubMed

Magalhães, Elisângela Jaqueline; Ribeiro de Queiroz, Maria Eliana Lopes; Penido, Marcus Luiz de Oliveira; Paiva, Marco Antônio Ribeiro; Teodoro, Janaína Aparecida Reis; Augusti, Rodinei; Nascentes, Clésia Cristina

2013-09-27

A simple and efficient method was developed for the determination of cocaine in post-mortem samples of human liver via solid-liquid extraction with low temperature partitioning (SLE-LTP) and analysis by gas chromatography coupled to mass spectrometry (GC-MS). The extraction procedure was optimized by evaluating the influence of the following variables: pH of the extract, volume and composition of the extractor solvent, addition of a sorbent material (PSA: primary-secondary amine) and NaCl to clean up and increase the ionic strength of the extract. A bovine liver sample that was free of cocaine was used as a blank for the optimization of the SLE-LTP extraction procedure. The highest recovery was obtained when crushed bovine liver (2g) was treated with 2mL of ultrapure water plus 8mL of acetonitrile at physiological pH (7.4). The results also indicated no need for using PSA and NaCl. The complete analytical procedure was validated for the following figures of merit: selectivity, lower limit of quantification (LLOQ), calibration curve, recovery, precision and accuracy (for within-run and between-run experiments), matrix effect, dilution integrity and stability. The within-run and between-run precision (at four levels) varied from 2.1% to 9.4% and from 4.0% to 17.0%, respectively. A maximum deviation of 11.62% for the within-run and between-run accuracies in relation to the nominal concentrations was observed. Moreover, the LLOQ value for cocaine was 50.0ngg(-1) whereas no significant effects were noticed in the assays of dilution integrity and stability. To assess its overall performance, the optimized method was applied to the analysis of eight human liver samples collected from individuals who died due to the abusive consumption of cocaine. Due to the existence of a significant matrix effect, a blank human liver was used to construct a matrix-matched analytical curve. The concentrations of cocaine found in these samples ranged from 333.5 to 5969ngg(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Acute normovolemic hemodilution is safe in neurosurgery.

PubMed

Oppitz, Paulo P; Stefani, Marco A

2013-01-01

To determine the safety of acute normovolemic hemodilution (ANH) for patients undergoing neurosurgical procedures. A group of 100 patients undergoing neurosurgical procedures was assigned prospectively to receive ANH. A group of 47 patients who underwent craniotomy for aneurysm clipping and standard anesthetic management was used as a control. Procedures conducted under ANH were performed without significant variations in physiologic parameters. Compared with controls, intraoperative blood loss, operative time, incidence and grade of complications, and length of hospital stay were similar between the two groups. Although the ANH group showed a difference in prothrombin levels before and after hemodilution procedures, the levels were still considered within physiologic parameters. Platelet counts and partial thromboplastin time (PTT) levels indicated no significant variations in either group. During the ANH procedure, a considerable reduction of brain oxygen extraction was observed in individuals with worse preoperative neurologic status (P < 0.05), indicating potential benefit. Among patients with cerebral aneurysm, patients with good initial clinical grades had better clinical results as indicated by Glasgow Outcome Scale scores (P < 0.02). ANH is a safe procedure for patients undergoing neurosurgical procedures. Further studies are necessary to confirm the improvement in brain oxygen extraction and the clinical impact. Nonetheless, patients undergoing aneurysm clipping with good clinical grades seem to profit from ANH. Copyright © 2013 Elsevier Inc. All rights reserved.

Field guide for collecting and processing stream-water samples for the National Water-Quality Assessment Program

USGS Publications Warehouse

Shelton, Larry R.

1994-01-01

The U.S. Geological Survey's National Water-Quality Assessment program includes extensive data- collection efforts to assess the quality of the Nations's streams. These studies require analyses of stream samples for major ions, nutrients, sediments, and organic contaminants. For the information to be comparable among studies in different parts of the Nation, consistent procedures specifically designed to produce uncontaminated samples for trace analysis in the laboratory are critical. This field guide describes the standard procedures for collecting and processing samples for major ions, nutrients, organic contaminants, sediment, and field analyses of conductivity, pH, alkalinity, and dissolved oxygen. Samples are collected and processed using modified and newly designed equipment made of Teflon to avoid contamination, including nonmetallic samplers (D-77 and DH-81) and a Teflon sample splitter. Field solid-phase extraction procedures developed to process samples for organic constituent analyses produce an extracted sample with stabilized compounds for more accurate results. Improvements to standard operational procedures include the use of processing chambers and capsule filtering systems. A modified collecting and processing procedure for organic carbon is designed to avoid contamination from equipment cleaned with methanol. Quality assurance is maintained by strict collecting and processing procedures, replicate sampling, equipment blank samples, and a rigid cleaning procedure using detergent, hydrochloric acid, and methanol.

An efficient microwave-assisted extraction process of stevioside and rebaudioside-A from Stevia rebaudiana (Bertoni).

PubMed

Jaitak, Vikas; Bikram Singh, Bandna; Kaul, V K

2009-01-01

Stevioside and rebaudioside-A are major low-calorie diterpene steviol glycosides in the leaves of Stevia rebaudiana. They are widely used as natural sweeteners for diabetic patients, but the long extraction procedures required and the optimisation of product yield present challenging problems. To develop a rapid and effective methodology for the extraction of stevioside and rebaudioside-A from S. rebaudiana leaves and to compare yields using different extraction techniques. Dried and powdered leaves of S. rebaudiana were extracted by conventional, ultrasound and microwave-assisted extraction techniques using methanol, ethanol and water as single solvents as well as in binary mixtures. Conventional cold extraction was performed at 25 degrees C for 12 h while ultrasound extraction was carried out at temperature of 35 +/- 5 degrees C for 30 min. Microwave-assisted extraction (MAE) was carried out at a power level of 80 W for 1 min at 50 degrees C. MAE yielded 8.64 and 2.34% of stevioside and rebaudioside-A, respectively, while conventional and ultrasound techniques yielded 6.54 and 1.20%, and 4.20 and 1.98% of stevioside and rebaudioside-A, respectively. A rapid and efficient method has been developed for the extraction of stevioside and rebaudioside-A in optimum yields using MAE procedure. This method has the advantage of rapid extraction and fast screening of a large number of S. rebaudiana samples for assessment of planting material. MAE saves considerable time, energy and has implications in the quality assessment of stevioside and rebaudioside-A prior to their industrial production from the leaves of S. rebaudiana. Copyright (c) 2009 John Wiley & Sons, Ltd.

42 CFR 493.1256 - Standard: Control procedures.

Code of Federal Regulations, 2010 CFR

2010-10-01

... for having control procedures that monitor the accuracy and precision of the complete analytic process..., include two control materials, including one that is capable of detecting errors in the extraction process... control materials having previously determined statistical parameters. (e) For reagent, media, and supply...

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

PubMed

Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

2000-02-11

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

Toxicity of algicidal extracts from Mangrovimonas yunxiaonensis strain LY01 on a HAB causing Alexandrium tamarense.

PubMed

Li, Yi; Zhu, Hong; Zhang, Huajun; Chen, Zhangran; Tian, Yun; Xu, Hong; Zheng, Tianling; Zheng, Wei

2014-08-15

Toxicity of algicidal extracts from Mangrovimonas yunxiaonensis strain LY01 on Alexandrium tamarense were measured through studying the algicidal procedure, nuclear damage and transcription of related genes. Medium components were optimized to improve algicidal activity, and characteristics of algicidal extracts were determined. Transmission electron microscope analysis revealed that the cell structure was broken. Cell membrane integrity destruction and nuclear structure degradation were monitored using confocal laser scanning microscope, and the rbcS, hsp and proliferating cell nuclear antigen (PCNA) gene expressions were studied. Results showed that 1.0% tryptone, 0.4% glucose and 0.8% MgCl2 were the optimal nutrient sources. The algicidal extracts were heat and pH stable, non-protein and less than 1kD. Cell membrane and nuclear structure integrity were lost, and the transcription of the rbcS and PCNA genes were significantly inhibited and there was up-regulation of hsp gene expression during the exposure procedure. The algicidal extracts destroyed the cell membrane and nuclear structure integrity, inhibited related gene expression and, eventually, lead to the inhibition of algal growth. All the results may elaborate firstly the cell death process and nuclear damage in A. tamarense which was induced by algicidal extracts, and the algicidal extracts could be potentially used as bacterial control of HABs in future. Copyright © 2014 Elsevier B.V. All rights reserved.

Sinus floor elevation from a maxillary molar tooth extraction socket in a patient with chronic inflammation.

PubMed

Tözüm, Tolga F; Dursun, Erhan; Tulunoglu, Ibrahim

2009-03-01

The compromised nature of the residual interradicular bone after extraction of periodontally hopeless maxillary molars often requires a sinus elevation procedure to ideally place the implants to accept future prosthesis. Maxillary sinus elevation surgery is a procedure used to increase the volume of bone mass so that dental implants can be placed. This article documents a sinus floor elevation technique through an extraction socket in a 65-year-old white male with chronic inflammation to increase the bone mass after the extraction of a periodontally involved maxillary molar tooth. Computerized tomography revealed an increased thickness of the sinus membrane, which was attributed to possible chronic sinus inflammation and periodontal inflammation. After consultation with the Department of Otolaryngology, it was diagnosed as chronic inflammation without any contraindication for sinus elevation surgery or implant placement. One month after the extraction, the sinus floor elevation surgery was performed through the extraction socket, and implants were placed 4 months later. An uneventful healing was noted after 6 months of osseointegration; two porcelain-fused-to-metal crowns were fabricated. Clinical follow-up took place every 3 months for 3 years, and successful healing was achieved. The patient was satisfied with the esthetic and functional results of the oral rehabilitation. Sinus floor elevation through an extraction socket without any residual bone, followed by dental implant placement, provided successful functional results and acceptable stability.

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. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extracting metalworking fluid aerosol samples in cassettes by provisional ASTM and NIOSH methods.

PubMed

Harper, Martin

2002-01-01

Recent provisional methods for the determination of metalworking fluid aerosol in workplace air involve a solvent extraction procedure to separate the nonvolatile fraction of the fluid from insoluble material such as metal turnings and dirt. The procedure calls for preweighing a filter (W1) and assembling it into a cassette and taking a sample. In the laboratory the filter is removed from the cassette, desiccated to remove any collected water or other volatile substances, and weighed again (W2). The filter is then extracted in an organic solvent blend, allowed to dry, and weighed a final time (W3). The total weight collected by the filter is given by (W2-W1), and the weight of (nonvolatile) metalworking fluid collected is given by (W2-W3). The extraction step can take place within a cassette housing if it is relatively inert to the solvent blend used. The extraction of four metalworking fluids (straight oil, soluble oil, synthetic and semisynthetic) within disposable polypropylene cassettes was investigated using the same protocol used to evaluate the original method. For all fluids the extraction efficiency was greater than 95% with a precision better than 5%. The mean blank contribution to the extraction step was 16 micrograms. Blanks were also evaluated after storage, and after transport and storage. A small additional blank contribution could be removed by desiccation. The limits of detection and quantitation of the extraction step were calculated to be 28 and 94 micrograms, respectively.

Alkaloid profiles of Mimosa tenuiflora and associated methods of analysis

USDA-ARS?s Scientific Manuscript database

The alkaloid contents of the leaves and seeds of M. tenuiflora collected from northeastern Brazil were studied. Alkaloids were isolated by classical acid/base extraction procedures and by cation exchange solid phase extraction. The crude alkaloid fractions were then analysed by thin layer chromatogr...

INFLUENCE OF MINERAL FORM, MATRIX CONCENTRATION AND PH ON IN-VITRO EXTRACTABILITY

EPA Science Inventory

Due to extensive resources required to conduct bioavailability studies, there is a veritable need for a laboratory in-vitro extraction procedure that yields a strong correlation to actual animal results that is simple to conduct and relatively rapid in data productivity. Research...

Determination of Polychlorinated Biphenyls in Soil and Sediment by Selective Pressurized Liquid Extraction with Immunochemical Detection

EPA Science Inventory

A selective liquid pressurized extraction (SPLE) method was developed as a streamlined sample preparation/cleanup procedure for determining Aroclors and coplanar polychlorinated biphenyls (PCBs) in soil and sediment matrices. The SPLE method was coupled with an enzyme-linked imm...

76 FR 64055 - Special Rules Governing Certain Information Obtained Under the Clean Air Act: Technical Correction

Federal Register 2010, 2011, 2012, 2013, 2014

2011-10-17

... natural gas. 211112 Natural gas liquid extraction facilities. Petrochemical Production....... 32511... facilities. 211112 Natural gas liquid extraction facilities. Suppliers of Industrial 325120 Industrial gas... reference in EPA's procedures for handling data collected under the Mandatory Greenhouse Gas Reporting Rule...

Parent experiences and information needs relating to procedural pain in children: a systematic review protocol.

PubMed

Gates, Allison; Shave, Kassi; Featherstone, Robin; Buckreus, Kelli; Ali, Samina; Scott, Shannon; Hartling, Lisa

2017-06-06

There exist many evidence-based interventions available to manage procedural pain in children and neonates, yet they are severely underutilized. Parents play an important role in the management of their child's pain; however, many do not possess adequate knowledge of how to effectively do so. The purpose of the planned study is to systematically review and synthesize current knowledge of the experiences and information needs of parents with regard to the management of their child's pain and distress related to medical procedures in the emergency department. We will conduct a systematic review using rigorous methods and reporting based on the PRISMA statement. We will conduct a comprehensive search of literature published between 2000 and 2016 reporting on parents' experiences and information needs with regard to helping their child manage procedural pain and distress. Ovid MEDLINE, Ovid PsycINFO, CINAHL, and PubMed will be searched. We will also search reference lists of key studies and gray literature sources. Two reviewers will screen the articles following inclusion criteria defined a priori. One reviewer will then extract the data from each article following a data extraction form developed by the study team. The second reviewer will check the data extraction for accuracy and completeness. Any disagreements with regard to study inclusion or data extraction will be resolved via discussion. Data from qualitative studies will be summarized thematically, while those from quantitative studies will be summarized narratively. The second reviewer will confirm the overarching themes resulting from the qualitative and quantitative data syntheses. The Critical Appraisal Skills Programme Qualitative Research Checklist and the Quality Assessment Tool for Quantitative Studies will be used to assess the quality of the evidence from each included study. To our knowledge, no published review exists that comprehensively reports on the experiences and information needs of parents related to the management of their child's procedural pain and distress. A systematic review of parents' experiences and information needs will help to inform strategies to empower them with the knowledge necessary to ensure their child's comfort during a painful procedure. PROSPERO CRD42016043698.

Determination of novel brominated flame retardants and polybrominated diphenyl ethers in serum using gas chromatography-mass spectrometry with two simplified sample preparation procedures.

PubMed

Gao, Le; Li, Jian; Wu, Yandan; Yu, Miaohao; Chen, Tian; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei

2016-11-01

Two simple and efficient pretreatment procedures have been developed for the simultaneous extraction and cleanup of six novel brominated flame retardants (NBFRs) and eight common polybrominated diphenyl ethers (PBDEs) in human serum. The first sample pretreatment procedure was a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based approach. An acetone/hexane mixture was employed to isolate the lipid and analytes from the serum with a combination of MgSO 4 and NaCl, followed by a dispersive solid-phase extraction (d-SPE) step using C18 particles as a sorbent. The second sample pretreatment procedure was based on solid-phase extraction. The sample extraction and cleanup were conducted directly on an Oasis HLB SPE column using 5 % aqueous isopropanol, concentrated sulfuric acid, and 10 % aqueous methanol, followed by elution with dichloromethane. The NBFRs and PBDEs were then detected using gas chromatography-negative chemical ionization mass spectrometry (GC-NCI MS). The methods were assessed for repeatability, accuracy, selectivity, limits of detection (LODs), and linearity. The results of spike recovery experiments in fetal bovine serum showed that average recoveries ranged from 77.9 % to 128.8 % with relative standard deviations (RSDs) from 0.73 % to 12.37 % for most of the analytes. The LODs for the analytes in fetal bovine serum ranged from 0.3 to 50.8 pg/mL except for decabromodiphenyl ethane. The proposed method was successfully applied to the determination of the 14 brominated flame retardants in human serum. The two pretreatment procedures described here are simple, accurate, and precise, and are suitable for the routine analysis of human serum. Graphical Abstract Workflow of a QuEChERS-based approach (top) and an SPE-based approach (bottom) for the detection of PBDEs and NBFRs in serum.

Glyoxal and methylglyoxal as urinary markers of diabetes. Determination using a dispersive liquid-liquid microextraction procedure combined with gas chromatography-mass spectrometry.

PubMed

Pastor-Belda, M; Fernández-García, A J; Campillo, N; Pérez-Cárceles, M D; Motas, M; Hernández-Córdoba, M; Viñas, P

2017-08-04

Glyoxal (GO) and methylglyoxal (MGO) are α-oxoaldehydes that can be used as urinary diabetes markers. In this study, their levels were measured using a sample preparation procedure based on salting-out assisted liquid-liquid extraction (SALLE) and dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography-mass spectrometry (GC-MS). The effect of the derivatization reaction with 2,3-diaminonaphthalene, the addition of acetonitrile and sodium chloride to urine, and the DLLME step using the acetonitrile extract as dispersant solvent and carbon tetrachloride as extractant solvent were carefully optimized. Quantification was performed by the internal standard method, using 5-bromo-2-chloroanisole. The intraday and interday precisions were lower than 6%. Limits of detection were 0.12 and 0.06ngmL -1 , and enrichment factors 140 and 130 for GO and MGO, respectively. The concentrations of these α-oxoaldehydes in urine were between 0.9 and 35.8ngg -1 levels (creatinine adjusted). A statistical comparison of the analyte contents of urine samples from non-diabetic and diabetic patients pointed to significant differences (P=0.046, 24 subjects investigated), particularly regarding MGO, which was higher in diabetic patients. The novelty of this study compared with previous procedures lies in the treatment of the urine sample by SALLE based on the addition of acetonitrile and sodium chloride to the urine. The DLLME procedure is performed with a sedimented drop of the extractant solvent, without a surfactant reagent, and using acetonitrile as dispersant solvent. Separation of the analytes was performed using GC-MS detection, being the analytes unequivocal identified. The proposed procedure is the first microextraction method applied to the analysis of urine samples from diabetic and non-diabetic patients that allows a clear differentiation between both groups using a simple analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Traditional child health practices in communities in north-west Ethiopia.

PubMed

Dagnew, M B; Damena, M

1990-01-01

A study in 3 villages in northwest Ethiopia was designed to find the type and extent of health damaging traditional child practices. The result of the survey showed high rates of uvulectomy and milk teeth extraction, and low rates of eyelid incision and female circumcision. More than 84.5% and 98.8% of the mothers surveyed, respectively, reported milk teeth extraction as a useful treatment for diarrhea and eyelid incision in the treatment of eye disease. The damage done by milk teeth extraction includes complications from unhygienic conditions (e.g. ostitis and osteomyelitis). Although many children survive these ill advised procedures and their complications, the considerable damage done to some of the children makes these procedures serious health hazards. Intensive health education with relevant health activities to correct the use of these traditional practices is advised.

Determination of Low Level Alpha and Beta Emitters Using Liquid-Liquid Extraction and a Liquid Scintillation Spectrometer

NASA Astrophysics Data System (ADS)

Yu, Yu-Fu; BjØRnstad, H. E.; Salbu, B.

Two radiochemical procedures for determination of low level strontium-90 and plutonium-239+240 in environmental and biological materials using combined selective solvent extraction with low level liquid scintillation counting have been presented. Y-90, the daughter nuclide of Sr-90, and Pu-239+240 are selectively extracted from nitric acid solution into 5% di(-2ethylhexyl)phosphoric acid (HDEHP) in toluene and the radionuclides of interest in organic phase are counted with an ultra low level scintillation counter "Quantulus". The lower detection limits for Sr-90 and Pu-239+240 are estimated to be 20 mBq and 0.3 mBq respectively. The developed procedures have been tested for soma environmental and biological samples and the preminarly results show that they are more simple and time-saving than traditional methods.

Solid-phase extraction of acidic herbicides.

PubMed

Wells, M J; Yu, L Z

2000-07-14

A discussion of solid-phase extraction method development for acidic herbicides is presented that reviews sample matrix modification, extraction sorbent selection, derivatization procedures for gas chromatographic analysis, and clean-up procedures for high-performance liquid chromatographic analysis. Acidic herbicides are families of compounds that include derivatives of phenol (dinoseb, dinoterb and pentachlorophenol), benzoic acid (acifluorfen, chloramben, dicamba, 3,5-dichlorobenzoic acid and dacthal--a dibenzoic acid derivative), acetic acid [2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T)], propanoic acid [dichlorprop, fluazifop, haloxyfop, 2-(4-chloro-2-methylphenoxy)propanoic acid (MCPP) and silvex], butanoic acid [4-(2,4-dichlorophenoxy)butanoic acid (2,4-DB) and 4-(4-chloro-2-methylphenoxy)butanoic acid (MCPB)], and other miscellaneous acids such as pyridinecarboxylic acid (picloram) and thiadiazine dioxide (bentazon).

Comparative Evaluation of Efficacy of Physics Forceps versus Conventional Forceps in Orthodontic Extractions: A Prospective Randomized Split Mouth Study.

PubMed

Patel, Harsh S; Managutti, Anil M; Menat, Shailesh; Agarwal, Arvind; Shah, Dishan; Patel, Jigar

2016-07-01

Tooth extraction is one of the most commonly performed procedures in dentistry. It is usually a traumatic procedure often resulting in immediate destruction and loss of alveolar bone and surrounding soft tissues. Various instruments have been described to perform atraumatic extractions which can prevent damage to the paradental structures. Recently developed physics forceps is one of the instruments which is claimed to perform atraumatic extractions. The aim of the present study was to compare the efficacy of physics forceps with conventional forceps in terms of operating time, prevention of marginal bone loss & soft tissue loss, postoperative pain and postoperative complications following bilateral premolar extractions for orthodontic purpose. In this prospective split-mouth study, outcomes of the 2 groups (n = 42 premolars) requiring extraction of premolars for orthodontic treatment purpose using Physics forceps and Conventional forceps were compared. Clinical outcomes in form of time taken, loss of buccal soft tissue and buccal cortical plate based on extraction defect classification system, postoperative pain and other complication associated with extraction were recorded and compared. Statistically significant reduction in the operating time was noted in physics forceps group. Marginal bone loss and soft tissue loss was also significantly lesser in physics forceps group when compared to conventional forceps group. However, there was no statistically significant difference in severity of postoperative pain between both groups. The results of the present study suggest that physics forceps was more efficient in reducing operating time and prevention of marginal bone loss & soft tissue loss when compared to conventional forceps in orthodontically indicated premolar extractions.

Potential for leaching of arsenic from excavated rock after different drying treatments.

PubMed

Li, Jining; Kosugi, Tomoya; Riya, Shohei; Hashimoto, Yohey; Hou, Hong; Terada, Akihiko; Hosomi, Masaaki

2016-07-01

Leaching of arsenic (As) from excavated rock subjected to different drying methods is compared using sequential leaching tests and rapid small-scale column tests combined with a sequential extraction procedure. Although the total As content in the rock was low (8.81 mg kg(-1)), its resulting concentration in the leachate when leached at a liquid-to-solid ratio of 10 L kg(-1) exceeded the environmental standard (10 μg L(-1)). As existed mainly in dissolved forms in the leachates. All of the drying procedures applied in this study increased the leaching of As, with freeze-drying leading to the largest increase. Water extraction of As using the two tests showed different leaching behaviors as a function of the liquid-to-solid ratio, and achieved average extractions of up to 35.7% and 25.8% total As, respectively. Dissolution of As from the mineral surfaces and subsequent re-adsorption controlled the short-term release of As; dissolution of Fe, Al, and dissolved organic carbon played important roles in long-term As leaching. Results of the sequential extraction procedure showed that use of 0.05 M (NH4)2SO4 underestimates the readily soluble As. Long-term water extraction removed almost all of the non-specifically sorbed As and most of the specifically sorbed As. The concept of pollution potential indices, which are easily determined by the sequential leaching test, is proposed in this study and is considered for possible use in assessing efficacy of treatment of excavated rocks. Copyright © 2016 Elsevier Ltd. All rights reserved.

A two-stage extraction procedure for insensitive munition (IM) explosive compounds in soils.

PubMed

Felt, Deborah; Gurtowski, Luke; Nestler, Catherine C; Johnson, Jared; Larson, Steven

2016-12-01

The Department of Defense (DoD) is developing a new category of insensitive munitions (IMs) that are more resistant to detonation or promulgation from external stimuli than traditional munition formulations. The new explosive constituent compounds are 2,4-dinitroanisole (DNAN), nitroguanidine (NQ), and nitrotriazolone (NTO). The production and use of IM formulations may result in interaction of IM component compounds with soil. The chemical properties of these IM compounds present unique challenges for extraction from environmental matrices such as soil. A two-stage extraction procedure was developed and tested using several soil types amended with known concentrations of IM compounds. This procedure incorporates both an acidified phase and an organic phase to account for the chemical properties of the IM compounds. The method detection limits (MDLs) for all IM compounds in all soil types were <5 mg/kg and met non-regulatory risk-based Regional Screening Level (RSL) criteria for soil proposed by the U.S. Army Public Health Center. At defined environmentally relevant concentrations, the average recovery of each IM compound in each soil type was consistent and greater than 85%. The two-stage extraction method decreased the influence of soil composition on IM compound recovery. UV analysis of NTO established an isosbestic point based on varied pH at a detection wavelength of 341 nm. The two-stage soil extraction method is equally effective for traditional munition compounds, a potentially important point when examining soils exposed to both traditional and insensitive munitions. Copyright © 2016 Elsevier Ltd. All rights reserved.

Leadless Cardiac Pacemaker Implantation After Lead Extraction in Patients With Severe Device Infection.

PubMed

Kypta, Alexander; Blessberger, Hermann; Kammler, Juergen; Lambert, Thomas; Lichtenauer, Michael; Brandstaetter, Walter; Gabriel, Michael; Steinwender, Clemens

2016-09-01

Conventional pacemaker therapy is limited by short- and long-term complications, most notably device infection. Transcatheter pacing systems (TPS) may be beneficial in this kind of patients as they eliminate the need for a device pocket and leads and thus may reduce the risk of re-infection. We assessed a novel procedure in 6 patients with severe device infection who were pacemaker dependent. After lead extraction a single chamber TPS was implanted into the right ventricle. Of the 6 patients who underwent lead extraction due to severe device infection at our institution, 3 were diagnosed with a pocket infection only, whereas the other 3 showed symptoms of both pocket and lead infection. Successful lead extraction and TPS implantation was accomplished in all patients. Four patients were bridged with a temporary pacemaker between 2 hours and 2 days after lead extraction, whereas 2 patients had the TPS implanted during the same procedure just before traditional pacemaker system removal. All patients stayed free of infection during the follow-up period of 12 weeks. An additional positron emission tomography scan was performed in each patient and indicated no signs of an infection around the TPS. Transcather pacemaker implantation was safe and feasible in 6 patients and did not result in re-infection even if implanted before removal of the infected pacemaker system within the same procedure. Therefore, implantation of a TPS may be an option for patients with severe device infection, especially in those with blocked venous access or who are pacemaker dependent. © 2016 Wiley Periodicals, Inc.

Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

NASA Astrophysics Data System (ADS)

Oliveira, J. M.; Carvalho, F. P.

2006-01-01

A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom® and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample).

Determination of the in-place hot-mix asphalt layer modulus for rehabilitation projects using a mechanistic-empirical procedure.

DOT National Transportation Integrated Search

2006-01-01

This project evaluated the procedures proposed by the Mechanistic-Empirical Pavement Design Guide (MEPDG) to characterize existing hot-mix asphalt (HMA) layers for rehabilitation purposes. Thirty-three cores were extracted from nine sites in Virginia...

Simple procedures for enrichment of chlorinated aromatic pollutants from fat, water and milk for subsequent analysis by high-resolution methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Egestad, B.; Curstedt, T.; Sjoevall, J.

1982-01-01

Procedures for enrichment of non-volatile chlorinated aromatic pollutants from fat, water and milk are described. /sup 14/C-DDT was used as a model compound in recovery experiments. A several thousand-fold enrichment of DDT added to butter was achieved by two consecutive straight-phase chromatographies on Lipidex 5000. Trace amounts of DDT in liter volumes of water could be quantitatively extracted by rapid filtration through 2 ml beds of Lipidex 1000. A batch extraction procedure permitted enrichment of DDT from milk after addition of n-pentylamine, methanol and water. DDT could then be eluted from the gel with retention of more than 90% ofmore » the lipids. A reversed-phase system with Lipidex 5000 could be used for separation of TCDD from DDT and PCBs. The liquid-gel chromatographic procedures are simple and suitable for clean-up of samples prior to application of high-resolution methods. 5 tables.« less

Two-step liquid phase microextraction combined with capillary electrophoresis: a new approach to simultaneous determination of basic and zwitterionic compounds.

PubMed

Nojavan, Saeed; Moharami, Arezoo; Fakhari, Ali Reza

2012-08-01

In this work, two-step hollow fiber-based liquid-phase microextraction procedure was evaluated for extraction of the zwitterionic cetirizine (CTZ) and basic hydroxyzine (HZ) in human plasma. In the first step of extraction, the pH of sample was adjusted at 5.0 in order to promote liquid-phase microextraction of the zwitterionic CTZ. In the second step, the pH of sample was increased up to 11.0 for extraction of basic HZ. In this procedure, the extraction times for the first and the second steps were 30 and 20 min, respectively. Owing to the high ratio between the volumes of donor phase and acceptor phase, CTZ and HZ were enriched by factors of 280 and 355, respectively. The linearity of the analytical method was investigated for both compounds in the range of 10-500 ng mL(-1) (R(2) > 0.999). Limit of quantification (S/N = 10) for CTZ and HZ was 10 ng mL(-1) , while the limit of detection was 3 ng mL(-1) for both compounds at a signal to noise ratio of 3:1. Intraday and interday relative standard deviations (RSDs, n = 6) were in the range of 6.5-16.2%. This procedure enabled CTZ and HZ to be analyzed simultaneously by capillary electrophoresis. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

HS3D, A Dataset of Homo Sapiens Splice Regions, and its Extraction Procedure from a Major Public Database

NASA Astrophysics Data System (ADS)

Pollastro, Pasquale; Rampone, Salvatore

The aim of this work is to describe a cleaning procedure of GenBank data, producing material to train and to assess the prediction accuracy of computational approaches for gene characterization. A procedure (GenBank2HS3D) has been defined, producing a dataset (HS3D - Homo Sapiens Splice Sites Dataset) of Homo Sapiens Splice regions extracted from GenBank (Rel.123 at this time). It selects, from the complete GenBank Primate Division, entries of Human Nuclear DNA according with several assessed criteria; then it extracts exons and introns from these entries (actually 4523 + 3802). Donor and acceptor sites are then extracted as windows of 140 nucleotides around each splice site (3799 + 3799). After discarding windows not including canonical GT-AG junctions (65 + 74), including insufficient data (not enough material for a 140 nucleotide window) (686 + 589), including not AGCT bases (29 + 30), and redundant (218 + 226), the remaining windows (2796 + 2880) are reported in the dataset. Finally, windows of false splice sites are selected by searching canonical GT-AG pairs in not splicing positions (271 937 + 332 296). The false sites in a range +/- 60 from a true splice site are marked as proximal. HS3D, release 1.2 at this time, is available at the Web server of the University of Sannio: http://www.sci.unisannio.it/docenti/rampone/.

Gastrodia elata Bl. Attenuated learning deficits induced by forced-swimming stress in the inhibitory avoidance task and Morris water maze.

PubMed

Chen, Pei-Ju; Liang, Keng-Chen; Lin, Hui-Chen; Hsieh, Ching-Liang; Su, Kuan-Pin; Hung, Mei-Chu; Sheen, Lee-Yan

2011-06-01

This study adopted the forced-swimming paradigm to induce depressive symptoms in rats and evaluated the effects on learning and memory processing. Furthermore, the effects of the water extract of Gastrodia elata Bl., a well-known Chinese traditional medicine, on amnesia in rats subjected to the forced-swimming procedure were studied. Rats were subjected to the forced-swimming procedure, and the inhibitory avoidance task and Morris water maze were used to assess learning and memory performance. The acquisition of the two tasks was mostly impaired after the 15-minute forced-swimming procedure. Administration of the water extract of G. elata Bl. for 21 consecutive days at a dosage of 0.5 or 1.0 g/kg of body weight significantly improved retention in the inhibitory avoidance test, and the lower dose showed a better effect than the higher one and the antidepressant fluoxetine (18 mg/kg of body weight). In the Morris water maze, the lower dose of the water extract of G. elata Bl. significantly improved retention by shortening escape latency in the first test session and increasing the time in searching the target zone during the probe test. These findings suggest that water extracts of G. elata Bl. ameliorate the learning and memory deficits induced by forced swimming.

Comparison of manual and semi-automatic DNA extraction protocols for the barcoding characterization of hematophagous louse flies (Diptera: Hippoboscidae).

PubMed

Gutiérrez-López, Rafael; Martínez-de la Puente, Josué; Gangoso, Laura; Soriguer, Ramón C; Figuerola, Jordi

2015-06-01

The barcoding of life initiative provides a universal molecular tool to distinguish animal species based on the amplification and sequencing of a fragment of the subunit 1 of the cytochrome oxidase (COI) gene. Obtaining good quality DNA for barcoding purposes is a limiting factor, especially in studies conducted on small-sized samples or those requiring the maintenance of the organism as a voucher. In this study, we compared the number of positive amplifications and the quality of the sequences obtained using DNA extraction methods that also differ in their economic costs and time requirements and we applied them for the genetic characterization of louse flies. Four DNA extraction methods were studied: chloroform/isoamyl alcohol, HotShot procedure, Qiagen DNeasy(®) Tissue and Blood Kit and DNA Kit Maxwell(®) 16LEV. All the louse flies were morphologically identified as Ornithophila gestroi and a single COI-based haplotype was identified. The number of positive amplifications did not differ significantly among DNA extraction procedures. However, the quality of the sequences was significantly lower for the case of the chloroform/isoamyl alcohol procedure with respect to the rest of methods tested here. These results may be useful for the genetic characterization of louse flies, leaving most of the remaining insect as a voucher. © 2015 The Society for Vector Ecology.

Development of fast and robust multiresidual LC-MS/MS method for determination of pharmaceuticals in soils.

PubMed

Golovko, Oksana; Koba, Olga; Kodesova, Radka; Fedorova, Ganna; Kumar, Vimal; Grabic, Roman

2016-07-01

The aim of this study was to develop a simple extraction procedure and a multiresidual liquid chromatography-tandem mass spectrometry method for determination of a wide range of pharmaceuticals from various soil types. An extraction procedure for 91 pharmaceuticals from 13 soil types, followed by liquid chromatography-tandem mass spectrometry analysis, was optimized. The extraction efficiencies of three solvent mixtures for ultrasonic extraction were evaluated for 91 pharmaceuticals. The best results were obtained using acetonitrile/water (1/1 v/v with 0.1 % formic acid) followed by acetonitrile/2-propanol/water (3/3/4 v/v/v with 0.1 % formic acid) for extracting 63 pharmaceuticals. The method was validated at three fortification levels (10, 100, and 1000 ng/g) in all types of representative soils; recovery of 44 pharmaceuticals ranged between 55 and 135 % across all tested soils. The method was applied to analyze actual environmental samples of sediments, soils, and sludge, and 24 pharmaceuticals were found above limit of quantification with concentrations ranging between 0.83 ng/g (fexofenadine) and 223 ng/g (citalopram).

Compositional similarities of non-solvent extractable fatty acids from recent marine sediments deposited in differing environments

NASA Astrophysics Data System (ADS)

Nishimura, Mitsugu; Baker, Earl W.

1987-06-01

Five recent sediment samples from a variety of North American continental shelves were analyzed for fatty acids (FAs) in the solvent-extractable (SOLEX) lipids as well as four types of non-solvent extractable (NONEX) lipids. The NONEX lipids were operationally defined by the succession of extraction procedure required to recover them. The complete procedure included (i) very mild acid treatment, (ii) HF digestion and (iii) saponification of the sediment residue following exhaustive solvent extraction. The distribution pattern and various compositional parameters of SOLEX FAs in the five sediments were divided into three different groups, indicating the difference of biological sources and also diagenetic factors and processes among the three groups of samples. Nevertheless, the compositions of the corresponding NONEX FAs after acid treatment were surprisingly very similar. This was also true for the remaining NONEX FA groups in the five sediment samples. The findings implied that most of the NONEX FAs reported here are derived directly from living organisms. It is also concluded that a large part of NONEX FAs are much more resistant to biodegradation than we have thought, so that they can form the large percentage of total lipids with increasing depth of water and sediments.

Characterization of Rabbit Corneas Subjected to Stromal Stiffening by the Açaí Extract (Euterpe oleracea).

PubMed

Bersanetti, Patrícia A; Bueno, Tatiane L N; Morandim-Giannetti, Andreia de A; Nogueira, Regina F; Matos, Jivaldo R; Schor, Paulo

2017-04-01

In this study, we characterized rabbit corneas subjected to corneal cross-linking (CXL) with açaí extract compared with a riboflavin photo-stimulated procedure. The corneas of the slaughterhouse rabbits were divided into three groups: control, consisting of untreated corneal samples; riboflavin/UVA, where corneas were treated with 0.1% riboflavin photo-stimulated at 365 nm as the standard protocol; and açaí, where the samples were subjected to 4% açaí extract for 0.5-2 h. After the CXL procedure, corneas of the three groups were characterized by analyzing their elastic modulus and thermal denaturation profile. The elastic modulus at 3% strain showed an approximately threefold increase in the riboflavin/UVA group and 10.5 times in the corneas treated with 4% açaí extract for 2 h, compared with the control group (p < 0.01). The denaturation temperature values of the two groups of crosslinked corneas increased significantly (p < 0.05) and were more pronounced in the açaí group. The açaí extract was effective in promoting CXL in rabbit corneas as characterized by the different techniques.

Improved sample treatment for the determination of insoluble soap in sewage sludge samples by liquid chromatography with fluorescence detection.

PubMed

Cantarero, Samuel; Zafra-Gómez, A; Ballesteros, O; Navalón, A; Vílchez, J L; Crovetto, G; Verge, C; de Ferrer, J A

2010-09-15

A new selective and sensitive method for the determination of insoluble fatty acid salts (soap) in sewage sludge samples is proposed. The method involves a clean up of sample with petroleum ether, the conversion of calcium and magnesium insoluble salts into soluble potassium salts, potassium salts extraction with methanol, and a derivatization procedure previous to the liquid chromatography with fluorescence detection (LC-FLD) analysis. Three different extraction techniques (Soxhlet, microwave-assisted extraction and ultrasounds) were compared and microwave-assisted extraction (MAE) was selected as appropriate for our purpose. This allowed to reduce the extraction time and solvent waste (50 mL of methanol in contrast with 250 mL for Soxhlet procedure). The absence of matrix effect was demonstrated with two standards (C(13:0) and C(17:0)) that are not commercials and neither of them has been detected in sewage sludge samples. Therefore, it was possible to evaluate the matrix effect since both standards have similar environmental behaviour (adsorption and precipitation) to commercial soaps (C(10:0)-C(18:0)). The method was successfully applied to samples from different sources and consequently, with different composition. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Evaluating specificity of sequential extraction for chemical forms of lead in artificially-contaminated and field-contaminated soils.

PubMed

Tai, Yiping; McBride, Murray B; Li, Zhian

2013-03-30

In the present study, we evaluated a commonly employed modified Bureau Communautaire de Référence (BCR test) 3-step sequential extraction procedure for its ability to distinguish forms of solid-phase Pb in soils with different sources and histories of contamination. When the modified BCR test was applied to mineral soils spiked with three forms of Pb (pyromorphite, hydrocerussite and nitrate salt), the added Pb was highly susceptible to dissolution in the operationally-defined "reducible" or "oxide" fraction regardless of form. When three different materials (mineral soil, organic soil and goethite) were spiked with soluble Pb nitrate, the BCR sequential extraction profiles revealed that soil organic matter was capable of retaining Pb in more stable and acid-resistant forms than silicate clay minerals or goethite. However, the BCR sequential extraction for field-collected soils with known and different sources of Pb contamination was not sufficiently discriminatory in the dissolution of soil Pb phases to allow soil Pb forms to be "fingerprinted" by this method. It is concluded that standard sequential extraction procedures are probably not very useful in predicting lability and bioavailability of Pb in contaminated soils. Copyright © 2013 Elsevier B.V. All rights reserved.

Parameter Extraction Method for the Electrical Model of a Silicon Photomultiplier

NASA Astrophysics Data System (ADS)

Licciulli, Francesco; Marzocca, Cristoforo

2016-10-01

The availability of an effective electrical model, able to accurately reproduce the signals generated by a Silicon Photo-Multiplier coupled to the front-end electronics, is mandatory when the performance of a detection system based on this kind of detector has to be evaluated by means of reliable simulations. We propose a complete extraction procedure able to provide the whole set of the parameters involved in a well-known model of the detector, which includes the substrate ohmic resistance. The technique allows achieving very good quality of the fit between simulation results provided by the model and experimental data, thanks to accurate discrimination between the quenching and substrate resistances, which results in a realistic set of extracted parameters. The extraction procedure has been applied to a commercial device considering a wide range of different conditions in terms of input resistance of the front-end electronics and interconnection parasitics. In all the considered situations, very good correspondence has been found between simulations and measurements, especially for what concerns the leading edge of the current pulses generated by the detector, which strongly affects the timing performance of the detection system, thus confirming the effectiveness of the model and the associated parameter extraction technique.

In-tube extraction for the determination of the main volatile compounds in Physalis peruviana L.

PubMed

Kupska, Magdalena; Jeleń, Henryk H

2017-01-01

An analytical procedure based on in-tube extraction followed by gas chromatography with mass spectrometry has been developed for the analysis of 24 of the main volatile components in cape gooseberry (Physalis peruviana L.) samples. According to their chemical structure, the compounds were organized into different groups: one hydrocarbon, one aldehyde, four alcohols, four esters, and 14 monoterpenes. By single-factor experiments, incubation temperature, incubation time, extraction volume, extraction strokes, extraction speed, desorption temperature, and desorption speed were determined as 60°C, 20 min, 1000 μL, 20, 50:50 μL/s, 280°C, 100 μL/s, respectively. Quantitative analysis using authentic standards and external calibration curves was performed. The limit of detection and limit of quantification for the analytical procedure were calculated. Results shown the benzaldehyde, ethyl butanoate, 2-methyl-1-butanol, 1-hexanol, 1-butanol, α-terpineol, and terpinen-4-ol were the most abundant volatile compounds in analyzed fruits (68.6-585 μg/kg). The obtained data may contribute to qualify cape gooseberry to the group of superfruits and, therefore, increase its popularity. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Road Network Extraction from Dsm by Mathematical Morphology and Reasoning

NASA Astrophysics Data System (ADS)

Li, Yan; Wu, Jianliang; Zhu, Lin; Tachibana, Kikuo

2016-06-01

The objective of this research is the automatic extraction of the road network in a scene of the urban area from a high resolution digital surface model (DSM). Automatic road extraction and modeling from remote sensed data has been studied for more than one decade. The methods vary greatly due to the differences of data types, regions, resolutions et al. An advanced automatic road network extraction scheme is proposed to address the issues of tedium steps on segmentation, recognition and grouping. It is on the basis of a geometric road model which describes a multiple-level structure. The 0-dimension element is intersection. The 1-dimension elements are central line and side. The 2-dimension element is plane, which is generated from the 1-dimension elements. The key feature of the presented approach is the cross validation for the three road elements which goes through the entire procedure of their extraction. The advantage of our model and method is that linear elements of the road can be derived directly, without any complex, non-robust connection hypothesis. An example of Japanese scene is presented to display the procedure and the performance of the approach.

Improved sample extraction and clean-up for the GC-MS determination of BADGE and BFDGE in vegetable oil.

PubMed

Brede, C; Skjevrak, I; Herikstad, H; Anensen, E; Austvoll, R; Hemmingsen, T

2002-05-01

A straightforward method was established for the determination of migration contaminants in olive oil with a special focus on the two can-coating migration compounds bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE). The preferred sample preparation was a single liquid-liquid extraction of compounds from the oil into 20% (v/v) methanol in acetonitrile, followed by clean-up with solid-phase extraction on aminopropyl bonded to silica. This purification procedure selectively removed all free fatty acids from the extracts without removing phenolic compounds of interest. The solid-phase extraction columns were used many times by implementing a procedure of washing out the strongly retained fatty acids with 2% acetic acid in methanol. Gas chromatography coupled with full scan (m/z 33-700) electron ionization mass spectrometry was used for the determination of several model compounds in olive oil samples. BADGE and BFDGE could be determined in the 0.05-2 mg kg(-1) range in oil samples with a relative SD of <6% (six replicates). The method was used in an enforcement campaign for the Norwegian Food Control Authority to analyse vegetable oil samples from canned fish-in-oil.

How-to-Do-It. An Exercise in Gene Mapping.

ERIC Educational Resources Information Center

Seidel-Rogol, Bonnie L.

1990-01-01

Described is a laboratory exercise designed to introduce students to the theory and practice of gene mapping including RNA extraction, sucrose density gradient centrifugation, labelling of nucleic acids in vitro, DNA extraction, digestion of DNA with restriction enzymes, and the southern hybridization analysis. Procedures and sample results are…

Pressure-Assisted Chelating Extraction as a Teaching Tool in Instrumental Analysis

ERIC Educational Resources Information Center

Sadik, Omowunmi A.; Wanekaya, Adam K.; Yevgeny, Gelfand

2004-01-01

A novel instrumental-digestion technique using pressure-assisted chelating extraction (PACE), for undergraduate laboratory is reported. This procedure is used for exposing students to safe sample-preparation techniques, for correlating wet-chemical methods with modern instrumental analysis and comparing the performance of PACE with conventional…

Tooth extraction by orthodontic force after radiation therapy: report of case

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rodu, B.; Filler, S.J.; Woodfin, G.K.

1985-12-01

This report presents a therapeutic approach to orthodontic tooth extraction in a patient at high risk for the development of osteoradionecrosis with conventional techniques. The rationale for this procedure is discussed in detail, combining principles of radiation biology, clinical radiation therapy, and biomechanics of tooth movement.

Comparison of two extraction methods for the analysis of petroleum hydrocarbon residues in mallard duck eggs by GC and GC-MS

USGS Publications Warehouse

Belisle, A.A.; Gay, M.L.; Coon, N.C.

1981-01-01

Hydrocarbon residues in pooled eggs from a mallard duck on a diet of 25,000 ppm South Louisiana crude oil were compared after cleanup with and without saponification. The saponification procedure yielded superior reproducibility and extraction efficiency

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.13)

EPA Science Inventory

The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.

COMPARISON OF TWO DIFFERENT SOLID PHASE EXTRACTION/LARGE VOLUME INJECTION PROCEDURES FOR METHOD 8270

EPA Science Inventory

Two solid phase (SPE) and one traditional continuous liquid-liquid extraction method are compared for analysis of Method 8270 SVOCs. Productivity parameters include data quality, sample volume, analysis time and solvent waste.

One SPE system, unique in the U.S., uses aut...

EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High Performance Liquid Chromatography-Thermospray-Mass Spectrometry (HPLC-TS-MS) or Ultraviolet (UV) Detection

EPA Pesticide Factsheets

Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.

Influence of gelatinization on the extraction of phenolic acids from wheat fractions

USDA-ARS?s Scientific Manuscript database

The effect of gelatinization on the analysis of phenolic acids from wheat bran, whole-wheat, and refined flour samples was investigated using two extraction procedures, namely, ultrasonic (UAE) and microwave (MAE). The total phenolic acid (TPA) concentration quantity in wheat bran (2711-2913 µg/g) w...

75 FR 17170 - Notice of Opportunity To Request a Hearing for the License Application From International...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-04-05

... Fluoride Extraction and Uranium Deconversion Facility in Lea County NM and Order Imposing Procedures for... application from International Isotopes Fluorine Products, Inc. (IIFP), for a proposed fluoride extraction and... applicant to process depleted uranium hexafluoride (DUF 6 ) into commercially resalable fluoride products...

Comparison of two extraction methods for the analysis of petroleum hydrocarbon residues in mallard duck eggs by GC and GC-MS. [NONE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Belisle, A.A.; Gay, M.L.; Coon, N.C.

Hydrocarbon residues in pooled eggs from a mallard duck on a diet of 25,000 ppm South Louisiana crude oil were compared after cleanup with and without saponification. The saponification procedure yielded superior reproducibility and extraction efficiency..

ION COMPOSITION ELUCIDATION (ICE): A HIGH RESOLUTION MASS SPECTROMETRIC TOOL FOR IDENTIFYING ORGANIC COMPOUNDS IN COMPLEX EXTRACTS OF ENVIRONMENTAL SAMPLES

EPA Science Inventory

Unidentified Organic Compounds. For target analytes, standards are purchased, extraction and clean-up procedures are optimized, and mass spectra and retention times for the chromatographic separation are obtained for comparison to the target compounds in environmental sample ...

Xylan extraction from pretreated sugarcane bagasse using alkaline and enzymatic approaches.

PubMed

Sporck, Daniele; Reinoso, Felipe A M; Rencoret, Jorge; Gutiérrez, Ana; Del Rio, José C; Ferraz, André; Milagres, Adriane M F

2017-01-01

New biorefinery concepts are necessary to drive industrial use of lignocellulose biomass components. Xylan recovery before enzymatic hydrolysis of the glucan component is a way to add value to the hemicellulose fraction, which can be used in papermaking, pharmaceutical, and food industries. Hemicellulose removal can also facilitate subsequent cellulolytic glucan hydrolysis. Sugarcane bagasse was pretreated with an alkaline-sulfite chemithermomechanical process to facilitate subsequent extraction of xylan by enzymatic or alkaline procedures. Alkaline extraction methods yielded 53% (w/w) xylan recovery. The enzymatic approach provided a limited yield of 22% (w/w) but produced the xylan with the lowest contamination with lignin and glucan components. All extracted xylans presented arabinosyl side groups and absence of acetylation. 2D-NMR data suggested the presence of O -methyl-glucuronic acid and p -coumarates only in enzymatically extracted xylan. Xylans isolated using the enzymatic approach resulted in products with molecular weights (Mw) lower than 6 kDa. Higher Mw values were detected in the alkali-isolated xylans. Alkaline extraction of xylan provided a glucan-enriched solid readily hydrolysable with low cellulase loads, generating hydrolysates with a high glucose/xylose ratio. Hemicellulose removal before enzymatic hydrolysis of the cellulosic fraction proved to be an efficient manner to add value to sugarcane bagasse biorefining. Xylans with varied yield, purity, and structure can be obtained according to the extraction method. Enzymatic extraction procedures produce high-purity xylans at low yield, whereas alkaline extraction methods provided higher xylan yields with more lignin and glucan contamination. When xylan extraction is performed with alkaline methods, the residual glucan-enriched solid seems suitable for glucose production employing low cellulase loadings.

Determination of rutin and quercetin in Chinese herbal medicine by ionic liquid-based pressurized liquid extraction-liquid chromatography-chemiluminescence detection.

PubMed

Wu, Hongwei; Chen, Meilan; Fan, Yunchang; Elsebaei, Fawzi; Zhu, Yan

2012-01-15

A novel ionic liquid-based pressurized liquid extraction (IL-PLE) procedure coupled with high performance liquid chromatography (HPLC) tandem chemiluminescence (CL) detection capable of quantifying trace amounts of rutin and quercetin in four Chinese medicine plants including Flos sophorae Immaturus, Crateagus pinnatifida Bunge, Hypericum japonicum Thunb and Folium Mori was described in this paper. To avoid environmental pollution and toxicity to the operators, ionic liquids (ILs), 1-alkyl-3-methylimidazolium chloride ([C(n)mim][Cl]) aqueous solutions were used in the PLE procedure as extractants replacing traditional organic solvents. In addition, chemiluminescence detection was utilized for its minimal interference from endogenous components of complex matrix. Parameters affecting extraction and analysis were carefully optimized. Compared with the conventional ultrasonic-assisted extraction (UAE) and heat-reflux extraction (HRE), the optimized method achieved the highest extraction efficiency in the shortest extraction time with the least solvent consumption. The applicability of the proposed method to real sample was confirmed. Under the optimized conditions, good reproducibility of extraction performance was obtained and good linearity was observed with correlation coefficients (r) between 0.9997 and 0.9999. The detection limits of rutin and quercetin (LOD, S/N=3) were 1.1×10(-2)mg/L and 3.8×10(-3)mg/L, respectively. The average recoveries of rutin and quercetin for real samples were 93.7-105% with relative standard deviation (RSD) lower than 5.7%. To the best of our knowledge, this paper is the first contribution to utilize a combination of IL-PLE with chemiluminescence detection. And the experimental results indicated that the proposed method shows a promising prospect in extraction and determination of rutin and quercetin in medicinal plants. Copyright © 2011 Elsevier B.V. All rights reserved.

A novel sample preparation procedure for effect-directed analysis of micro-contaminants of emerging concern in surface waters.

PubMed

Osorio, Victoria; Schriks, Merijn; Vughs, Dennis; de Voogt, Pim; Kolkman, Annemieke

2018-08-15

A novel sample preparation procedure relying on Solid Phase Extraction (SPE) combining different sorbent materials on a sequential-based cartridge was optimized and validated for the enrichment of 117 widely diverse contaminants of emerging concern (CECs) from surface waters (SW) and further combined chemical and biological analysis on subsequent extracts. A liquid chromatography coupled to high resolution tandem mass spectrometry LC-(HR)MS/MS protocol was optimized and validated for the quantitative analysis of organic CECs in SW extracts. A battery of in vitro CALUX bioassays for the assessment of endocrine, metabolic and genotoxic interference and oxidative stress were performed on the same SW extracts. Satisfactory recoveries ([70-130]%) and precision (< 30%) were obtained for the majority of compounds tested. Internal standard calibration curves used for quantification of CECs, achieved the linearity criteria (r 2 > 0.99) over three orders of magnitude. Instrumental limits of detection and method limits of quantification were of [1-96] pg injected and [0.1-58] ng/L, respectively; while corresponding intra-day and inter-day precision did not exceed 11% and 20%. The developed procedure was successfully applied for the combined chemical and toxicological assessment of SW intended for drinking water supply. Levels of compounds varied from < 10 ng/L to < 500 ng/L. Endocrine (i.e. estrogenic and anti-androgenic) and metabolic interference responses were observed. Given the demonstrated reliability of the validated sample preparation method, the authors propose its integration in an effect-directed analysis procedure for a proper evaluation of SW quality and hazard assessment of CECs. Copyright © 2018 Elsevier B.V. All rights reserved.

Dispersed particle extraction--a new procedure for trace element enrichment from natural aqueous samples with subsequent ICP-OES analysis.

PubMed

Bauer, Gerald; Neouze, Marie-Alexandra; Limbeck, Andreas

2013-01-15

A novel sample pre-treatment method for multi trace element enrichment from environmental waters prior to optical emission spectrometry analysis with inductively coupled plasma (ICP-OES) is proposed, based on dispersed particle extraction (DPE). This method is based on the use of silica nanoparticles functionalized with strong cation exchange ligands. After separation from the investigated sample solution, the nanoparticles used for the extraction are directly introduced in the ICP for measurement of the adsorbed target analytes. A prerequisite for the successful application of the developed slurry approach is the use of sorbent particles with a mean size of 500 nm instead of commercially available μm sized beads. The proposed method offers the known advantages of common bead-injection (BI) techniques, and further circumvents the elution step required in conventional solid phase extraction procedures. With the use of 14.4 mL sample and addition of ammonium acetate buffer and particle slurry limits of detection (LODs) from 0.03 μg L(-1) for Be to 0.48 μg L(-1) for Fe, with relative standard deviations ranging from 1.7% for Fe and 5.5% for Cr and an average enrichment factor of 10.4 could be achieved. By implementing this method the possibility to access sorbent materials with irreversible bonding mechanisms for sample pre-treatment is established, thus improvements in the selectivity of sample pre-treatment procedures can be achieved. The presented procedure was tested for accuracy with NIST standard reference material 1643e (fresh water) and was applied to drinking water samples from the vicinity of Vienna. Copyright © 2012 Elsevier B.V. All rights reserved.

Extraction and identification of cyclobutanones from irradiated cheese employing a rapid direct solvent extraction method.

PubMed

Tewfik, Ihab

2008-01-01

2-Alkylcyclobutanones (cyclobutanones) are accepted as chemical markers for irradiated foods containing lipid. However, current extraction procedures (Soxhlet-florisil chromatography) for the isolation of these markers involve a long and tedious clean-up regime prior to gas chromatography-mass spectrophotometry identification. This paper outlines an alternative isolation and clean-up method for the extraction of cyclobutanones in irradiated Camembert cheese. The newly developed direct solvent extraction method enables the efficient screening of large numbers of food samples and is not as resource intensive as the BS EN 1785:1997 method. Direct solvent extraction appears to be a simple, robust method and has the added advantage of a considerably shorter extraction time for the analysis of foods containing lipid.

A preliminary report on the rapid fluorimetric determination of uranium in low-grade ores

USGS Publications Warehouse

Grimaldi, F.S.; Levine, Harry

1950-01-01

A simple and very rapid fluorimetric procedure is described for the determination of uranium in low-grade shale and phosphate ores. The best working range is from 0.001 to about 0.04 percent U. The procedure employs batch extraction of uranium nitrate by ethyl acetate, using aluminum nitrate as the salting agent, prior to the visual fluorimetric estimation. The procedure is especially designed to save reagents; only 9.5 g of aluminum nitrate and 10 ml of ethyl acetate being used for one analysis. The solution of the sample by means of a fusion with NaOH-NaNO3 flux is rapid. After fusion the sample is immediately extracted without removing silica and other hydrolytic precipitates. Aluminum nitrate very effectively ties up fluoride and phosphate, thus eliminating steps required for their removal.

Intracellular coagulation inhibits the extraction of proteins from Prochloron

NASA Technical Reports Server (NTRS)

Fall, R.; Lewin, R. A.; Fall, L. R.

1983-01-01

Protein extraction from the prokaryotic alga Prochloron LP (isolated from the ascidian host Lissoclinum patella) was complicated by an irreversible loss of cell fragility in the isolated algae. Accompanying this phenomenon, which is termed intracellular coagulation, was a redistribution of thylakoids around the cell periphery, a loss of photosynthetic O2 production, and a drastic decrease in the extractability of cell proteins. Procedures are described for the successful preparation and transport of cell extracts yielding the enzymes glucose-6-phosphate dehydrogenase and 6-phosphogluconate dehydrogenase as well as other soluble proteins.

Dual-wavelength phase-shifting digital holography selectively extracting wavelength information from wavelength-multiplexed holograms.

PubMed

Tahara, Tatsuki; Mori, Ryota; Kikunaga, Shuhei; Arai, Yasuhiko; Takaki, Yasuhiro

2015-06-15

Dual-wavelength phase-shifting digital holography that selectively extracts wavelength information from five wavelength-multiplexed holograms is presented. Specific phase shifts for respective wavelengths are introduced to remove the crosstalk components and extract only the object wave at the desired wavelength from the holograms. Object waves in multiple wavelengths are selectively extracted by utilizing 2π ambiguity and the subtraction procedures based on phase-shifting interferometry. Numerical results show the validity of the proposed technique. The proposed technique is also experimentally demonstrated.

Analysis of trace contamination of phthalate esters in ultrapure water using a modified solid-phase extraction procedure and automated thermal desorption-gas chromatography/mass spectrometry.

PubMed

Liu, Hsu-Chuan; Den, Walter; Chan, Shu-Fei; Kin, Kuan Tzu

2008-04-25

The present study was aimed to develop a procedure modified from the conventional solid-phase extraction (SPE) method for the analysis of trace concentration of phthalate esters in industrial ultrapure water (UPW). The proposed procedure allows UPW sample to be drawn through a sampling tube containing hydrophobic sorbent (Tenax TA) to concentrate the aqueous phthalate esters. The solid trap was then demoisturized by two-stage gas drying before subjecting to thermal desorption and analysis by gas chromatography-mass spectrometry. This process removes the solvent extraction procedure necessary for the conventional SPE method, and permits automation of the analytical procedure for high-volume analyses. Several important parameters, including desorption temperature and duration, packing quantity and demoisturizing procedure, were optimized in this study based on the analytical sensitivity for a standard mixture containing five different phthalate esters. The method detection limits for the five phthalate esters were between 36 ng l(-1) and 95 ng l(-1) and recovery rates between 15% and 101%. Dioctyl phthalate (DOP) was not recovered adequately because the compound was both poorly adsorbed and desorbed on and off Tenax TA sorbents. Furthermore, analyses of material leaching from poly(vinyl chloride) (PVC) tubes as well as the actual water samples showed that di-n-butyl phthalate (DBP) and di(2-ethylhexyl) phthalate (DEHP) were the common contaminants detected from PVC contaminated UPW and the actual UPW, as well as in tap water. The reduction of DEHP in the production processes of actual UPW was clearly observed, however a DEHP concentration of 0.20 microg l(-1) at the point of use was still being quantified, suggesting that the contamination of phthalate esters could present a barrier to the future cleanliness requirement of UPW. The work demonstrated that the proposed modified SPE procedure provided an effective method for rapid analysis and contamination identification in UPW production lines.

Optimizing conditions for the extraction of pigments in cochineals (Dactylopius coccus Costa) using response surface methodology.

PubMed

González, Mónica; Méndez, Jesús; Carnero, Aurelio; Lobo, M Gloria; Afonso, Ana

2002-11-20

A simple method was developed for the extraction and determination of color pigments in cochineals (Dactylopius coccus Costa). The procedure was based on the solvent extraction of pigments in insect samples using methanol:water (65:35, v:v) as extractant. Two-level factorial design was used in order to optimize the solvent extraction parameters: temperature, time, methanol concentration in the extractant mixture, and the number of extractions. The results suggest that the number of extractions is statistically the most significant factor. The separation and determination of the pigments was carried out by high-performance liquid chromatography with UV-visible detection. Because the absorption spectra of different pigments are different in the visible region, it is convenient to use a diode array detector to obtain chromatographic profiles that allow for the characterization of the extracted pigments.

First Aid Procedures for Dental Emergencies.

ERIC Educational Resources Information Center

Barsky, Nancy Happel; Londeree, Kathy

1982-01-01

Guidelines for first aid procedures for temporary relief of dental emergencies include information on: (1) dental first aid supplies; (2) treatment of oral injuries; (3) orthodontic emergencies; (4) toothaches; and (5) prolonged bleeding due to an extraction. Consulting a dentist as soon as possible is strongly recommended. (JN)

Fractionation of metals by sequential extraction procedures (BCR and Tessier) in soil exposed to fire of wide temperature range

NASA Astrophysics Data System (ADS)

Fajkovic, Hana; Rončević, Sanda; Nemet, Ivan; Prohić, Esad; Leontić-Vazdar, Dana

2017-04-01

Forest fire presents serious problem, especially in Mediterranean Region. Effects of fire are numerous, from climate change and deforestation to loss of soil organic matter and changes in soil properties. One of the effects, not well documented, is possible redistribution and/or remobilisation of pollutants previously deposited in the soil, due to the new physical and chemical soil properties and changes in equilibrium conditions. For understanding and predicting possible redistribution and/or remobilisation of potential pollutants from soil, affected by fire different in temperature, several laboratory investigations were carried out. To evaluate the influence of organic matter on soil under fire, three soil samples were analysed and compared: (a) the one with added coniferous organic matter; (b) deciduous organic matter (b) and (c) soil without additional organic matter. Type of organic matter is closely related to pH of soil, as pH is influencing the mobility of some pollutants, e.g. metals. For that reason pH was also measured through all experimental steps. Each of mentioned soil samples (a, b and c) were heated at 1+3 different temperatures (25°C, 200°C, 500°C and 850°C). After heating, whereby fire effect on soil was simulated, samples were analysed by BCR protocol with the addition of a first step of sequential extraction procedure by Tessier and analysis of residual by aqua regia. Element fractionation of heavy metals by this procedure was used to determine the amounts of selected elements (Al, Cd, Cr, Co, Cu, Fe, Mn, Ni, Pb and Zn). Selected metal concentrations were determined using inductively coupled plasma atomic emission spectrometer. Further on, loss of organic matter was calculated after each heating procedure as well as the mineral composition. The mineral composition was determined using an X-ray diffraction. From obtained results, it can be concluded that temperature has an influence on concentration of elements in specific step of sequential extraction procedures. The first step of Tessier and BCR extraction of samples heated at 250°C and 500°C showed increasing trend of elemental concentrations. Results of these steps are especially important since they indicate mobile fraction of the elements (exchangeable, water- and acid-soluble fraction), which can easily affect the environment. Extraction procedures of samples combusted at 850°C showed that decrease in measured elemental content occurred. Some correlation is also noticed between type of organic matter, pH and concentration of analysed elements.

The Science and Art of Eyebrow Transplantation by Follicular Unit Extraction

PubMed Central

Gupta, Jyoti; Kumar, Amrendra; Chouhan, Kavish; Ariganesh, C; Nandal, Vinay

2017-01-01

Eyebrows constitute a very important and prominent feature of the face. With growing information, eyebrow transplant has become a popular procedure. However, though it is a small area it requires a lot of precision and knowledge regarding anatomy, designing of brows, extraction and implantation technique. This article gives a comprehensive view regarding eyebrow transplant with special emphasis on follicular unit extraction technique, which has become the most popular technique. PMID:28852290

Direct ultrasonic agitation for rapid extraction of organic matter from airborne particulate.

PubMed

Lee, S C; Zou, S C; Ho, K F; Chan, L Y

2001-01-02

Direct ultrasonic extraction (DUE) is proposed as simple and rapid sample pretreatment method. This new approach is applied to the extraction of particulate organic matter (POM) from airborne particulate by using dichloromethane (DCM) or DCM/methanol (90/10, v/v) as extractant. The analytical determination was carried out by weighing the extractable POM on an electrobalance. Total recovery for POM could be obtained when the sample was extracted three times with 25-50 mL extractant each for about 5 min at 50 W ultrasonic power. In comparison with conventional Soxhlet extraction, less extraction time (total 15 min only) and solvent consumption (100 mL) were required by DUE. The efficiency of the DUE was similar or even higher than the routine Soxhlet method. Additionally, the new extractor is very simple and easy to use and can accelerate the extraction procedures of organic components from various solid samples.

The extraction of gold nanoparticles from oat and wheat biomasses using sodium citrate and cetyltrimethylammonium bromide, studied by x-ray absorption spectroscopy, high-resolution transmission electron microscopy, and UV-visible spectroscopy.

PubMed

Armendariz, Veronica; Parsons, Jason G; Lopez, Martha L; Peralta-Videa, Jose R; Jose-Yacaman, Miguel; Gardea-Torresdey, Jorge L

2009-03-11

Gold (Au) nanoparticles can be produced through the interaction of Au(III) ions with oat and wheat biomasses. This paper describes a procedure to recover gold nanoparticles from oat and wheat biomasses using cetyltrimethylammonium bromide or sodium citrate. Extracts were analyzed using UV-visible spectroscopy, high-resolution transmission electron microscopy (HRTEM), and x-ray absorption spectroscopy. The HRTEM data demonstrated that smaller nanoparticles are extracted first, followed by larger nanoparticles. In the fourth extraction, coating of chelating agents is visible on the extracted nanoparticles.

Sample-space-based feature extraction and class preserving projection for gene expression data.

PubMed

Wang, Wenjun

2013-01-01

In order to overcome the problems of high computational complexity and serious matrix singularity for feature extraction using Principal Component Analysis (PCA) and Fisher's Linear Discrinimant Analysis (LDA) in high-dimensional data, sample-space-based feature extraction is presented, which transforms the computation procedure of feature extraction from gene space to sample space by representing the optimal transformation vector with the weighted sum of samples. The technique is used in the implementation of PCA, LDA, Class Preserving Projection (CPP) which is a new method for discriminant feature extraction proposed, and the experimental results on gene expression data demonstrate the effectiveness of the method.

DEGRADATION OF ERGOTHIONEINE BY CELL-FREE EXTRACTS OF ALCALIGENES FAECALIS II.

PubMed Central

Booth, James S.; Appleman, Milo D.

1963-01-01

Booth, James S. (University of Southern California, Los Angeles) and Milo D. Appleman. Degradation of ergothioneine by cell-free extracts of Alcaligenes faecalis. II. Production of glutamic acid. J. Bacteriol. 85:654–657. 1963.—On the basis of oxidation and paper chromatographic procedures, glutamic acid was identified as the end product of ergothioneine degradation by cell-free extracts of Alcaligenes faecalis. Hydrogen sulfide and ammonia yields were determined. Several differences between the metabolism of whole cells and cell-free extracts were noted. Cleavage of the imidazole ring by cell-free extracts appeared to be hydrolytic rather than oxidative. PMID:14042946

Results of the first provisional technical secretariat interlaboratory comparison test

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stuff, J.R.; Hoffland, L.

1995-06-01

The principal task of this laboratory in the first Provisional Technical Secretariat (PTS) Interlaboratory Comparison Test was to verify and test the extraction and preparation procedures outlined in the Recommended Operating Procedures for Sampling and Analysis in the Verification of Chemical Disarmament in addition to our laboratory extraction methods and our laboratory analysis methods. Sample preparation began on 16 May 1994 and analysis was completed on 12 June 1994. The analytical methods used included NMR ({sup 1}H and {sup 31}P) GC/AED, GC/MS (EI and methane CI), GC/IRD, HPLC/IC, HPLC/TSP/MS, MS/MS(Electrospray), and CZE.

Direct determination of gallium on polyurethane foam by X-ray fluorescence.

PubMed

Carvalho, M S; Medeiros, J A; Nóbrega, A W; Mantovano, J L; Rocha, V P

1995-01-01

Gallium chloride is easily extracted from 6M HCl by comminuted polyether-type polyurethane foam. After the extraction step, the gallium absorbed by the PU foam can be quantitatively determined by X-ray fluorescence. A procedure for the direct determination of gallium absorbed by PU foam by XRFS is thus described. Gallium is determined at levels as low as 60 ng/ml (C(L)), with a calibration sensitivity of 424 cps ml/mug, within a linear range 0.1-2.30 mug/ml. The procedure investigated was successfully applied to determination of gallium in aluminum alloys, bauxite and industrial residue samples.

THE ALLEGED OCCURRENCE OF ADRENALIN IN THE MEALWORM

PubMed Central

Gregerman, Robert I.; Wald, George

1952-01-01

Wense has reported the isolation of crystalline adrenalin from larvae of the beetle Tenebrio molitor. An attempt to repeat his procedures failed to yield any evidence of adrenalin. Analysis of mealworm extracts by paper chromatography and colorimetric means also yielded no indication of adrenalin, though adrenalin added to mealworms can be detected by these procedures in amounts less than 1 mg. per 100 gm. Mealworm extracts reveal on the paper chromatogram the presence of two other orthodiphenols, neither of which appears to be dopa but which may be 3,4-dihydroxyphenyllactic acid and 3,4-dihydroxyphenylacetic acid, compounds recently isolated elsewhere from this organism. PMID:14898031

The Use of Isotope Dilution Alpha Spectrometry and Liquid Scintillation Counting to Determine Radionuclides in Environmental Samples (abstract)

NASA Astrophysics Data System (ADS)

Bylyku, Elida

2009-04-01

In Albania in recent years it has been of increasing interest to determine various pollutants in the environment and their possible effects on human health. The radiochemical procedure used to identify Pu, Am, U, Th, and Sr radioisotopes in soil, sediment, water, coal, and milk samples is described. The analysis is carried out in the presence of respective tracer solutions and combines the procedure for Pu analysis based on anion exchange, the selective method for Sr isolation based on extraction chromatography using Sr-Spec resin, and the application of the TRU-Spec column for separation of Am fraction. An acid digestion method has been applied for the decomposition of samples. The radiochemical procedure involves the separation of Pu from Th, Am, and Sr by anion exchange, followed by the preconcentration of Am and Sr by coprecipitation with calcium oxalate. Am is separated from Sr by extraction chromatography. Uranium is separated from the bulk elements by liquid-liquid extraction using UTEVA® resin. Thin sources for alpha spectrometric measurements are prepared by microprecipitation with NdF3. Two International Atomic Energy Agency reference materials were analyzed in parallel with the samples.

A method for estimating the relative degree of saponification of xanthophyll sources and feedstuffs.

PubMed

Fletcher, D L

2006-05-01

Saponification of xanthophyll esters in various feed sources has been shown to improve pigmentation efficiency in broiler skin and egg yolks. Three trials were conducted to evaluate a rapid liquid chromatography procedure for estimating the relative degree of xanthophyll saponification using samples of yellow corn, corn gluten meal, alfalfa, and 6 commercially available marigold meal concentrates. In each trial, samples were extracted using a modification of the 1984 Association of Official Analytical Chemists hot saponification procedure with and without the addition of KOH. A comparison of the chromatography results was used to estimate percent saponification of the original sample by dividing the nonsaponified extraction values by the saponified extraction values. A comparison of the percent saponified xanthophylls for each product (mg/kg) was: yellow corn, 101; corn gluten meal, 78; alfalfa, 97.9; and marigold concentrates A through F, 99.8, 4.6, 99.0, 95.6, 96.8, and 6.6, respectively. These results indicate that a modification of the 1984 Association of Official Analytical Chemists procedure and liquid column chromatography can be used to quickly verify saponification and can be used to estimate the relative degree of saponification of an unknown xanthophyll source.

Tracking transcriptional activities with high-content epifluorescent imaging

NASA Astrophysics Data System (ADS)

Hua, Jianping; Sima, Chao; Cypert, Milana; Gooden, Gerald C.; Shack, Sonsoles; Alla, Lalitamba; Smith, Edward A.; Trent, Jeffrey M.; Dougherty, Edward R.; Bittner, Michael L.

2012-04-01

High-content cell imaging based on fluorescent protein reporters has recently been used to track the transcriptional activities of multiple genes under different external stimuli for extended periods. This technology enhances our ability to discover treatment-induced regulatory mechanisms, temporally order their onsets and recognize their relationships. To fully realize these possibilities and explore their potential in biological and pharmaceutical applications, we introduce a new data processing procedure to extract information about the dynamics of cell processes based on this technology. The proposed procedure contains two parts: (1) image processing, where the fluorescent images are processed to identify individual cells and allow their transcriptional activity levels to be quantified; and (2) data representation, where the extracted time course data are summarized and represented in a way that facilitates efficient evaluation. Experiments show that the proposed procedure achieves fast and robust image segmentation with sufficient accuracy. The extracted cellular dynamics are highly reproducible and sensitive enough to detect subtle activity differences and identify mechanisms responding to selected perturbations. This method should be able to help biologists identify the alterations of cellular mechanisms that allow drug candidates to change cell behavior and thereby improve the efficiency of drug discovery and treatment design.

Effect of preparation procedures on intensity of radioautographic labeling is studied

NASA Technical Reports Server (NTRS)

Baserga, R.; Kisieleski, W. E.

1967-01-01

Effects of tissue preparation and extractive procedures on the intensity of radioautographic labeling are presented in terms of mean grain count per cell in cells labeled with tritiated precursors of proteins or nucleic acids. This information would be of interest to medical researchers and cytologists.

Microchemical urinalysis. IX - Determination of hydroxyproline in urine.

NASA Technical Reports Server (NTRS)

Grunbaum, B. W.; Pace, N.

1973-01-01

A simplified procedure is described for the determination of hydroxyproline in human or monkey urine. In this procedure 1 ml of urine is subjected in succession to hydrolysis, oxidation, extraction, and color development. During these steps impurities and interfering substances are eliminated, thus resulting in a chromophore due to hydroxyproline alone.

Obtaining eigensolutions for multiple frequency ranges in a single NASTRAN execution

NASA Technical Reports Server (NTRS)

Pamidi, P. R.; Brown, W. K.

1990-01-01

A novel and general procedure for obtaining eigenvalues and eigenvectors for multiple frequency ranges in a single NASTRAN execution is presented. The scheme is applicable to normal modes analyzes employing the FEER and Inverse Power methods of eigenvalue extraction. The procedure is illustrated by examples.

Effects of Storage Temperature and Extraction Procedure on Recovery of Plant-parasitic Nematodes from Field Soils

PubMed Central

Barker, K. R.; Nusbaum, C. J.; Nelson, L. A.

1969-01-01

Storage of nematodes in soil at -15 C for 1 to 16 weeks greatly increased nematode recovery by a sugar-flotation-sieving procedure. One week of exposure to -15 C killed all nematodes except Pratylenchus zeae and Tylenchorhynchus claytoni which were recoverable in decreasing numbers up to 10 weeks by the Baermann funnel method. Optimum storage temperature for survival of most nematode species was 13 C. The numbers of Meloidogyne incognita, T. claytoni, Belonolaimus Iongicaudatus, and P. zeae recoverable by either extraction method remained constant or increased when stored at 13-24 C for 16 weeks. This was also true for Helicotylenchtts dihystera and Xiphinema americanum extracted by the Baermann funnel technique, whereas the numbers retrieved by the sugar-flotation-sieving method decreased slightly. All species except T. claytoni decreased appreciably in soil stored at 36 C. PMID:19325684

Kinetics from Replica Exchange Molecular Dynamics Simulations.

PubMed

Stelzl, Lukas S; Hummer, Gerhard

2017-08-08

Transitions between metastable states govern many fundamental processes in physics, chemistry and biology, from nucleation events in phase transitions to the folding of proteins. The free energy surfaces underlying these processes can be obtained from simulations using enhanced sampling methods. However, their altered dynamics makes kinetic and mechanistic information difficult or impossible to extract. Here, we show that, with replica exchange molecular dynamics (REMD), one can not only sample equilibrium properties but also extract kinetic information. For systems that strictly obey first-order kinetics, the procedure to extract rates is rigorous. For actual molecular systems whose long-time dynamics are captured by kinetic rate models, accurate rate coefficients can be determined from the statistics of the transitions between the metastable states at each replica temperature. We demonstrate the practical applicability of the procedure by constructing master equation (Markov state) models of peptide and RNA folding from REMD simulations.

Multiple functional ionic liquids based dispersive liquid-liquid microextraction combined with high performance chromatography for the determination of phenolic compounds in water samples.

PubMed

Sun, Jian-Nan; Chen, Juan; Shi, Yan-Ping

2014-07-01

A new mode of ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) is developed. In this work, [C6MIm][PF6] was chosen as the extraction solvent, and two kinds of hydrophilic ionic liquids, [EMIm][BF4] and [BSO3HMIm][OTf], functioned as the dispersive solvent. So in the whole extraction procedure, no organic solvent was used. With the aid of SO3H group, the acidic compound was extracted from the sample solution without pH adjustment. Two phenolic compounds, namely, 2-naphthol and 4-nitrophenol were chosen as the target analytes. Important parameters affecting the extraction efficiency, such as the type of hydrophilic ionic liquids, the volume ratio of [EMIm][BF4] to [BSO3HMIm][OTf], type and volume of extraction solvent, pH value of sample solution, sonication time, extraction time and centrifugation time were investigated and optimized. Under the optimized extraction conditions, the method exhibited good sensitivity with the limits of detection (LODs) at 5.5 μg L(-1)and 10.0 μg L(-1) for 4-nitrophenol and 2-naphthol, respectively. Good linearity over the concentration ranges of 24-384 μg L(-1) for 4-nitrophenol and 28-336 μg L(-1) for 2-naphthol was obtained with correlation coefficients of 0.9998 and 0.9961, respectively. The proposed method can directly extract acidic compound from environmental sample or even more complex sample matrix without any pH adjustment procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of pressurized subcritical water extraction combined with stir bar sorptive extraction for the analysis of organochlorine pesticides and chlorobenzenes in soils.

PubMed

Rodil, Rosario; Popp, Peter

2006-08-18

An analytical method for the determination of several organochlorine pesticides (OCPs) like hexachlorocyclohexanes (HCHs), cyclodiene derivates (dieldrin, aldrin, endrin, heptachlor, heptachlor epoxide, endrin aldehyde, endosulfan and ensodulfan sulphate) and DDX compounds (p,p'-DDE, p,p'-DDD and p,p'-DDT) as well as chlorobenzenes in soils has been developed. The procedure is based on pressurized subcritical water extraction (PSWE) followed by stir bar sorptive extraction (SBSE) and subsequent thermodesorption-gas chromatography/mass spectrometry analysis. Significant PSWE and SBSE parameters were optimized using spiked soil and water samples. For the PSWE of the organochlorine compounds, water modified with acetonitrile as the extraction solvent, at an extraction temperature of 120 degrees C, and three cycles of 10 min extraction proved to be optimal. Under optimized conditions, the figures of merit, such as precision, accuracy and detection limits were evaluated. The detection limits obtained for soil samples were in the range 0.002-4.7 ng/g. Recoveries between 4.1 and 85.2% were achieved from samples spiked at a concentration level of 25-155 ng/g. The main advantages of this method are the avoidance of clean-up and concentration procedures as well as the significant reduction of the required volume of organic solvents. The described method was applied to the determination of the pollutants in soil samples collected from a polluted area, the Bitterfeld region (Germany). The results obtained by PSWE-SBSE were in a good agreement with those obtained by a reference method, a conventional pressurized liquid extraction (PLE).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Favorito, Jessica E.; Luxton, Todd P.; Eick, Matthew J.

Selenium is a trace element found in western US soils, where ingestion of Se-accumulating plants has resulted in livestock fatalities. Therefore, a reliable understanding of Se speciation and bioavailability is critical for effective mitigation. Sequential extraction procedures (SEP) are often employed to examine Se phases and speciation in contaminated soils but may be limited by experimental conditions. We examined the validity of a SEP using X-ray absorption spectroscopy (XAS) for both whole and a sequence of extracted soils. The sequence included removal of soluble, PO4-extractable, carbonate, amorphous Fe-oxide, crystalline Fe-oxide, organic, and residual Se forms. For whole soils, XANES analysesmore » indicated Se(0) and Se(-II) predominated, with lower amounts of Se(IV) present, related to carbonates and Fe-oxides. Oxidized Se species were more elevated and residual/elemental Se was lower than previous SEP results from ICP-AES suggested. For soils from the SEP sequence, XANES results indicated only partial recovery of carbonate, Fe-oxide and organic Se. This suggests Se was incompletely removed during designated extractions, possibly due to lack of mineral solubilization or reagent specificity. Selenium fractions associated with Fe-oxides were reduced in amount or removed after using hydroxylamine HCl for most soils examined. XANES results indicate partial dissolution of solid-phases may occur during extraction processes. This study demonstrates why precautions should be taken to improve the validity of SEPs. Mineralogical and chemical characterizations should be completed prior to SEP implementation to identify extractable phases or mineral components that may influence extraction effectiveness. Sequential extraction procedures can be appropriately tailored for reliable quantification of speciation in contaminated soils.« less

Rural-urban differences in dental service use among children enrolled in a private dental insurance plan in Wisconsin: analysis of administrative data.

PubMed

Bhagavatula, Pradeep; Xiang, Qun; Szabo, Aniko; Eichmiller, Fredrick; Kuthy, Raymond A; Okunseri, Christopher E

2012-12-21

Studies on rural-urban differences in dental care have primarily focused on differences in utilization rates and preventive dental services. Little is known about rural-urban differences in the use of wider range of dental procedures. This study examined patterns of preventive, restorative, endodontic, and extraction procedures provided to children enrolled in Delta Dental of Wisconsin (DDWI). We analyzed DDWI enrollment and claims data for children aged 0-18 years from 2002 to 2008. We modified and used a rural and urban classification based on ZIP codes developed by the Wisconsin Area Health Education Center (AHEC). We categorized the ZIP codes into 6 AHEC categories (3 rural and 3 urban). Descriptive and multivariable analysis using generalized linear mixed models (GLMM) were used to examine the patterns of dental procedures provided to children. Tukey-Kramer adjustment was used to control for multiple comparisons. Approximately, 50%, 67% and 68% of enrollees in inner-city Milwaukee, Rural 1 (less than 2500 people), and suburban-Milwaukee had at least one annual dental visit, respectively. Children in inner city-Milwaukee had the lowest utilization rates for all procedures examined, except for endodontic procedures. Compared to children from inner-city Milwaukee, children in other locations had significantly more preventive procedures. Children in Rural 1-ZIP codes had more restorative, endodontic and extraction procedures, compared to children from all other regions. We found significant geographic variation in dental procedures received by children enrolled in DDWI.

Evaluation of a method for the simultaneous quantification of N-nitrosamines in water samples based on stir bar sorptive extraction combined with high-performance liquid chromatography and diode array detection.

PubMed

Talebpour, Zahra; Rostami, Simindokht; Rezadoost, Hassan

2015-05-01

A simple, sensitive, and reliable procedure based on stir bar sorptive extraction coupled with high-performance liquid chromatography was applied to simultaneously extract and determine three semipolar nitrosamines including N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine. To achieve the optimum conditions, the effective parameters on the extraction efficiency including desorption solvent and time, ionic strength of sample, extraction time, and sample volume were systematically investigated. The optimized extraction procedure was carried out by stir bars coated with polydimethylsiloxane. Under optimum extraction conditions, the performance of the proposed method was studied. The linear dynamic range was obtained in the range of 0.95-1000 ng/mL (r = 0.9995), 0.26-1000 ng/mL (r = 0.9988) and both 0.32-100 ng/mL (r = 0.9999) and 100-1000 ng/mL (r = 0.9998) with limits of detection of 0.28, 0.08, and 0.09 ng/mL for N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine, respectively. The average recoveries were obtained >81%, and the reproducibility of the proposed method presented as intra- and interday precision were also found with a relative standard deviation <6%. Finally, the proposed method was successfully applied to the determination of trace amounts of selected nitrosamines in various water and wastewater samples and the obtained results were confirmed using mass spectrometry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of the clean-up efficiency of the solid-phase extraction of rosemary extracts: Application of full-factorial design in hyphenation with Gaussian peak fit function.

PubMed

Meischl, Florian; Kirchler, Christian Günter; Jäger, Michael Andreas; Huck, Christian Wolfgang; Rainer, Matthias

2018-02-01

We present a novel method for the quantitative determination of the clean-up efficiency to provide a calculated parameter for peak purity through iterative fitting in conjunction with design of experiments. Rosemary extracts were used and analyzed before and after solid-phase extraction using a self-fabricated mixed-mode sorbent based on poly(N-vinylimidazole/ethylene glycol dimethacrylate). Optimization was performed by variation of washing steps using a full three-level factorial design and response surface methodology. Separation efficiency of rosmarinic acid from interfering compounds was calculated using an iterative fit of Gaussian-like signals and quantifications were performed by the separate integration of the two interfering peak areas. Results and recoveries were analyzed using Design-Expert® software and revealed significant differences between the washing steps. Optimized parameters were considered and used for all further experiments. Furthermore, the solid-phase extraction procedure was tested and compared with commercial available sorbents. In contrast to generic protocols of the manufacturers, the optimized procedure showed excellent recoveries and clean-up rates for the polymer with ion exchange properties. Finally, rosemary extracts from different manufacturing areas and application types were studied to verify the developed method for its applicability. The cleaned-up extracts were analyzed by liquid chromatography with tandem mass spectrometry for detailed compound evaluation to exclude any interference from coeluting molecules. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Beavin, P. Jr.

A rapid direct dilution procedure for the estimation of soluble zirconium and a fusion procedure for the determination of total zirconium (soluble and insoluble forms) in cream base concentrates prepared from antiperspirant aerosols are described. The direct dilution procedure involves extraction of soluble zirconium with HCl (55 + 45). The filtered extract is reacted with alizarin red S to form a stable colored complex which is measured spectrophotometrically. The fusion procedure involves ashing the aerosol concentrate followed by fusion of the ash with potassium pyrosulfate to form an acid-soluble melt. Zirconium is precipitated from solution as the hydroxide and washedmore » to eliminate interfering ions, particularly sulfate. After redissolving in HCl (55 + 45) and reacting with alizarin red S, total zirconium is measured. Zirconyl chloride octahydrate, assayed gravimetrically by hydroxide precipitation and conversion to the oxide, is used as the zirconium reference standard. Concentration range of zirconium measured was 200 to 500 ..mu..g/100 ml. Recoveries of standard zirconium added to commercial aerosols labeled to contain aluminum and zirconyl hydroxychlorides ranged from 97 to 101 percent by the fusion procedure. Analysis of these aerosols by direct dilution gave generally slightly lower results than by fusion.« less

[Determination of serum or plasma alpha-tocopherol by high performance liquid chromatography: optimization of operative models].

PubMed

Jezequel-Cuer, M; Le Moël, G; Mounié, J; Peynet, J; Le Bizec, C; Vernet, M H; Artur, Y; Laschi-Loquerie, A; Troupel, S

1995-01-01

A previous multicentric study set up by the Société française de biologie clinique has emphasized the usefulness of a standardized procedure for the determination by high performance liquid chromatography of alpha-tocopherol in serum or plasma. In our study, we have tested every step of the different published procedures: internal standard adduct, lipoprotein denaturation and vitamin extraction. Reproducibility of results was improved by the use of tocol as an internal standard when compared to retinol or alpha-tocopherol acetates. Lipoprotein denaturation was more efficient with ethanol addition than with methanol and when the ethanol/water ratio was > or = 0.7. Use of n-hexane or n-heptane gave the same recovery of alpha-tocopherol. When organic solvent/water ratio was > or = 1, n-hexane enabled to efficiently extract, in a one-step procedure, the alpha-tocopherol from both normo and hyperlipidemic sera. Performances of the selected procedure were: detection limit: 0.5 microM--linear range: 750 microM--within run coefficient of variation: 2.03%--day to day: 4.76%. Finally, this pluricentric study allows us to propose an optimised procedure for the determination of alpha-tocopherol in serum or plasma.

Evaluation of a Low-Cost Commercially Available Extraction Device for Assessing Lead Bioaccessibility in Contaminated Soils

EPA Science Inventory

The U.S. EPA’s in vitro bioaccessibility (IVBA) method 9200.1-86 defines a validated analytical procedure for the determination of lead bioaccessibility in contaminated soils. The method requires the use of a custom-fabricated extraction device that uses a heated water bath for ...

Nautical Education for Offshore Extractive Industries. Support Operations & Seamanship.

ERIC Educational Resources Information Center

Hoffmann, G. L.

This training manual is intended for persons who will be employed on supply vessels or towboats which support ocean-based oil extraction operations. The text deals with the basic skills of marine towing procedures, boat handling, deck maintenance, cargo operations, and rope and wire handling. Additional sections treat the proper attitude of a…

COMPARISON OF TWO FIELD SAMPLING PROCEDURES (EN CORE AND FIELD METHANOL EXTRACTION) FOR VOLATILE ORGANIC COMPOUNDS

EPA Science Inventory

In-situ Lasagna technology was recently evaluated at a contaminated site at Offutt Air Force Base. The site was contaminated with low levels (< 30 mg/kg) of volatile organic compounds (VOCs). Originally, researchers planned to use field methanol extraction for both pre- and pos...

Synthesis, characterization, and application of a Zn (II)-imprinted polymer grafted on graphene oxide/magnetic chitosan nanocomposite for selective extraction of zinc ions from different food samples.

PubMed

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Ranjbar, Mansoureh

2017-12-15

A novel Zn(II) imprinted polymer was synthesized via a co-precipitation method using graphene oxide/magnetic chitosan nanocomposite as supporting material. The synthesized imprinted polymer was characterized by Fourier transform infrared spectrometry (FTIR) and scanning electron microscopy (SEM) and applied as a sorbent for selective magnetic solid phase extraction of zinc followed by its determination by flame atomic absorption spectrometry. The kinetic and isothermal adsorption experiments were carried out and all parameters affecting the extraction process was optimized. Under the optimal experimental conditions, the developed procedure exhibits a linear dynamic range of 0.5-5.0µgL -1 with a detection limit of 0.09µgL -1 and quantification limit of 0.3µgL -1 . The maximum sorption capacity of the sorbent was found to be 71.4mgg -1 . The developed procedure was successfully applied to the selective extraction and determination of zinc in various samples including well water, drinking water, black tea, rice, and milk. Copyright © 2017 Elsevier Ltd. All rights reserved.

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

PubMed Central

Islas, Gabriela; Hernandez, Prisciliano

2017-01-01

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. PMID:29181027

Novel procedure for the extraction and concentration of carotenoid-containing chromoplasts from selected plant systems.

PubMed

Fish, Wayne W

2007-02-21

Natural sources of carotenoids for nutraceutical use are desired by the food industry as a result of the increased production of convenience and other highly processed foods. As new physiological roles are discovered for some of the minor carotenoids that are found in only small amounts in present sources, the need for discovery of new sources will amplify. Thus, a method is needed that will effectively and gently concentrate carotenoids from potential new sources for subsequent identification and analysis. A procedure is presented by which carotenoid-containing tissue chromoplasts can be extracted and subsequently concentrated by precipitation, all in an aqueous milieu. The chromoplasts are extracted and solubilized with 0.3% sodium dodecyl sulfate (SDS) in water. The addition of a nominally equal volume of acetonitrile to the chromoplasts in SDS immediately precipitates the chromoplasts out of solution with generally >90% recovery. Carotenoids contained in the concentrated, still-intact chromoplasts can then be solubilized by organic solvent extraction for subsequent analysis. This methodology offers a means to effectively and gently concentrate carotenoids from fruit tissues where yields are often low (e.g., yellow watermelon).

Solvent effects on quantitative analysis of brominated flame retardants with Soxhlet extraction.

PubMed

Zhong, Yin; Li, Dan; Zhu, Xifen; Huang, Weilin; Peng, Ping'an

2017-05-18

Reliable quantifications of brominated flame retardants (BFRs) not only ensure compliance with laws and regulations on the use of BFRs in commercial products, but also is key for accurate risk assessments of BFRs. Acetone is a common solvent widely used in the analytical procedure of BFRs, but our recent study found that acetone can react with some BFRs. It is highly likely that such reactions can negatively affect the quantifications of BFRs in environmental samples. In this study, the effects of acetone on the extraction yields of three representative BFRs [i.e., decabrominated diphenyl ether (decaBDE), hexabromocyclododecane (HBCD) and tetrabromobisphenol A (TBBPA)] were evaluated in the Soxhlet extraction (SE) system. The results showed that acetone-based SE procedure had no measureable effect for the recovery efficiencies of decaBDE but could substantially lower the extraction yields for both TBBPA and HBCD. After 24 h of extraction, the recovery efficiencies of TBBPA and HBCD by SE were 93 and 78% with acetone, 47 and 70% with 3:1 acetone:n-hexane, and 82 and 94% with 1:1 acetone:n-hexane, respectively. After 72 h of extraction, the extraction efficiencies of TBBPA and HBCD decreased to 68 and 55% with acetone, 0 and 5% with 3:1 acetone/n-hexane mixtures, and 0 and 13% with 1:1 acetone/n-hexane mixtures, respectively. The study suggested that the use of acetone alone or acetone-based mixtures should be restricted in the quantitative analysis of HBCD and TBBPA. We further evaluated nine alternative solvents for the extraction of the three BFRs. The result showed that diethyl ether might be reactive with HBCD and may not be considered as the alternative to acetone used solvents for the extraction of HBCD.

Data for free--can an electronic medical record provide outcome data for incontinence/prolapse repair procedures?

PubMed

Steidl, Matthew; Zimmern, Philippe

2013-01-01

We determined whether a custom computer program can improve the extraction and accuracy of key outcome measures from progress notes in an electronic medical record compared to a traditional data recording system for incontinence and prolapse repair procedures. Following institutional review board approval, progress notes were exported from the Epic electronic medical record system for outcome measure extraction by a custom computer program. The extracted data (D1) were compared against a manually maintained outcome measures database (D2). This work took place in 2 phases. During the first phase, volatile data such as questionnaires and standardized physical examination findings using the POP-Q (pelvic organ prolapse quantification) system were extracted from existing progress notes. The second phase used a progress note template incorporating key outcome measures to evaluate improvement in data accuracy and extraction rates. Phase 1 compared 6,625 individual outcome measures from 316 patients in D2 to 3,534 outcome measures extracted from progress notes in D1, resulting in an extraction rate of 53.3%. A subset of 3,763 outcome measures from D1 was created by excluding data that did not exist in the extraction, yielding an accuracy rate of 93.9%. With the use of the template in phase 2, the extraction rate improved to 91.9% (273 of 297) and the accuracy rate improved to 100% (273 of 273). In the field of incontinence and prolapse, the disciplined use of an electronic medical record template containing a preestablished set of key outcome measures can provide the ideal interface between required documentation and clinical research. Copyright © 2013 American Urological Association Education and Research, Inc. Published by Elsevier Inc. All rights reserved.

Comparison of extraction procedures on the immunocontraceptive activity of neem seed extracts.

PubMed

Garg, S; Talwar, G P; Upadhyay, S N

1994-10-01

Azadirachta indica (Neem) seed extracts are known to activate the local cell-mediated immune reactions after a single intrauterine administration, leading to a long term reversible block of fertility. In order to identify and characterize the active fraction responsible for this activity, neem seeds were extracted by both mechanical expression and solvent extraction using a range of polar to non-polar solvents which yielded 3 broad fractions. The mechanically expressed oil was fractionated using different approaches and studied for antifertility activity. The hexane extract and a corresponding column fraction showed potent and reproducible antifertility activity. Other fractions were less stable with regard to reproducibility of effects and composition. It is our conclusion that for subsequent fractionation to reach the last active fraction, the hexane extract is the most useful starting material.

Oxidative stability, phenolic compounds and antioxidant potential of a virgin olive oil enriched with natural bioactive compounds.

PubMed

Delgado-Adámez, Jonathan; Baltasar, M Nieves Franco; Yuste, María Concepción Ayuso; Martín-Vertedor, Daniel

2014-01-01

The aim of this research was to evaluate strategies for the development of a virgin olive oil (VOO) enriched with aqueous extracts of olive leaf and cake to increase the necessary dose in the diet of phenolic compounds with a natural product, as phenolic compounds are involved on the healthy properties of olive oil. Different extraction procedures were evaluated with the aim of increasing the phenol content and antioxidant potential of extracts of olive leaf and cake. As leaves extract presented a higher total phenolic content, it was characterized in order to determine its phenolic profile, and was employed to enrich VOO. Diverse procedures were used to prepare enriched VOO with the leaves extract, and finally the effects of phenol enrichment were evaluated based on the antioxidant potential and oxidative stability of the prepared phenol-enriched virgin olive oils. These enriched VOOs increased significantly the content in phenolic compounds, antioxidant potential and oxidative stability 40, 4 and 1.5 fold more, respectively, than the Control oil. Furthermore, the addition of lecithin had a positive effect both on the phenolic compounds content, and on the antioxidant potential of the oils. Besides, the use of the olive leaves extract, with and without lecithin respectively, supposes a strategy potential for reducing the harmful effects that inflicts long-term preservation of VOOs and its possible deterioration.

Impact of ultrasound on solid-liquid extraction of phenolic compounds from maritime pine sawdust waste. Kinetics, optimization and large scale experiments.

PubMed

Meullemiestre, A; Petitcolas, E; Maache-Rezzoug, Z; Chemat, F; Rezzoug, S A

2016-01-01

Maritime pine sawdust, a by-product from industry of wood transformation, has been investigated as a potential source of polyphenols which were extracted by ultrasound-assisted maceration (UAM). UAM was optimized for enhancing extraction efficiency of polyphenols and reducing time-consuming. In a first time, a preliminary study was carried out to optimize the solid/liquid ratio (6g of dry material per mL) and the particle size (0.26 cm(2)) by conventional maceration (CVM). Under these conditions, the optimum conditions for polyphenols extraction by UAM, obtained by response surface methodology, were 0.67 W/cm(2) for the ultrasonic intensity (UI), 40°C for the processing temperature (T) and 43 min for the sonication time (t). UAM was compared with CVM, the results showed that the quantity of polyphenols was improved by 40% (342.4 and 233.5mg of catechin equivalent per 100g of dry basis, respectively for UAM and CVM). A multistage cross-current extraction procedure allowed evaluating the real impact of UAM on the solid-liquid extraction enhancement. The potential industrialization of this procedure was implemented through a transition from a lab sonicated reactor (3 L) to a large scale one with 30 L volume. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of a gas chromatography/mass spectrometry procedure for confirmation of para-toluenesulfonamide in edible fish fillet tissue

USGS Publications Warehouse

Idowu, O.R.; Kijak, P.J.; Meinertz, J.R.; Schmidt, L.J.

2004-01-01

Chloramine-T is a disinfectant being developed as a treatment for bacterial gill disease in cultured fish. As part of the drug approval process, a method is required for the confirmation of chloramine-T residues in edible fish tissue. The marker residue that will be used to determine the depletion of chloramine-T residues from the edible tissue of treated fish is para-toluenesulfonamide (p-TSA), a metabolite of chloramine-T. The development and validation of a procedure for the confirmation of p-TSA is described. Homogenized fish tissue is dried by mixing with anhydrous sodium sulfate, and the mixture is extracted with methylene chloride. The extract is passed through a silica gel solid-phase extraction column, from which p-TSA is subsequently eluted with acetonitrile. The acetonitrile extract is evaporated, and the oily residue is dissolved in hexane. The hexane solution is shaken with fresh acetonitrile. The acetonitrile solution is evaporated and the residue is redissolved in dilute potassium hydroxide solution. The aqueous solution is extracted with methylene chloride to further remove more of the fat co-extractive. The aqueous solution is reacted with pentafluorobenzyl bromide in presence of tetrabutylammonium hydrogensulfate. The resulting di-(pentafluorobenzyl) derivative of p-TSA is analyzed by gas chromatography/mass spectrometry. This method permits the confirmation of p-TSA in edible fish tissue at 20 ppb.

Development and validation of a gas chromatography/mass spectrometry procedure for confirmation of para-toluenesulfonamide in edible fish fillet tissue.

PubMed

Idowu, Olutosin R; Kijak, Philip J; Meinertz, Jeffery R; Schmidt, Larry J

2004-01-01

Chloramine-T is a disinfectant being developed as a treatment for bacterial gill disease in cultured fish. As part of the drug approval process, a method is required for the confirmation of chloramine-T residues in edible fish tissue. The marker residue that will be used to determine the depletion of chloramine-T residues from the edible tissue of treated fish is para-toluenesulfonamide (p-TSA), a metabolite of chloramine-T. The development and validation of a procedure for the confirmation of p-TSA is described. Homogenized fish tissue is dried by mixing with anhydrous sodium sulfate, and the mixture is extracted with methylene chloride. The extract is passed through a silica gel solid-phase extraction column, from which p-TSA is subsequently eluted with acetonitrile. The acetonitrile extract is evaporated, and the oily residue is dissolved in hexane. The hexane solution is shaken with fresh acetonitrile. The acetonitrile solution is evaporated and the residue is redissolved in dilute potassium hydroxide solution. The aqueous solution is extracted with methylene chloride to further remove more of the fat co-extractive. The aqueous solution is reacted with pentafluorobenzyl bromide in presence of tetrabutylammonium hydrogensulfate. The resulting di-(pentafluorobenzyl) derivative of p-TSA is analyzed by gas chromatography/mass spectrometry. This method permits the confirmation of p-TSA in edible fish tissue at 20 ppb.

Automation of DNA and miRNA co-extraction for miRNA-based identification of human body fluids and tissues.

PubMed

Kulstein, Galina; Marienfeld, Ralf; Miltner, Erich; Wiegand, Peter

2016-10-01

In the last years, microRNA (miRNA) analysis came into focus in the field of forensic genetics. Yet, no standardized and recommendable protocols for co-isolation of miRNA and DNA from forensic relevant samples have been developed so far. Hence, this study evaluated the performance of an automated Maxwell® 16 System-based strategy (Promega) for co-extraction of DNA and miRNA from forensically relevant (blood and saliva) samples compared to (semi-)manual extraction methods. Three procedures were compared on the basis of recovered quantity of DNA and miRNA (as determined by real-time PCR and Bioanalyzer), miRNA profiling (shown by Cq values and extraction efficiency), STR profiles, duration, contamination risk and handling. All in all, the results highlight that the automated co-extraction procedure yielded the highest miRNA and DNA amounts from saliva and blood samples compared to both (semi-)manual protocols. Also, for aged and genuine samples of forensically relevant traces the miRNA and DNA yields were sufficient for subsequent downstream analysis. Furthermore, the strategy allows miRNA extraction only in cases where it is relevant to obtain additional information about the sample type. Besides, this system enables flexible sample throughput and labor-saving sample processing with reduced risk of cross-contamination. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of nonylphenol and nonylphenol ethoxylates in environmental solid samples by ultrasonic-assisted extraction and high performance liquid chromatography-fluorescence detection.

PubMed

Núñez, L; Turiel, E; Tadeo, J L

2007-04-06

A simple and rapid analytical method for the determination of nonylphenol (NP) and nonylphenol ethoxylates (NPEOx) in solid environmental samples has been developed. This method combines an ultrasonic-assisted extraction procedure in small columns and an enrichment step onto C(18) solid-phase extraction cartridges prior to separation using HPLC with fluorescence detection. Method optimization was carried out using soil samples fortified at different concentration levels (from 0.1 to 100 microg/g). Under optimum conditions, 2g of soil was placed in small glass columns and extraction was performed assisted by sonication (SAESC) at 45 degrees C in two consecutive steps of 15 min using a mixture of H(2)O/MeOH (30/70). The obtained extracts were collected, loaded onto 500 mg C(18) cartridges, and analytes were eluted with 3 x 1 ml of methanol and 1 ml of acetonitrile. Finally, sample extracts were evaporated under a nitrogen stream, redissolved in 500 microl H(2)O/AcN (50/50), and passed though a 0.45 microm nylon filter before final determination by HPLC-FL. The developed procedure allowed to achieve quantitative recoveries for NP and NPEOx, and was properly validated. Finally, the method was applied to the determination of these compounds in soils and other environmental solid samples such as sediments, compost and sludge.

Synthesis and application of molecularly imprinted polymers for the selective extraction of organophosphorus pesticides from vegetable oils.

PubMed

Boulanouar, Sara; Combès, Audrey; Mezzache, Sakina; Pichon, Valérie

2017-09-01

The increasing use of pesticides in agriculture causes environmental issues and possible serious health risks to humans and animals. Their determination at trace concentrations in vegetable oils constitutes a significant analytical challenge. Therefore, their analysis often requires both an extraction and a purification step prior to separation with liquid chromatography (LC) and mass spectrometry (MS) detection. This work aimed at developing sorbents that are able to selectively extract from vegetable oil samples several organophosphorus (OPs) pesticides presenting a wide range of physico-chemical properties. Therefore, different conditions were screened to prepare molecularly imprinted polymers (MIPs) by a non-covalent approach. The selectivity of the resulting polymers was evaluated by studying the OPs retention in pure media on both MIPs and non-imprinted polymers (NIP) used as control. The most promising MIP sorbent was obtained using monocrotophos (MCP) as the template, methacrylic acid (MAA) as the monomer and ethylene glycol dimethacrylate (EGDMA) as the cross-linker with a molar ratio of 1/4/20 respectively. The repeatability of the extraction procedure and of the synthesis procedure was demonstrated in pure media. The capacity of this MIP was 1mg/g for malathion. This MIP was also able to selectively extract three OPs from almond oil by applying the optimized SPE procedure. Recoveries were between 73 and 99% with SD values between 4 and 6% in this oil sample. The calculated LOQs (between 0.3 and 2μg/kg) in almond seeds with a SD between 0.1 and 0.4μg/kg were lower than the Maximum Residue Levels (MRLs) established for the corresponding compounds in almond seed. Copyright © 2017 Elsevier B.V. All rights reserved.

Chemical speciation and recovery of gold(I, III) from wastewater and silver by liquid-liquid extraction with the ion-pair reagent amiloride mono hydrochloride and AAS determination.

PubMed

El-Shahawi, M S; Bashammakh, A S; Bahaffi, S O

2007-06-15

A novel and low cost liquid-liquid extraction procedure for the separation of gold(III) at trace level from aqueous medium of pH 5-9 has been developed. The method has been based upon the formation of a yellow colored ternary complex ion associate of tetrachloro gold(III) complex anion, AuCl(4)(-) with the ion-pair reagent 1-(3,5-diamino-6-chloropyrazinecarboxyl) guanidine hydrochloride monohydrate, namely amiloride, DPG(+).Cl(-). The effect of various parameters, e.g. pH, organic solvent, shaking time, etc. on the preconcentration of gold(III) from the aqueous media by the DPG(+).Cl(-) reagent has been investigated. The colored gold species was quantitatively extracted into 4-methyl pentan-2-one. The chemical composition of the ion associate of DPG(+).Cl(-) with AuCl(4)(-) in the organic solvent has been determined by the Job's method. The molar absorptivity (2.19x10(4)Lmol(-1)cm(-1)) of the associate DPG(+).AuCl(4)(-) at 362nm enabled a convenient application of the developed extraction procedure for the separation and AAS determination of traces of aurate ions. Mono-valence gold ions after oxidation to gold(III) with bromine water in HCl (1.0molL(-1)) media have been also extracted quantitatively from the aqueous media by the developed procedure. The chemical speciation of mono- and/or tri-valence gold species spiked to fresh and industrial wastewater samples has been achieved. The method has been also applied successfully from the separation of gold(I) and gold(III) species from metallic ions and silver. The developed method has also the advantage of freedom from most diverse ions.

The use of multimedia consent programs for surgical procedures: a systematic review.

PubMed

Nehme, Jean; El-Khani, Ussamah; Chow, Andre; Hakky, Sherif; Ahmed, Ahmed R; Purkayastha, Sanjay

2013-02-01

To compare multimedia and standard consent, in respect to patient comprehension, anxiety, and satisfaction, for various surgical/interventional procedures. Electronic searches of PubMed, MEDLINE, Ovid, Embase, and Google Scholar were performed. Relevant articles were assessed by 2 independent reviewers. Comparative (randomized and nonrandomized control trials) studies of multimedia and standard consent for a variety of surgical/interventional procedures were included. Studies had to report on at least one of the outcome measures. Studies were reviewed by 2 independent investigators. The first investigator extracted all relevant data, and consensus of each extraction was performed by a second investigator to verify the data. Overall, this review suggests that the use of multimedia as an adjunct to conventional consent appears to improve patient comprehension. Multimedia leads to high patient satisfaction in terms of feasibility, ease of use, and availability of information. There is no conclusive evidence demonstrating a significant reduction in preoperative anxiety.

Procedures adopted by orthodontists for space closure and anchorage control.

PubMed

Monini, André da Costa; Gandini Júnior, Luiz Gonzaga; dos Santos-Pinto, Ary; Maia, Luiz Guilherme Martins; Rodrigues, Willian Caetano

2013-01-01

The aim of this study was to identify the procedures adopted by Brazilian orthodontists in the following situations: extraction space closure, anchorage control in case of necessary anchorage for group A and frequency of skeletal anchorage use, especially in the upper jaw. A questionnaire was sent to the e-mail address of all dentists registered in the Brazilian Federal Council of Dentistry. The results showed that most Brazilian orthodontists usually perform extraction space closure by means of sliding mechanics. The use of palatal bar, inclusion of second molars in the archwire and space closure performed in two phases are the most used techniques for anchorage control in the upper jaw. The skeletal anchorage is referenced by 36.5% of specialists as a routine practice for the upper arch anchorage. There is a wide variety of procedures adopted by Brazilian orthodontists for orthodontic space closure and anchorage control.

Validation of an automated solid-phase extraction method for the analysis of 23 opioids, cocaine, and metabolites in urine with ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Ramírez Fernández, María del Mar; Van Durme, Filip; Wille, Sarah M R; di Fazio, Vincent; Kummer, Natalie; Samyn, Nele

2014-06-01

The aim of this work was to automate a sample preparation procedure extracting morphine, hydromorphone, oxymorphone, norcodeine, codeine, dihydrocodeine, oxycodone, 6-monoacetyl-morphine, hydrocodone, ethylmorphine, benzoylecgonine, cocaine, cocaethylene, tramadol, meperidine, pentazocine, fentanyl, norfentanyl, buprenorphine, norbuprenorphine, propoxyphene, methadone and 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine from urine samples. Samples were extracted by solid-phase extraction (SPE) with cation exchange cartridges using a TECAN Freedom Evo 100 base robotic system, including a hydrolysis step previous extraction when required. Block modules were carefully selected in order to use the same consumable material as in manual procedures to reduce cost and/or manual sample transfers. Moreover, the present configuration included pressure monitoring pipetting increasing pipetting accuracy and detecting sampling errors. The compounds were then separated in a chromatographic run of 9 min using a BEH Phenyl analytical column on a ultra-performance liquid chromatography-tandem mass spectrometry system. Optimization of the SPE was performed with different wash conditions and elution solvents. Intra- and inter-day relative standard deviations (RSDs) were within ±15% and bias was within ±15% for most of the compounds. Recovery was >69% (RSD < 11%) and matrix effects ranged from 1 to 26% when compensated with the internal standard. The limits of quantification ranged from 3 to 25 ng/mL depending on the compound. No cross-contamination in the automated SPE system was observed. The extracted samples were stable for 72 h in the autosampler (4°C). This method was applied to authentic samples (from forensic and toxicology cases) and to proficiency testing schemes containing cocaine, heroin, buprenorphine and methadone, offering fast and reliable results. Automation resulted in improved precision and accuracy, and a minimum operator intervention, leading to safer sample handling and less time-consuming procedures.

Internet pseudoscience: Testing opioid containing formulations with tampering potential.

PubMed

Pascali, Jennifer P; Fais, Paolo; Vaiano, Fabio; Pigaiani, Nicola; D'Errico, Stefano; Furlanetto, Sandra; Palumbo, Diego; Bertol, Elisabetta

2018-05-10

Drug tampering practices, with the aim to increase availability of drug delivery and/or enhance drug effects, are accessible on Internet and are practiced by some portion of recreational drug users. Not rarely, recreational misuse may result in toxic and even fatal results. The aim of the present study was to assess the tampering risk of medicaments containing different formulations of an opioid in combination with paracetamol or dexketoprofen, following the procedures reported in dedicated forums on the web. Tablets and suppositories containing codeine, tramadol and oxycodone were extracted following the reported "Cold water extraction"; dextromethorphan was extracted from cough syrup following the procedure reported as "Acid/base extraction" and fentanyl was extracted from transdermal patches according the procedure reported in Internet. The tampered products and opportunely prepared calibrators in water were analysed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The separation of the analytes was carried on Agilent ZORBAX Eclipse Plus C18 (RRHT 2.1 mm × 50 mm, 1.8 μm) by the gradient elution of 0.01% formic acid in water and 0.01% formic acid in methanol. Acquisition was by MRM mode considering at least two transitions for compound. Declared recoveries for these home-made extractions claimed to exceed 99% for the opioid and to complete remove paracetamol, often associated to liver toxicity and thus to obtain a "safer" preparation. In this study, the authors demonstrated that rarely the recoveries for the opioid reached 90% and that up to 60% of the paracetamol amount remained in solution. Thus, high risks for health remained both for the potential lethality of the opioid content, but also for the sub-lethal chronic use of these mixtures, which contained still uncontrolled, ignored, but often important amounts of paracetamol. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparing silica aerogel monoliths via a rapid supercritical extraction method.

PubMed

Carroll, Mary K; Anderson, Ann M; Gorka, Caroline A

2014-02-28

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The procedure requires 15-20 min of preparation time, during which a liquid precursor mixture is prepared and poured into wells of a metal mold that is placed between the platens of a hydraulic hot press, followed by several hours of processing within the hot press. The precursor solution consists of a 1.0:12.0:3.6:3.5 x 10(-3) molar ratio of tetramethylorthosilicate (TMOS):methanol:water:ammonia. In each well of the mold, a porous silica sol-gel matrix forms. As the temperature of the mold and its contents is increased, the pressure within the mold rises. After the temperature/pressure conditions surpass the supercritical point for the solvent within the pores of the matrix (in this case, a methanol/water mixture), the supercritical fluid is released, and monolithic aerogel remains within the wells of the mold. With the mold used in this procedure, cylindrical monoliths of 2.2 cm diameter and 1.9 cm height are produced. Aerogels formed by this rapid method have comparable properties (low bulk and skeletal density, high surface area, mesoporous morphology) to those prepared by other methods that involve either additional reaction steps or solvent extractions (lengthier processes that generate more chemical waste).The rapid supercritical extraction method can also be applied to the fabrication of aerogels based on other precursor recipes.

Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

PubMed Central

Gorka, Caroline A.

2014-01-01

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The procedure requires 15-20 min of preparation time, during which a liquid precursor mixture is prepared and poured into wells of a metal mold that is placed between the platens of a hydraulic hot press, followed by several hours of processing within the hot press. The precursor solution consists of a 1.0:12.0:3.6:3.5 x 10-3 molar ratio of tetramethylorthosilicate (TMOS):methanol:water:ammonia. In each well of the mold, a porous silica sol-gel matrix forms. As the temperature of the mold and its contents is increased, the pressure within the mold rises. After the temperature/pressure conditions surpass the supercritical point for the solvent within the pores of the matrix (in this case, a methanol/water mixture), the supercritical fluid is released, and monolithic aerogel remains within the wells of the mold. With the mold used in this procedure, cylindrical monoliths of 2.2 cm diameter and 1.9 cm height are produced. Aerogels formed by this rapid method have comparable properties (low bulk and skeletal density, high surface area, mesoporous morphology) to those prepared by other methods that involve either additional reaction steps or solvent extractions (lengthier processes that generate more chemical waste).The rapid supercritical extraction method can also be applied to the fabrication of aerogels based on other precursor recipes. PMID:24637334

Automated extraction of natural drainage density patterns for the conterminous United States through high performance computing

USGS Publications Warehouse

Stanislawski, Larry V.; Falgout, Jeff T.; Buttenfield, Barbara P.

2015-01-01

Hydrographic networks form an important data foundation for cartographic base mapping and for hydrologic analysis. Drainage density patterns for these networks can be derived to characterize local landscape, bedrock and climate conditions, and further inform hydrologic and geomorphological analysis by indicating areas where too few headwater channels have been extracted. But natural drainage density patterns are not consistently available in existing hydrographic data for the United States because compilation and capture criteria historically varied, along with climate, during the period of data collection over the various terrain types throughout the country. This paper demonstrates an automated workflow that is being tested in a high-performance computing environment by the U.S. Geological Survey (USGS) to map natural drainage density patterns at the 1:24,000-scale (24K) for the conterminous United States. Hydrographic network drainage patterns may be extracted from elevation data to guide corrections for existing hydrographic network data. The paper describes three stages in this workflow including data pre-processing, natural channel extraction, and generation of drainage density patterns from extracted channels. The workflow is concurrently implemented by executing procedures on multiple subbasin watersheds within the U.S. National Hydrography Dataset (NHD). Pre-processing defines parameters that are needed for the extraction process. Extraction proceeds in standard fashion: filling sinks, developing flow direction and weighted flow accumulation rasters. Drainage channels with assigned Strahler stream order are extracted within a subbasin and simplified. Drainage density patterns are then estimated with 100-meter resolution and subsequently smoothed with a low-pass filter. The extraction process is found to be of better quality in higher slope terrains. Concurrent processing through the high performance computing environment is shown to facilitate and refine the choice of drainage density extraction parameters and more readily improve extraction procedures than conventional processing.

Deaths and cardiovascular injuries due to device-assisted implantable cardioverter–defibrillator and pacemaker lead extraction

PubMed Central

Hauser, Robert G.; Katsiyiannis, William T.; Gornick, Charles C.; Almquist, Adrian K.; Kallinen, Linda M.

2010-01-01

Aims An estimated 10 000–15 000 pacemaker and implantable cardioverter–defibrillator (ICD) leads are extracted annually worldwide using specialized tools that disrupt encapsulating fibrous tissue. Additional information is needed regarding the safety of the devices that have been approved for lead extraction. The aim of this study was to determine whether complications due to device-assisted lead extraction might be more hazardous than published data suggest, and whether procedural safety precautions are effective. Methods and results We searched the US Food and Drug Administration's (FDA) Manufacturers and User Defined Experience (MAUDE) database from 1995 to 2008 using the search terms ‘lead extraction and death’ and ‘lead extraction and injury’. Additional product specific searches were performed for the terms ‘death’ and ‘injury’. Between 1995 and 2008, 57 deaths and 48 serious cardiovascular injuries associated with device-assisted lead extraction were reported to the FDA. Owing to underreporting, the FDA database does not contain all adverse events that occurred during this period. Of the 105 events, 27 deaths and 13 injuries occurred in 2007–2008. During these 2 years, 23 deaths were linked with excimer laser or mechanical dilator sheath extractions. The majority of deaths and injuries involved ICD leads, and most were caused by lacerations of the right atrium, superior vena cava, or innominate vein. Overall, 62 patients underwent emergency surgical repair of myocardial perforations and venous lacerations and 35 (56%) survived. Conclusion These findings suggest that device-assisted lead extraction is a high-risk procedure and that serious complications including death may not be mitigated by emergency surgery. However, skilled standby cardiothoracic surgery is essential when performing pacemaker and ICD lead extractions. Although the incidence of these complications is unknown, the results of our study imply that device-assisted lead extractions should be performed by highly qualified physicians and their teams in specialized centres. PMID:19946113

Antimicrobial activity and chemical analysis of Microlicia hatschbachii Wurdack (Melastomataceae) extract.

PubMed

Cassiano, Dayse S A; Pacheco, Alessandra G M; da Costa, Mateus M; Almeida, Jackson R G S; Vieira, Ivo J C; Branco, Alexsandro

2014-01-01

Aerial parts of Microlicia hatschbachii were extracted with hexane, and the extract was evaluated for antimicrobial activity by a broth dilution method. After phytochemical procedures: GC-MS identified aliphatic alkanes, carboxylic acids and methyl esters of long-chain fatty acids; and two diterpenoids [labd-8(17)-en-15-oic acid and labd-8(17),13-dien-15-oic acid] were identified by (1)H and (13)C NMR. The antimicrobial activity of the hexane extract could be attributed to the presence of labdanes. This identification is the first reported occurrence of labdane diterpenes in the Melastomataceae family.

QUANTITATIVE RADIO-CHEMICAL ANALYSIS-SOLVENT EXTRACTION OF MOLYBDENUM-99

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wish, L.

1961-09-12

A method was developed for the rapid quantitative separation of Mo/sup 99/ from fission product mixtures. It is based on the extraction of Mo into a solution of alpha -benzoin oxime in chloroform. The main contaminants are Zr, Nb, and 1. The first two are eliminated by couple with fluoride and the third by volatilization or solvent extraction. About 5% of the Te/sup 99/ daughter is extracted with its parent, and it is necessary to wait 48 hrs for equilibrium of fission product mixtures by this method and a standard radiochemical gravimetric procedure showed agreement within 1 to 2%. (auth)

Study of process variables in supercritical carbon dioxide extraction of soybeans.

PubMed

Wilkinson, Nikolas; Hilton, Ramsey; Hendry, Doug; Venkitasamy, Chandrasekar; Jacoby, William

2014-01-01

Soybean flakes were extracted using supercritical carbon dioxide at 48.3 MPa and 80 °C, which is a higher temperature than previously reported. Several operational parameters were explored to determine their effect on extractions. Flakes, as typically used in this industry, provided the best extraction performance. Particle size distributions were created through grinding. Reducing average particle diameters smaller than 0.069 mm had no appreciable effect on increasing extraction efficiencies. Exploration of flow rate indicated that a residence time of less than 60 s for the supercritical carbon dioxide would be sufficient for complete extractions. A solvent mass to load mass ratio of 10:1 was found to be sufficient for extraction of oils from soybean flakes. Increasing moisture in the soybeans led to decreasing extraction efficiency of oils. Finally, soybean hulls had no effect on extraction efficiency. Thus, the de-hulling procedure can be removed from the extraction process without decreasing extraction efficiency.

Long‐term Outcomes of Catheter Ablation of Atrial Fibrillation: A Systematic Review and Meta‐analysis

PubMed Central

Ganesan, Anand N.; Shipp, Nicholas J.; Brooks, Anthony G.; Kuklik, Pawel; Lau, Dennis H.; Lim, Han S.; Sullivan, Thomas; Roberts‐Thomson, Kurt C.; Sanders, Prashanthan

2013-01-01

Background In the past decade, catheter ablation has become an established therapy for symptomatic atrial fibrillation (AF). Until very recently, few data have been available to guide the clinical community on the outcomes of AF ablation at ≥3 years of follow‐up. We aimed to systematically review the medical literature to evaluate the long‐term outcomes of AF ablation. Methods and Results A structured electronic database search (PubMed, Embase, Web of Science, Cochrane) of the scientific literature was performed for studies describing outcomes at ≥3 years after AF ablation, with a mean follow‐up of ≥24 months after the index procedure. The following data were extracted: (1) single‐procedure success, (2) multiple‐procedure success, and (3) requirement for repeat procedures. Data were extracted from 19 studies, including 6167 patients undergoing AF ablation. Single‐procedure freedom from atrial arrhythmia at long‐term follow‐up was 53.1% (95% CI 46.2% to 60.0%) overall, 54.1% (95% CI 44.4% to 63.4%) in paroxysmal AF, and 41.8% (95% CI 25.2% to 60.5%) in nonparoxysmal AF. Substantial heterogeneity (I2>50%) was noted for single‐procedure outcomes. With multiple procedures, the long‐term success rate was 79.8% (95% CI 75.0% to 83.8%) overall, with significant heterogeneity (I2>50%).The average number of procedures per patient was 1.51 (95% CI 1.36 to 1.67). Conclusions Catheter ablation is an effective and durable long‐term therapeutic strategy for some AF patients. Although significant heterogeneity is seen with single procedures, long‐term freedom from atrial arrhythmia can be achieved in some patients, but multiple procedures may be required. PMID:23537812

Variation in levels of some leaf enzymes.

PubMed

Downton, J; Slatyer, R O

1971-03-01

Several procedures were compared for efficiency in the extraction of certain leaf enzymes (phosphoenolpyruvate carboxylase, ribulose 1,5-diphosphate carboxylase and malate dehydrogenase) in Atriplex hastata (a "C3" species exhibiting conventional photosynthetic metabolism), and in A. spongiosa (a "C4" species in which the initial photosynthetic products are C4 dicarboxylic acids). Glycolate oxidase was also assayed in some cases, and Atriplex nummularia and Sorghum bicolor were also used as test material. A simple procedure, involving a mortar and pestle grind with carborundum added to the grinding mixture, was found to be as effective as glass bead grind procedures. In addition, it was more rapid and showed less variability with different operations.Using the carborundum grind procedure, sources of variability in enzyme activity in apparently uniform leaves were compared, as were effects of time of day, leaf age and storage procedure. In general, if apparently uniform leaves could be selected, variability in levels of enzyme activity appeared to be relatively small, not exceeding about 12%. Time of day also appeared to be relatively unimportant for the enzymes examined. However, the ontogentic status of the plant was found to be an important source of variability. Leaf age was also a major source of variability where the activity was expressed on a fresh weight basis, but specific activity (i.e. activity expressed on a protein basis) was relatively constant, at least with the range of species and leaf ages examined here.Storage of fresh samples in liquid nitrogen for 24 h, prior to extraction and assay, led to only a small reduction in activity, but substantial changes occurred if storage was in dry ice or in ice and also where extracts were stored in a deep freeze.

Use of Antibiotic Prophylaxis for Tooth Extractions, Dental Implants, and Periodontal Surgical Procedures

PubMed Central

Henschel, Heather; Patel, Ursula; Fitzpatrick, Margaret A; Evans, Charlesnika T

2018-01-01

Abstract Background Guidelines for antibiotics prior to dental procedures for patients with specific cardiac conditions and prosthetic joints have changed, reducing indications for antibiotic prophylaxis. In addition to guidelines focused on patient comorbidities, systematic reviews specific to dental extractions and implants support preprocedure antibiotics for all patients. However, data on dentist adherence to these recommendations are scarce. Methods This was a cross-sectional study of veterans undergoing tooth extractions, dental implants, and periodontal procedures. Patients receiving antibiotics for oral or nonoral infections were excluded. Data were collected through manual review of the health record. Results Of 183 veterans (mean age, 62 years; 94.5% male) undergoing the included procedures, 82.5% received antibiotic prophylaxis (mean duration, 7.1 ± 1.6 days). Amoxicillin (71.3% of antibiotics) and clindamycin (23.8%) were prescribed most frequently; 44.7% of patients prescribed clindamycin were not labeled as penicillin allergic. Of those who received prophylaxis, 92.1% received postprocedure antibiotics only, 2.6% received preprocedural antibiotics only, and 5.3% received pre- and postprocedure antibiotics. When prophylaxis was indicated, 87.3% of patients received an antibiotic. However, 84.9% received postprocedure antibiotics when preprocedure administration was indicated. While the majority of antibiotics were indicated, only 8.2% of patients received antibiotics appropriately. The primary reason was secondary to prolonged duration. Three months postprocedure, there were no occurrences of Clostridium difficile infection, infective endocarditis, prosthetic joint infections, or postprocedure oral infections. Conclusion The majority of patients undergoing a dental procedure received antibiotic prophylaxis as indicated. Although patients for whom antibiotic prophylaxis was indicated should have received a single preprocedure dose, most antibiotics were prescribed postprocedure. Dental stewardship efforts should ensure appropriate antibiotic timing, indication, and duration. PMID:29326959

Comparison of six extraction techniques for isolation of DNA from filamentous fungi.

PubMed

van Burik, J A; Schreckhise, R W; White, T C; Bowden, R A; Myerson, D

1998-10-01

Filamentous fungi have a sturdy cell wall which is resistant to the usual DNA extraction procedures. We determined the DNA extraction procedure with the greatest yield of high quality fungal DNA and the least predilection for cross-contamination of equipment between specimens. Each of six extraction methods was performed using Aspergillus fumigatus hyphae. The six methods were: (1) glass bead pulverization with vortexing; (2) grinding with mortar and pestle followed by glass bead pulverization; (3) glass bead pulverization using 1% hydroxyacetyl trimethyl ammonium bromide (CTAB) buffer in a water bath sonicator; (4) water bath sonication in CTAB buffer; (5) grinding followed by incubation with CTAB; and (6) lyticase enzymatic cell lysis. Genomic DNA yields were measured by spectrophotometry and by visual reading of 2% agarose gels, with shearing assessed by the migration of the DNA on the gel. Genomic fungal DNA yields were highest for Method 1, followed by Methods 5 approximately = to 2 >3 approximately = to 4 approximately = to 6. Methods 2 and 5, both of which involved grinding with mortar and pestle, led to shearing of the genomic DNA in one of two trials each. We conclude that the use of glass beads with extended vortexing is optimal for extraction of microgramme amounts of DNA from filamentous fungal cultures.

Assessment of priority pesticides, degradation products, and pesticide adjuvants in groundwaters and top soils from agricultural areas of the Ebro river basin.

PubMed

Hildebrandt, Alain; Lacorte, Sílvia; Barceló, Damià

2007-02-01

Gas chromatography-mass spectrometry (GC/MS) was employed for the determination of 30 widely used pesticides including various transformation products and alkylphenols in water and agricultural soils with the aim of assessing the impact of these compounds in agricultural soils and the underlying aquifer. The extraction, clean-up, and analytical procedures were optimized for both water and soil samples to provide a highly robust method capable of determining target analytes at the ppb-ppt level with high precision. For water samples, different solid-phase extraction cartridges and conditions were optimized; similarly, pressurized liquid extraction conditions were tested to provide interference-free extracts and high sensitivity. Instrumental LODs of 3-4 pg were obtained. The multi-residue extraction procedures were applied to the analysis of groundwaters and agricultural soils from the Ebro river basin (NE Spain). Most ubiquitous herbicides detected were triazines but some acetanilides and organophosphorus pesticides were also found; the pesticide additive tributylphosphate was found in all water samples. Levels varied between 0.57 and 5.37 microg/L in groundwater, whereas nonylphenol was the sole compound detected in soil. Alkylphenols are used as adjuvants in pesticide formulations and are present in sludges employed as soil fertilizers. Occurrence was found to be similar to other environmental studies.

Vortex assisted solid-phase extraction of lead(II) using orthorhombic nanosized Bi2WO6 as a sorbent.

PubMed

Baghban, Neda; Yilmaz, Erkan; Soylak, Mustafa

2017-12-07

Nanosized single crystal orthorhombic Bi 2 WO 6 was synthesized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The crystal and molecular structure of the sorbent was examined using XRD, Raman, SEM and SEM-EDX analysis. Various parameters affecting extraction efficiency were optimized by using multivariate design. The effect of diverse ions on the extraction also was studied. Lead was quantified by flame atomic absorption spectrometry (FAAS). The recoveries of lead(II) from spiked samples (at a typical spiking level of 200-400 ng·mL -1 ) are >95%. Other figures of merit includes (a) a detection limit of 6 ng·mL -1 , (b) a preconcentration factor of 50, (c) a relative standard deviation of 1.6%, and (d) and adsorption capacity of 6.6 mg·g -1 . The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples. Graphical abstract Nanosized single crystal orthorhombic Bi 2 WO 6 was synthesized and characterized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples.