A comparison of juice extraction methods in the pungency measurement of onion bulbs.

PubMed

Yoo, Kil Sun; Lee, Eun Jin; Hamilton, Brian K; Patil, Bhimanagouda S

2016-02-01

Onion pungency is estimated by measuring the pyruvic acid content in juice extracted from fresh tissues. We compared pyruvic acid content and its variation in the juices extracted by the pressing, maceration, blending with no water, or blending with water (blend/water) methods. There were considerable differences in the pyruvic acid content and coefficient of variation (CV) among these methods, and there was an interaction between the onion cultivars and the juice extraction methods. The pressing method showed over 30% CV in the quartered or composite samples. The blend/water method showed the greatest pyruvic acid content in the shortday-type ('TG1015Y' and 'Texas Early White') onions, while the pressing method showed the greatest pyruvic acid content in the longday-type onions. The blend/water method, which gave ratios between 1:1 and 1:4 (w/w), showed the same pyruvic acid content. The blending (no water) method had the highest correlation, followed by the maceration method. The lowest correlations were found with the pressing method and the blend/water method. Complete homogenisation of tissues with 1:1 or greater ratios of water was necessary for the maximum consistency and full development of the pyruvic acid reaction for onion pungency measurement. © 2015 Society of Chemical Industry.

Effectiveness of Liquid-Liquid Extraction, Solid Phase Extraction, and Headspace Technique for Determination of Some Volatile Water-Soluble Compounds of Rose Aromatic Water

PubMed Central

2017-01-01

Steam distillation is used to isolate scent of rose flowers. Rose aromatic water is commonly used in European cuisine and aromatherapy besides its use in cosmetic industry for its lovely scent. In this study, three different sampling techniques, liquid-liquid extraction (LLE), headspace technique (HS), and solid phase extraction (SPE), were compared for the analysis of volatile water-soluble compounds in commercial rose aromatic water. Some volatile water-soluble compounds of rose aromatic water were also analyzed by gas chromatography mass spectrometry (GCMS). In any case, it was concluded that one of the solid phase extraction methods led to higher recoveries for 2-phenylethyl alcohol (PEA) in the rose aromatic water than the liquid-liquid extraction and headspace technique. Liquid-liquid extraction method provided higher recovery ratios for citronellol, nerol, and geraniol than others. Ideal linear correlation coefficient values were observed by GCMS for quantitative analysis of volatile compounds (r2 ≥ 0.999). Optimized methods showed acceptable repeatability (RSDs < 5%) and excellent recovery (>95%). For compounds such as α-pinene, linalool, β-caryophyllene, α-humulene, methyl eugenol, and eugenol, the best recovery values were obtained with LLE and SPE. PMID:28791049

Critical Evaluation of Soil Pore Water Extraction Methods on a Natural Soil

NASA Astrophysics Data System (ADS)

Orlowski, Natalie; Pratt, Dyan; Breuer, Lutz; McDonnell, Jeffrey

2017-04-01

Soil pore water extraction is an important component in ecohydrological studies for the measurement of δ2H and δ18O. The effect of pore water extraction technique on resultant isotopic signature is poorly understood. Here we present results of an intercomparison of commonly applied lab-based soil water extraction techniques on a natural soil: high pressure mechanical squeezing, centrifugation, direct vapor equilibration, microwave extraction, and two types of cryogenic extraction systems. We applied these extraction methods to a natural summer-dry (gravimetric water contents ranging from 8% to 15%) glacio-lacustrine, moderately fine textured clayey soil; excavated in 10 cm sampling increments to a depth of 1 meter. Isotope results were analyzed via OA-ICOS and compared for each extraction technique that produced liquid water. From our previous intercomparison study among the same extraction techniques but with standard soils, we discovered that extraction methods are not comparable. We therefore tested the null hypothesis that all extraction techniques would be able to replicate the natural evaporation front in a comparable manner occurring in a summer-dry soil. Our results showed that the extraction technique utilized had a significant effect on the soil water isotopic composition. High pressure mechanical squeezing and vapor equilibration techniques produced similar results with similarly sloped evaporation lines. Due to the nature of soil properties and dryness, centrifugation was unsuccessful in obtaining pore water for isotopic analysis. Cryogenic extraction on both tested techniques produced similar results to each other on a similar sloping evaporation line, but dissimilar with depth.

A novel star extraction method based on modified water flow model

NASA Astrophysics Data System (ADS)

Zhang, Hao; Niu, Yanxiong; Lu, Jiazhen; Ouyang, Zibiao; Yang, Yanqiang

2017-11-01

Star extraction is the essential procedure for attitude measurement of star sensor. The great challenge for star extraction is to segment star area exactly from various noise and background. In this paper, a novel star extraction method based on Modified Water Flow Model(MWFM) is proposed. The star image is regarded as a 3D terrain. The morphology is adopted for noise elimination and Tentative Star Area(TSA) selection. Star area can be extracted through adaptive water flowing within TSAs. This method can achieve accurate star extraction with improved efficiency under complex conditions such as loud noise and uneven backgrounds. Several groups of different types of star images are processed using proposed method. Comparisons with existing methods are conducted. Experimental results show that MWFM performs excellently under different imaging conditions. The star extraction rate is better than 95%. The star centroid accuracy is better than 0.075 pixels. The time-consumption is also significantly reduced.

Effect of solvent type and high pressure treatment on the extraction of Gomphrena globosa L. bioactive compounds

NASA Astrophysics Data System (ADS)

Fernandes, L.; Ramalhosa, E.; Pereira, J. A.; Casal, S.; Saraiva, J. A.

2017-10-01

The present study aimed to compare the influence of different extraction solvents (water, methanol, water:acetone (6:4, v/v)), methods (heating (37 °C, 30 min) or high pressure (HP) (300 or 500 MPa) and extraction time (7.5 or 15 min)) on flavonoids, hydrolysable tannins and antioxidant activity (Total Reducing Capacity (TRC), DPPH Free Radical Scavenging Activity and Reducing Power) of Gomphrena globosa L. flower extracts. The water:acetone extracts obtained by heating had the highest values of flavonoids, hydrolysable tannins and antioxidant activity. When applying HP, variable results were obtained. Still, the application of HP to water allowed to extract more hydrolysable tannins, as well as to obtain extracts with higher antioxidant activity than with heating, but no significant alterations were observed with methanol. In conclusion, both solvent and extraction method influence the content of bioactive compounds, being HP treatment a promising method to obtain enriched aqueous extracts in line with the principles of green-chemistry.

Membrane contactor assisted water extraction system for separating hydrogen peroxide from a working solution, and method thereof

DOEpatents

Snyder, Seth W [Lincolnwood, IL; Lin, Yupo J [Naperville, IL; Hestekin', Jamie A [Fayetteville, AR; Henry, Michael P [Batavia, IL; Pujado, Peter [Kildeer, IL; Oroskar, Anil [Oak Brook, IL; Kulprathipanja, Santi [Inverness, IL; Randhava, Sarabjit [Evanston, IL

2010-09-21

The present invention relates to a membrane contactor assisted extraction system and method for extracting a single phase species from multi-phase working solutions. More specifically one preferred embodiment of the invention relates to a method and system for membrane contactor assisted water (MCAWE) extraction of hydrogen peroxide (H.sub.2O.sub.2) from a working solution.

Screening of extraction methods for glycoproteins from jellyfish ( Rhopilema esculentum) oral-arms by high performance liquid chromatography

NASA Astrophysics Data System (ADS)

Ren, Guoyan; Li, Bafang; Zhao, Xue; Zhuang, Yongliang; Yan, Mingyan; Hou, Hu; Zhang, Xiukun; Chen, Li

2009-03-01

In order to select an optimum extraction method for the target glycoprotein (TGP) from jellyfish ( Rhopilema esculentum) oral-arms, a high performance liquid chromatography (HPLC)-assay for the determination of the TGP was developed. Purified target glycoprotein was taken as a standard glycoprotein. The results showed that the calibration curves for peak area plotted against concentration for TGP were linear ( r = 0.9984, y = 4.5895 x+47.601) over concentrations ranging from 50 to 400 mgL-1. The mean extraction recovery was 97.84% (CV2.60%). The fractions containing TGP were isolated from jellyfish ( R. esculentum) oral-arms by four extraction methods: 1) water extraction (WE), 2) phosphate buffer solution (PBS) extraction (PE), 3) ultrasound-assisted water extraction (UA-WE), 4) ultrasound-assisted PBS extraction (UA-PE). The lyophilized extract was dissolved in Milli-Q water and analyzed directly on a short TSK-GEL G4000PWXL (7.8 mm×300 mm) column. Our results indicated that the UA-PE method was the optimum extraction method selected by HPLC.

Study on antibacterial effect of medlar and hawthorn compound extract in vitro.

PubMed

Niu, Yang; Nan, Yi; Yuan, Ling; Wang, Rong

2013-01-01

This paper evaluated the antibacterial effect of medlar and hawthorn compound extract in vitro. Water extract method and ethanol extraction method was adopted to prepare the compound extracts, and disc diffusion method and improved test tube doubling dilution method were used to conduct the antibacterial test on the two common pathogenic bacteria, Staphylococcus aureus and Klebsiella pneumonia, in vitro. The results showed that medlar and hawthorn compound extract was moderately sensitive to Staphylococcus aureus, while its inhibiting effect on Klebsiella pneumoniae was particularly significant, moreover, the antibacterial effect of ethanol extract was better than water extract. Medlar and hawthorn compounds had good antibacterial effect on the two pathogenic bacteria.

[Comparison study of different methods for extracting volatile oil from bergamot].

PubMed

Chen, Fei; Li, Qun-li; Sheng, Liu-qing; Qiu, Jiao-ying

2008-08-01

To test different methods for extracting volatile oil from bergamot. The determination of bergapten was carried out by RP-HPLC. Four different ways of organic solvent extraction, steam-input distillation, distillation of the material mixed with water and press extraction were compared. Bergapten wasnt extracted by ways of steam-input distillation and distillation of the material mixed with water. The steam distillation extraction can be taken to extract volatile oil from bergamot for protecting humans' skins.

Steroid hormones in environmental matrices: extraction method comparison.

PubMed

Andaluri, Gangadhar; Suri, Rominder P S; Graham, Kendon

2017-11-09

The U.S. Environmental Protection Agency (EPA) has developed methods for the analysis of steroid hormones in water, soil, sediment, and municipal biosolids by HRGC/HRMS (EPA Method 1698). Following the guidelines provided in US-EPA Method 1698, the extraction methods were validated with reagent water and applied to municipal wastewater, surface water, and municipal biosolids using GC/MS/MS for the analysis of nine most commonly detected steroid hormones. This is the first reported comparison of the separatory funnel extraction (SFE), continuous liquid-liquid extraction (CLLE), and Soxhlet extraction methods developed by the U.S. EPA. Furthermore, a solid phase extraction (SPE) method was also developed in-house for the extraction of steroid hormones from aquatic environmental samples. This study provides valuable information regarding the robustness of the different extraction methods. Statistical analysis of the data showed that SPE-based methods provided better recovery efficiencies and lower variability of the steroid hormones followed by SFE. The analytical methods developed in-house for extraction of biosolids showed a wide recovery range; however, the variability was low (≤ 7% RSD). Soxhlet extraction and CLLE are lengthy procedures and have been shown to provide highly variably recovery efficiencies. The results of this study are guidance for better sample preparation strategies in analytical methods for steroid hormone analysis, and SPE adds to the choice in environmental sample analysis.

Isolation and characterization of coagulant extracted from Moringa oleifera seed by salt solution.

PubMed

Okuda, T; Baes, A U; Nishijima, W; Okada, M

2001-02-01

It is known that M. oleifera contains a natural coagulant in the seeds. In our previous research, the method using salt water to extract the active coagulation component from M. oleifera seeds was developed and compared with the conventional method using water. In this research, the active coagulation component was purified from a NaCl solution crude extract of Moringa oleifera seeds. The active component was isolated and purified from the crude extract through a sequence of steps that included salting-out by dialysis, removal of lipids and carbohydrates by homogenization with acetone, and anion exchange. Specific coagulation activity of the active material increased up to 34 times more than the crude extract after the ion exchange. The active component was not the same as that of water extract. The molecular weight was about 3000 Da. The Lowry method and the phenol-sulfuric acid method indicated that the active component was neither protein nor polysaccharide. The optimum pH of the purified active component for coagulation of turbidity was pH 8 and above. Different from the conventional water extracts, the active component can be used for waters with low turbidity without increase in the dissolved organic carbon concentration.

[Comparison of essential oil enriched with ultrafiltration method and extraction method respectively from essential oil-in-water emulsion of Citri Reticulatae Pericarpium Viride by GC-MS].

PubMed

Yin, Ailing; Han, Zhifeng; Shen, Jie; Guo, Liwei; Cao, Guiping

2011-10-01

To study on the separation from essential oil-in-water emulsion of Citri Reticulatae Pericarpium Viride by ultrafiltration and acetoacetate extraction methods respectively, and the comparison of the oil yields and chemical compositions. Essential oil-in-water emulsion of Citri Reticulatae Pericarpium Viride was separated by ultrafiltration and acetoacetate extraction methods respectively, and the chemical compositions were analyzed and compared by GC-MS. Ultrafiltration method could enrich essential oil more and its chemical compositions were more similar to the essential oil prepared by steam distillation method. Ultrafiltration method is a good medium to separate essential oil from essential oil-in-water emulsion of Citri Reticulatae Pericarpium Viride.

Extraction of antioxidants from Chlorella sp. using subcritical water treatment

NASA Astrophysics Data System (ADS)

Zakaria, S. M.; Mustapa Kamal, S. M.; Harun, M. R.; Omar, R.; Siajam, S. I.

2017-06-01

Chlorella sp. microalgae is one of the main source of natural bioactive compounds used in the food and pharmaceutical industries. Subcritical water extraction is the technique that offers an efficient, non-toxic, and environmental-friendly method to obtain natural ingredients. In this work, the extracts of Chlorella sp. microalgae was evaluated in terms of: chemical composition, extraction (polysaccharides) yield and antioxidant activity, using subcritical water extraction. Extractions were performed at temperatures ranging from 100°C to 300°C. The results show that by using subcritical water, the highest yield of polysaccharides is 23.6 that obtained at 150°C. Analysis on the polysaccharides yield show that the contents were highly influenced by the extraction temperature. The individual antioxidant activity were evaluated by in vitro assay using a free radical method. In general, the antioxidant activity of the extracts obtained at different water temperatures was high, with values of 31.08-54.29 . The results indicated that extraction by subcritical water was effective and Chlorella sp. can be a useful source of natural antioxidants.

Extraction of GBH Film Medicine and Influence on Quality Evaluation of The Film

NASA Astrophysics Data System (ADS)

Ji, Y. B.; Lu, L.; Ru, X.; Guo, S. Z.; Qiao, A. N.; Wang, S. W.

2017-12-01

To know the extraction effects of GBH film medicine and the influence on film quality evaluation. Ultrasonic extraction and reflux extraction were used to extract the two methods with the traditional water decocting method to contrast. They were used to determining the content of total flavonoids. The same method was used to separate the root of the main medicinal herbs and the decoction of the water decoction of the other drug powder. They were used to determine the content of total flavonoids. The effect of extraction method on the preparation of membrane was investigated. The membrane preparation, evaluation and flexibility, respectively, film-forming property, smoothness and disintegration time are used to evaluating separately the effect of extraction method. The results showed that the extraction effect of 70% ethanol concentration of total flavonoids. The best extraction method had no effect on the film quality initial evaluation. This experiment provides a method for membrane extraction agent, has a certain practical significance.

Seasonal distribution of Legionella spp. and L. pneumophila in a river in Taiwan evaluated with culture-confirmed and direct DNA extraction methods

NASA Astrophysics Data System (ADS)

Tung, Min-Che; Chang, Tien-Yu; Hsu, Bing-Mu; Shen, Shu-Min; Huang, Jen-Te; Kao, Po-Min; Chiu, Yi-Chou; Fan, Cheng-Wei; Huang, Yu-Li

2013-07-01

In this study, we evaluated the presence and amount of Legionella in along a river in Taiwan, and the relations between seasonal distribution of Legionella spp. and geographic characteristics in the watershed were also evaluated. Water samples were pre-treated and analyzed with culture-confirmed and direct DNA extraction methods. For culture-confirmed method, water samples were cultivated through a series of selective media, and candidate colonies were confirmed by PCR. For direct DNA extraction method, direct DNA extraction was performed from pre-treated water samples. The DNA extracts were analyzed with PCR and DNA sequence analysis for species determination, quantitative PCR (qPCR) was performed to quantify Legionella concentration in the water sample. In all, 150 water samples were included in this study, with 73 (48.6%) water samples detected with Legionella spp., and 17 with L. pneumophila. Over 80% Legionella spp. detections were through direct DNA extraction method, but more than 80% L. pneumophila detections were through culture-confirmed method. While detection of Legionella spp. was done with two methods, positive results were found through only one method. Legionella spp. was detected in all seasons with detection rate ranging between 34.3-58.8% and seasonal average concentration from 1.9 × 102 to 7.1 × 103 CFU/L. Most of the L. pneumophila detections were from samples collected in fall (38.2%) and summer (6.0%), which also coincided with increased cases of Legionellosis reported through Center of Disease Control in Taiwan. The high prevalence and concentration of Legionella spp. and L. pneumophila in the surface waters should be further evaluated for potential health risks.

Subcritical water extraction of lipids from wet algal biomass

DOEpatents

Deng, Shuguang; Reddy, Harvind K.; Schaub, Tanner; Holguin, Francisco Omar

2016-05-03

Methods of lipid extraction from biomass, in particular wet algae, through conventionally heated subcritical water, and microwave-assisted subcritical water. In one embodiment, fatty acid methyl esters from solids in a polar phase are further extracted to increase biofuel production.

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

PubMed

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values < or =3-25% (n=5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were > or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

Validation of green-solvent extraction combined with chromatographic chemical fingerprint to evaluate quality of Stevia rebaudiana Bertoni.

PubMed

Teo, Chin Chye; Tan, Swee Ngin; Yong, Jean Wan Hong; Hew, Choy Sin; Ong, Eng Shi

2009-02-01

An approach that combined green-solvent methods of extraction with chromatographic chemical fingerprint and pattern recognition tools such as principal component analysis (PCA) was used to evaluate the quality of medicinal plants. Pressurized hot water extraction (PHWE) and microwave-assisted extraction (MAE) were used and their extraction efficiencies to extract two bioactive compounds, namely stevioside (SV) and rebaudioside A (RA), from Stevia rebaudiana Bertoni (SB) under different cultivation conditions were compared. The proposed methods showed that SV and RA could be extracted from SB using pure water under optimized conditions. The extraction efficiency of the methods was observed to be higher or comparable to heating under reflux with water. The method precision (RSD, n = 6) was found to vary from 1.91 to 2.86% for the two different methods on different days. Compared to PHWE, MAE has higher extraction efficiency with shorter extraction time. MAE was also found to extract more chemical constituents and provide distinctive chemical fingerprints for quality control purposes. Thus, a combination of MAE with chromatographic chemical fingerprints and PCA provided a simple and rapid approach for the comparison and classification of medicinal plants from different growth conditions. Hence, the current work highlighted the importance of extraction method in chemical fingerprinting for the classification of medicinal plants from different cultivation conditions with the aid of pattern recognition tools used.

A new method of tree xylem water extraction for isotopic analysis

NASA Astrophysics Data System (ADS)

Gierke, C.; Newton, B. T.

2011-12-01

The Sacramento Mountain Watershed Study in the southern Sacramento Mountains of New Mexico is designed to assess the forest restoration technique of tree thinning in mountain watersheds as an effective method of increasing local and regional groundwater recharge. The project is using a soil water balance approach to quantify the partitioning of local precipitation within this watershed before and after thinning trees. Understanding what sources trees extract their water from (e.g. shallow groundwater, unsaturated fractured bedrock, and soils) is difficult due to a complex hydrologic system and heterogeneous distribution of soil thicknesses. However, in order to accurately quantify the soil water balance and to assess how thinning trees will affect this water balance, it is important determine the sources from which trees extract their water. We plan to use oxygen and hydrogen stable isotopic analysis of various end member waters to identify these different sources. We are in the process of developing a new method of determining the isotopic composition of tree water that has several advantages over conventional methods. Within the tree there is the xylem which transports water from the roots to the leaves and the phloem which transports starches and sugars in a water media throughout the tree. Previous studies have shown that the isotopic composition of xylem water accurately reflects that of source water, while phloem water has undergone isotopic fractionation during photosynthesis and metabolism. The distillation of water from twigs, which is often used to extract tree water for isotopic analysis, is very labor intensive. Other disadvantages to distillation methods include possible fractionation due to phase changes and the possible extraction of fractionated phloem waters. Employing a new mixing method, the composition of the twig water (TW) can be determined by putting twigs of unknown isotopic water composition into waters of known compositions or initial waters (IW), allowing diffusive processes to proceed to equilibrium, measuring the composition of the resulting mixture or final water (FW) then, solving a simple mixing equation. To evaluate this method, we collected several twig samples from Douglas Firs in the Sacramento Mountains. Twig water was prepared for isotopic analysis both by cryogenic distillation and the mixing method. Soil in close proximity to these trees was also sampled and water was extracted by cryogenic distillation. Preliminary results show that the isotopic composition of distilled twig water and soil waters plot to the right of the local meteoric water line (LMWL) suggesting that trees are extracting shallow evaporated soil water. Twig water obtained from the mixing method plot near the LMWL within the range expected for local snow melt, suggesting a possibly deeper non-evaporated source. In general, distillation values are approximately 4% heavier with respect to delta 18O than waters obtained from the mixing method. It is possible that this difference is due to the contribution of the fractionated water of the twig phloem that is released during the distillation process. This difference is quite significant and can lead to very different interpretations. These results are being addressed with additional experiments.

Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection.

PubMed

Guo, Yuanming; Hu, Hongmei; Li, Tiejun; Xue, Lijian; Zhang, Xiaoning; Zhong, Zhi; Zhang, Yurong; Jin, Yanjian

2017-08-01

A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1:1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 μg/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed method was compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Triaxial- and uniaxial-compression testing methods developed for extraction of pore water from unsaturated tuff, Yucca Mountain, Nevada

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

Mower, T.E.; Higgins, J.D.; Yang, I.C.

1989-12-31

To support the study of hydrologic system in the unsaturated zone at Yucca Mountain, Nevada, two extraction methods were examined to obtain representative, uncontaminated pore-water samples from unsaturated tuff. Results indicate that triaxial compression, which uses a standard cell, can remove pore water from nonwelded tuff that has an initial moisture content greater than 11% by weight; uniaxial compression, which uses a specifically fabricated cell, can extract pore water from nonwelded tuff that has an initial moisture content greater than 8% and from welded tuff that has an initial moisture content greater than 6.5%. For the ambient moisture conditions ofmore » Yucca Mountain tuffs, uniaxial compression is the most efficient method of pore-water extraction. 12 refs., 7 figs., 2 tabs.« less

Determination of Low Concentrations of Acetochlor in Water by Automated Solid-Phase Extraction and Gas Chromatography with Mass-Selective Detection

USGS Publications Warehouse

Lindley, C.E.; Stewart, J.T.; Sandstrom, M.W.

1996-01-01

A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 ??g/L. Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 ??g/L. Average single-operator precision, over the course of 1 week, was better than 5%.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by Carbopak-B solid-phase extraction and high-preformance liquid chromatography

USGS Publications Warehouse

Werner, Stephen L.; Burkhardt, Mark R.; DeRusseau, Sabrina N.

1996-01-01

In accordance with the needs of the National Water-Quality Assessment Program (NAWQA), the U.S. Geological Survey has developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method. The method is used to determine 41 pesticides and pesticide metabolites that are not readily amenable to gas chromatography or other high-temperature analytical techniques. Pesticides are extracted from filtered environmental water samples using a 0.5-gram graphitized carbon-based solid-phase cartridge, eluted from the cartridge into two analytical fractions, and analyzed using high-performance liquid chromatography with photodiode-array detection. The upper concentration limit is 1.6 micrograms per liter (=B5g/L) for most compounds. Single-operator method detection limits in organic-free water samples ranged from 0.006 to 0.032 =B5g/L= Recoveries in organic-free water samples ranged from 37 to 88 percent. Recoveries in ground- and surface-water samples ranged from 29 to 94 percent. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time of 7 days.

a Framework of Change Detection Based on Combined Morphologica Features and Multi-Index Classification

NASA Astrophysics Data System (ADS)

Li, S.; Zhang, S.; Yang, D.

2017-09-01

Remote sensing images are particularly well suited for analysis of land cover change. In this paper, we present a new framework for detection of changing land cover using satellite imagery. Morphological features and a multi-index are used to extract typical objects from the imagery, including vegetation, water, bare land, buildings, and roads. Our method, based on connected domains, is different from traditional methods; it uses image segmentation to extract morphological features, while the enhanced vegetation index (EVI), the differential water index (NDWI) are used to extract vegetation and water, and a fragmentation index is used to the correct extraction results of water. HSV transformation and threshold segmentation extract and remove the effects of shadows on extraction results. Change detection is performed on these results. One of the advantages of the proposed framework is that semantic information is extracted automatically using low-level morphological features and indexes. Another advantage is that the proposed method detects specific types of change without any training samples. A test on ZY-3 images demonstrates that our framework has a promising capability to detect change.

Effects of extraction methods on the antioxidant activities of polysaccharides from Agaricus blazei Murrill.

PubMed

Jia, Shaoyi; Li, Feng; Liu, Yong; Ren, Haitao; Gong, Guili; Wang, Yanyan; Wu, Songhai

2013-11-01

Five polysaccharides were obtained from Agaricus blazei Murrill (ABM) through different extraction methods including hot water extraction, single enzyme extraction (pectinase, cellulase or papain) and compound enzymes extraction (cellulase:pectinase:papain). Their characteristics such as the polysaccharide yield, polysaccharide content, protein content, infrared spectra were determined, and antioxidant activities were investigated on the basis of hydroxyl radical, DPPH free radical, ABTS free radical and reducing power. The results showed that five extracts exhibited antioxidant activities in a concentration-dependent manner. Compared with other methods, the compound enzymes extraction method was found to present the highest polysaccharides yield (17.44%). Moreover, compound enzymes extracts exhibited the strongest reducing power and highest scavenging rates on hydroxyl radicals, DPPH radicals and ABTS radicals. On the contrary, hot water extraction method had the lowest polysaccharides yield of 11.95%, whose extracts also exhibited the lowest antioxidant activities. Overall, the available data obtained in vitro models suggested that ABM extracts were natural antioxidants and compound enzymes extraction was an appropriate, mild and effective extracting method for obtaining the polysaccharide extracts from Agaricus blazei Murrill (ABM). Copyright © 2013 Elsevier B.V. All rights reserved.

Development of a dispersive liquid-liquid microextraction method using a lighter-than-water ionic liquid for the analysis of polycyclic aromatic hydrocarbons in water.

PubMed

Medina, Giselle S; Reta, Mario

2016-11-01

A dispersive liquid-liquid microextraction method using a lighter-than-water phosphonium-based ionic liquid for the extraction of 16 polycyclic aromatic hydrocarbons from water samples has been developed. The extracted compounds were analyzed by liquid chromatography coupled to fluorescence/diode array detectors. The effects of several experimental parameters on the extraction efficiency, such as type and volume of ionic liquid and disperser solvent, type and concentration of salt in the aqueous phase and extraction time, were investigated and optimized. Three phosphonium-based ionic liquids were assayed, obtaining larger extraction efficiencies when trihexyl-(tetradecyl)phosphonium bromide was used. The optimized methodology requires a few microliters of a lighter-than-water phosphonium-based ionic liquid, which allows an easy separation of the extraction solvent phase. The obtained limits of detection were between 0.02 and 0.56 μg/L, enrichment factors between 109 and 228, recoveries between 60 and 108%, trueness between 0.4 and 9.9% and reproducibility values between 3 and 12% were obtained. These figures of merit combined with the simplicity, rapidity and low cost of the analytical methodology indicate that this is a viable and convenient alternative to the methods reported in the literature. The developed method was used to analyze polycyclic aromatic hydrocarbons in river water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

SIMPLE METHOD FOR ESTIMATING POLYCHLORINATED BIPHENYL CONCENTRATIONS ON SOILS AND SEDIMENTS USING SUBCRITICAL WATER EXTRACTION COUPLED WITH SOLID-PHASE MICROEXTRACTION. (R825368)

EPA Science Inventory

A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a seale...

Investigation of Polyhenolic Content of Rose Hip (Rosa canina L.) Tea Extracts: A Comparative Study

PubMed Central

İlbay, Zeynep; Şahin, Selin; Kırbaşlar, Ş. İsmail

2013-01-01

Three different brands of Rose hip (Rosa canina L.) tea were extracted with water, ethanol (EtOH), methanol (MeOH), and aqueous mixtures (50%, v/v) by ultrasound-assisted extraction (UAE) and Soxhlet methods. Total phenolic content was determined according to the Folin-Ciocalteu method. The results were presented by means of the extract yields and total phenolic contents, expressed in gallic acid equivalent (GAE) per g of dried matter (DM). The greatest amount of extract observed in tea samples was obtained by UAE through water with the value of 619.37 ± 0.58 mg/g DM. Regarding the phenolic content, the best result was achieved by the Soxhlet method through 50% MeOH mixture (59.69 ± 0.89 mg GAE/g DM), followed by the UAE method with water (48.59 ± 0.29 mg GAE/g DM). PMID:28239095

Method development for the analysis of N-nitrosodimethylamine and other N-nitrosamines in drinking water at low nanogram/liter concentrations using solid-phase extraction and gas chromatography with chemical ionization tandem mass spectrometry.

PubMed

Munch, Jean W; Bassett, Margarita V

2006-01-01

N-nitrosodimethylamine (NDMA) is a probable human carcinogen of concern that has been identified as a drinking water contaminant. U.S. Environmental Protection Agency Method 521 has been developed for the analysis of NDMA and 6 additional N-nitrosamines in drinking water at low ng/L concentrations. The method uses solid-phase extraction with coconut charcoal as the sorbent and dichloromethane as the eluent to concentrate 0.50 L water samples to 1 mL. The extracts are analyzed by gas chromatography-chemical ionization tandem mass spectrometry using large-volume injection. Method performance was evaluated in 2 laboratories. Typical analyte recoveries of 87-104% were demonstrated for fortified reagent water samples, and recoveries of 77-106% were demonstrated for fortified drinking water samples. All relative standard deviations on replicate analyses were < 11%.

Extraction of chemical warfare agents from water with hydrophilic-lipophilic balance and C18 cartridges: comparative study.

PubMed

Kanaujia, Pankaj K; Pardasani, Deepak; Gupta, A K; Dubey, D K

2007-01-19

Efficient extraction of chemical warfare agents (CWAs) from water is essential before subjecting them to gas chromatographic and spectral analysis aiming towards verification of the Chemical Weapons Convention (CWC). It requires development of fast, reliable, simple and reproducible sample preparation of CWAs from water which is likely to be contaminated during deliberate or inadvertent spread of CWAs. This work describes development of a solid-phase extraction method using hydrophilic-lipophilic balance (HLB) cartridges for extraction of CWAs from water. The extraction efficiencies of HLB and C18 cartridges were compared and the results revealed that HLB sorbents performed better. Extracts were analyzed by gas chromatography-mass spectrometry. Extraction parameters, such as extraction solvent, its volume and rinsing solvent were optimized. Best recoveries of target analytes were obtained using 1mL methanol and limits of detection were achieved up to 0.05microg/mL with dichloromethane. Precision of the method was found to be less than 9.2% RSD.

Study of the Effect of Surfactants on Extraction and Determination of Polyphenolic Compounds and Antioxidant Capacity of Fruits Extracts

PubMed Central

Hosseinzadeh, Reza; Khorsandi, Khatereh; Hemmaty, Syavash

2013-01-01

Micelle/water mixed solutions of different surface active agents were studied for their effectiveness in the extraction of polyphenolic compounds from various varieties of apples from west Azerbaijan province in Iran. The total content of polyphenolic compound in fruit extracts were determined using ferrous tartrate and Folin–Ciocalteu assays methods and chromatographic methods and compared with theme. High performance liquid chromatography is one of the most common and important methods in biochemical compound identification. The effect of pH, ionic strength, surfactant type, surfactant concentration, extraction time and common organic solvent in the apple polyphenolics extractions was studied using HPLC-DAD. Mixtures of surfactants, water and methanol at various ratios were examined and micellar-water solutions of Brij surfactant showed the highest polyphenol extraction efficiency. Optimum conditions for the extraction of polyphenolic compounds from apple occurred at 7 mM Brij35, pH 3. Effect of ionic strength on extraction was determined and 2% (W/V) potassium Chloride was determined to be the optimum salt concentration. The procedure worked well with an ultrasound bath. Total antioxidant capacity also was determined in this study. The method can be safely scaled up for pharmaceutical applications. PMID:23472082

Microwave-assisted extraction of lipid from fish waste

NASA Astrophysics Data System (ADS)

Rahimi, M. A.; Omar, R.; Ethaib, S.; Siti Mazlina, M. K.; Awang Biak, D. R.; Nor Aisyah, R.

2017-06-01

Processing fish waste for extraction of value added products such as protein, lipid, gelatin, amino acids, collagen and oil has become one of the most intriguing researches due to its valuable properties. In this study the extraction of lipid from sardine fish waste was carried out using microwave-assisted extraction (MAE) and compared with Soxhlets and Hara and Radin methods. A mixture of two organic solvents isopropanol/hexane and distilled water were used for MAE and Hara and Radin methods. Meanwhile, Soxhlet method utilized only hexane as solvent. The results show that the higher yield of lipid 80.5 mg/g was achieved using distilled water in MAE method at 10 min extraction time. Soxhlet extraction method only produced 46.6 mg/g of lipid after 4 hours of extraction time. Lowest yield of lipid was found at 15.8 mg/g using Hara and Radin method. Based on aforementioned results, it can be concluded MAE method is superior compared to the Soxhlet and Hara and Radin methods which make it an attractive route to extract lipid from fish waste.

Methods of Analysis - Determination of Pyrethroid Insecticides in Water and Sediment Using Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Hladik, Michelle; Smalling, Kelly L.; Kuivila, Kathryn

2009-01-01

A method for the determination of 14 pyrethroid insecticides in environmental water and sediment samples is described. The method was developed by the U.S. Geological Survey in response to increasing concern over the effects of pyrethroids on aquatic organisms. The pyrethroids included in this method are ones that are applied to many agricultural and urban areas. Filtered water samples are extracted for pyrethroids using solid-phase extraction (SPE) with no additional cleanup steps. Sediment and soil samples are extracted using a microwave-assisted extraction system, and the pyrethroids of interest are separated from co-extracted matrix interferences by passing the extracts through stacked graphitized carbon and alumina SPE cartridges, along with the use of high-performance liquid chromatography and gel-permeation chromatography (HPLC/GPC). Quantification of the pyrethroids from the extracted water and sediment samples is done using gas chromatography with mass spectrometry (GC/MS) or gas chromatography with tandem mass spectrometry (GC/MS/MS). Recoveries in test water samples fortified at 10 ng/L ranged from 83 to 107 percent, and recoveries in test sediment samples fortified at 10 ug/kg ranged from 82 to 101 percent; relative standard deviations ranged from 5 to 9 percent in the water samples and 3 to 9 percent in the sediment samples. Method detection limits (MDLs), calculated using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), in water ranged from 2.0 to 6.0 ng/L using GC/MS and 0.5 to 1.0 ng/L using GC/MS/MS. For sediment, the MDLs ranged from 1.0 to 2.6 ug/kg dry weight using GC/MS and 0.2 to 0.5 ug/kg dry weight using GC/MS/MS. The matrix-spike recoveries for each compound, when averaged for 12 environmental water samples, ranged from 84 to 96 percent, and when averaged for 27 environmental sediment samples, ranged from 88 to 100 percent.

Microwave-assisted extraction with water for fast extraction and simultaneous RP-HPLC determination of phenolic acids in radix Salviae Miltiorrhizae.

PubMed

Fang, Xinsheng; Wang, Jianhua; Zhou, Hongying; Jiang, Xingkai; Zhu, Lixiang; Gao, Xin

2009-07-01

An optimized microwave-assisted extraction method using water (MAE-W) as the extractant and an efficient HPLC analysis method were first developed for the fast extraction and simultaneous determination of D(+)-(3,4-dihydroxyphenyl) lactic acid (Dla), salvianolic acid B (SaB), and lithospermic acid (La) in radix Salviae Miltiorrhizae. The key parameters of MAE-W were optimized. It was found that the degradation of SaB was inhibited when using the optimized MAE-W and the stable content of Dla, La, and SaB in danshen was obtained. Furthermore, compared to the conventional extraction methods, the proposed MAE-W is a more rapid method with higher yield and lower solvent consumption with a reproducibility (RSD <6%). In addition, using water as extractant is safe and helpful for environment protection, which could be referred to as green extraction. The separation and quantitative determination of the three compounds was carried out by a developed reverse-phase high-performance liquid chromatographic (RP-HPLC) method with UV detection. Highly efficient separation was obtained using gradient solvent system. The optimized HPLC analysis method was validated to have specificity, linearity, precision, and accuracy. The results indicated that MAE-W followed by HPLC-UV determination is an appropriate alternative to previously proposed method for quality control of radix Salviae Miltiorrhizae.

Pore-water extraction from unsaturated tuff by triaxial and one-dimensional compression methods, Nevada Test Site, Nevada

USGS Publications Warehouse

Mower, Timothy E.; Higgins, Jerry D.; Yang, In C.; Peters, Charles A.

1994-01-01

Study of the hydrologic system at Yucca Mountain, Nevada, requires the extraction of pore-water samples from welded and nonwelded, unsaturated tuffs. Two compression methods (triaxial compression and one-dimensional compression) were examined to develop a repeatable extraction technique and to investigate the effects of the extraction method on the original pore-fluid composition. A commercially available triaxial cell was modified to collect pore water expelled from tuff cores. The triaxial cell applied a maximum axial stress of 193 MPa and a maximum confining stress of 68 MPa. Results obtained from triaxial compression testing indicated that pore-water samples could be obtained from nonwelded tuff cores that had initial moisture contents as small as 13 percent (by weight of dry soil). Injection of nitrogen gas while the test core was held at the maximum axial stress caused expulsion of additional pore water and reduced the required initial moisture content from 13 to 11 percent. Experimental calculations, together with experience gained from testing moderately welded tuff cores, indicated that the triaxial cell used in this study could not apply adequate axial or confining stress to expel pore water from cores of densely welded tuffs. This concern led to the design, fabrication, and testing of a one-dimensional compression cell. The one-dimensional compression cell used in this study was constructed from hardened 4340-alloy and nickel-alloy steels and could apply a maximum axial stress of 552 MPa. The major components of the device include a corpus ring and sample sleeve to confine the sample, a piston and base platen to apply axial load, and drainage plates to transmit expelled water from the test core out of the cell. One-dimensional compression extracted pore water from nonwelded tuff cores that had initial moisture contents as small as 7.6 percent; pore water was expelled from densely welded tuff cores that had initial moisture contents as small as 7.7 percent. Injection of nitrogen gas at the maximum axial stress did not produce additional pore water from nonwelded tuff cores, but was critical to recovery of pore water from densely welded tuff cores. Gas injection reduced the required initial moisture content in welded tuff cores from 7.7 to 6.5 percent. Based on the mechanical ability of a pore-water extraction method to remove water from welded and nonwelded tuff cores, one-dimensional compression is a more effective extraction method than triaxial compression. However, because the effects that one-dimensional compression has on pore-water chemistry are not completely understood, additional testing will be needed to verify that this method is suitable for pore-water extraction from Yucca Mountain tuffs.

Anti-fungal activity of cold and hot water extracts of spices against fungal pathogens of Roselle (Hibiscus sabdariffa) in vitro.

PubMed

Touba, Eslaminejad Parizi; Zakaria, Maziah; Tahereh, Eslaminejad

2012-02-01

Crude extracts of seven spices, viz. cardamom, chilli, coriander, onion, garlic, ginger, and galangale were made using cold water and hot water extraction and they were tested for their anti-fungal effects against the three Roselle pathogens i.e. Phoma exigua, Fusarium nygamai and Rhizoctonia solani using the 'poisoned food technique'. All seven spices studied showed significant anti-fungal activity at three concentrations (10, 20 and 30% of the crude extract) in-vitro. The cold water extract of garlic exhibited good anti-fungal activity against all three tested fungi. In the case of the hot water extracts, garlic and ginger showed the best anti-fungal activity. Of the two extraction methods, cold water extraction was generally more effective than hot water extraction in controlling the pathogens. Against P. exigua, the 10% cold water extracts of galangale, ginger, coriander and cardamom achieved total (100%) inhibition of pathogen mycelial growth. Total inhibition of F. nygamai mycelial growth was similarly achieved with the 10% cold water extracts garlic. Against R. solani, the 10% cold water extract of galangale was effective in imposing 100% inhibition. Accordingly, the 10% galangale extract effectively controlled both P. exigua and R. solani in vitro. None of the hot water extracts of the spices succeeded in achieving 100% inhibition of the pathogen mycelial growth. Copyright © 2011 Elsevier Ltd. All rights reserved.

High-throughput immunomagnetic scavenging technique for quantitative analysis of live VX nerve agent in water, hamburger, and soil matrixes.

PubMed

Knaack, Jennifer S; Zhou, Yingtao; Abney, Carter W; Prezioso, Samantha M; Magnuson, Matthew; Evans, Ronald; Jakubowski, Edward M; Hardy, Katelyn; Johnson, Rudolph C

2012-11-20

We have developed a novel immunomagnetic scavenging technique for extracting cholinesterase inhibitors from aqueous matrixes using biological targeting and antibody-based extraction. The technique was characterized using the organophosphorus nerve agent VX. The limit of detection for VX in high-performance liquid chromatography (HPLC)-grade water, defined as the lowest calibrator concentration, was 25 pg/mL in a small, 500 μL sample. The method was characterized over the course of 22 sample sets containing calibrators, blanks, and quality control samples. Method precision, expressed as the mean relative standard deviation, was less than 9.2% for all calibrators. Quality control sample accuracy was 102% and 100% of the mean for VX spiked into HPLC-grade water at concentrations of 2.0 and 0.25 ng/mL, respectively. This method successfully was applied to aqueous extracts from soil, hamburger, and finished tap water spiked with VX. Recovery was 65%, 81%, and 100% from these matrixes, respectively. Biologically based extractions of organophosphorus compounds represent a new technique for sample extraction that provides an increase in extraction specificity and sensitivity.

Extraction of trace tilmicosin in real water samples using ionic liquid-based aqueous two-phase systems.

PubMed

Pan, Ru; Shao, Dejia; Qi, Xueyong; Wu, Yun; Fu, Wenyan; Ge, Yanru; Fu, Haizhen

2013-01-01

The effective method of ionic liquid-based aqueous two-phase extraction, which involves ionic liquid (IL) (1-butyl-3-methyllimidazolium chloride, [C4mim]Cl) and inorganic salt (K2HPO4) coupled with high-performance liquid chromatography (HPLC), has been used to extract trace tilmicosin in real water samples which were passed through a 0.45 μm filter. The effects of the different types of salts, the concentration of K2HPO4 and of ILs, the pH value and temperature of the systems on the extraction efficiencies have all been investigated. Under the optimum conditions, the average extraction efficiency is up to 95.8%. This method was feasible when applied to the analysis of tilmicosin in real water samples within the range 0.5-40 μg mL(-1). The limit of detection was found to be 0.05 μg mL(-1). The recovery rate of tilmicosin was 92.0-99.0% from the real water samples by the proposed method. This process is suggested to have important applications for the extraction of tilmicosin.

Method for separating water soluble organics from a process stream by aqueous biphasic extraction

DOEpatents

Chaiko, David J.; Mego, William A.

1999-01-01

A method for separating water-miscible organic species from a process stream by aqueous biphasic extraction is provided. An aqueous biphase system is generated by contacting a process stream comprised of water, salt, and organic species with an aqueous polymer solution. The organic species transfer from the salt-rich phase to the polymer-rich phase, and the phases are separated. Next, the polymer is recovered from the loaded polymer phase by selectively extracting the polymer into an organic phase at an elevated temperature, while the organic species remain in a substantially salt-free aqueous solution. Alternatively, the polymer is recovered from the loaded polymer by a temperature induced phase separation (cloud point extraction), whereby the polymer and the organic species separate into two distinct solutions. The method for separating water-miscible organic species is applicable to the treatment of industrial wastewater streams, including the extraction and recovery of complexed metal ions from salt solutions, organic contaminants from mineral processing streams, and colorants from spent dye baths.

EPA Method 525.3 - Determination of Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS)

EPA Science Inventory

Method 525.3 is an analytical method that uses solid phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) for the identification and quantitation of 125 selected semi-volatile organic chemicals in drinking water.

Stir bar sorptive extraction and liquid chromatography-tandem mass spectrometry determination of polar and non-polar emerging and priority pollutants in environmental waters.

PubMed

Aparicio, Irene; Martín, Julia; Santos, Juan Luis; Malvar, José Luis; Alonso, Esteban

2017-06-02

An analytical method based on stir bar sorptive extraction (SBSE) was developed and validated for the determination of environmental concern pollutants in environmental waters by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Target compounds include six water and oil repellents (perfluorinated compounds), four preservatives (butylated hydroxytoluene and three parabens), two plasticizers (bisphenol A and di(2-ethylhexyl)phthalate), seven surfactants (four linear alkylbenzene sulfonates, nonylphenol and two nonylphenol ethoxylates), a flame retardant (hexabromocyclododecane), four hormones, fourteen pharmaceutical compounds, an UV-filter (2-ethylhexyl 4-methoxycinnamate) and nine pesticides. To achieve the simultaneous extraction of polar and non-polar pollutants two stir bar coatings were tested, the classic polydimethylsiloxane (PDMS) coating and the novel ethylene glycol modified silicone (EG-silicone). The best extraction recoveries were obtained using EG-silicone coating. The effects of sample pH, volume and ionic strength and extraction time on extraction recoveries were evaluated. The analytical method was validated for surface water and tap water samples. The method quantification limits ranged from 7.0ngL -1 to 177ngL -1 . The inter-day precision, expressed as relative standard deviation, was lower than 20%. Accuracy, expressed as relative recovery values, was in the range from 61 to 130%. The method was applied for the determination of the 48 target compounds in surface and tap water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

[Study on extraction of the total saponins of Chinese yam].

PubMed

Zhang, Min; Du, Lin; Huang, Gui-dong; Zhong, Xian-feng

2007-07-01

A method for the determination of total saponins of Chinese yam was established. The dioscin was used as a standard compound, the vanillin-perchloric acid as chromogenic agent and glacial acetic acid as solvent. The extraction technique of asponins from Chinese yam was studied by spectrometric method. Extracting temperature, extracting time, ethanol concentration and the ratio of raw material and water were selected as four factors to design the orthogonal test, and the optical condition of extraction was obtained. The results showed that the optical condition of extraction was as following: extracting temperature 60 degrees C, extracting time 6 h, ethanol concetration 80%, and the ratio of raw material and water 1:8.

AN ALTERNATIVE ELUENT TO BEEF EXTRACT FOR ELUTING POLIOVIRUS FROM ELECTROPOSITIVE FILTERS

EPA Science Inventory

Traditional methods for enteric virus removal from waters involve filtering the water through a positively charged filter followed by elution with beef extract, second step concentration by flocculation, and assay in cell culture. Two of the problems associated with this method ...

Method for extracting metals from aqueous waste streams for long term storage

DOEpatents

Chaiko, D.J.

1995-03-07

A liquid-liquid extraction method for removing metals and hydrous metal colloids from waste streams is provided wherein said waste streams are contacted with a solvent system containing a water-in-oil microemulsion wherein the inverted micelles contain the extracted metal. A silicon alkoxide, either alone or in combination with other metal alkoxide compounds is added to the water-in-oil microemulsion, thereby allowing encapsulation of the extracted metal within a silicon oxide network. Lastly, the now-encapsulated metal is precipitated from the water-in-oil microemulsion phase to yield aggregates of metal-silicate particles having average individual particle sizes of approximately 40 nanometers. 2 figs.

Method for extracting metals from aqueous waste streams for long term storage

DOEpatents

Chaiko, D.J.

1993-01-01

A liquid-liquid extraction method for removing metals and hydrous metal colloids from waste streams is provided wherein said waste streams are contacted with a solvent system containing a water-in-oil microemulsion wherein the inverted micelles contain the extracted metal. A silicon alkoxide, either alone or in combination with other metal alkoxide compounds is added to the water-in-oil microemulsion, thereby allowing encapsulation of the extracted metal within a silicon oxide network. Lastly, the now-encapsulated metal is precipitated from the water-in-oil microemulsion phase to yield aggregates of metal-silicate particles having average. individual particle sizes of approximately 40 manometers.

Method for extracting metals from aqueous waste streams for long term storage

DOEpatents

Chaiko, David J.

1995-01-01

A liquid--liquid extraction method for removing metals and hydrous metal colloids from waste streams is provided wherein said waste streams are contacted with a solvent system containing a water-in-oil microemulsion wherein the inverted micelles contain the extracted metal. A silicon alkoxide, either alone or in combination with other metal alkoxide compounds is added to the water-in-oil microemulsion, thereby allowing encapsulation of the extracted metal within a silicon oxide network. Lastly, the now-encapsulated metal is precipitated from the water-in-oil microemulsion phase to yield aggregates of metal-silicate particles having average individual particle sizes of approximately 40 nanometers.

The high-performance liquid chromatography/multistage electrospray mass spectrometric investigation and extraction optimization of beech (Fagus sylvatica L.) bark polyphenols.

PubMed

Hofmann, Tamás; Nebehaj, Esztella; Albert, Levente

2015-05-08

The aim of the present work was the high-performance liquid chromatographic separation and multistage mass spectrometric characterization of the polyphenolic compounds of beech bark, as well as the extraction optimization of the identified compounds. Beech is a common and widely used material in the wood industry, yet its bark is regarded as a by-product. Using appropriate extraction methods these compounds could be extracted and utilized in the future. Different extraction methods (stirring, sonication, microwave assisted extraction) using different solvents (water, methanol:water 80:20 v/v, ethanol:water 80:20 v/v) and time/temperature schedules have been compared basing on total phenol contents (Folin-Ciocâlteu) and MRM peak areas of the identified compounds to investigate optimum extraction efficiency. Altogether 37 compounds, including (+)-catechin, (-)-epicatechin, quercetin-O-hexoside, taxifolin-O-hexosides (3), taxifolin-O-pentosides (4), B-type (6) and C-type (6) procyanidins, syringic acid- and coumaric acid-di-O-glycosides, coniferyl alcohol- and sinapyl alcohol-glycosides, as well as other unknown compounds with defined [M-H](-) m/z values and MS/MS spectra have been tentatively identified. The choice of the method, solvent system and time/temperature parameters favors the extraction of different types of compounds. Pure water can extract compounds as efficiently as mixtures containing organic solvents under high-pressure and high temperature conditions. This supports the implementation of green extraction methods in the future. Extraction times that are too long and high temperatures can result in the decrease of the concentrations. Future investigations will focus on the evaluation of the antioxidant capacity and utilization possibilities of the prepared extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

1992-01-01

A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

USGS Publications Warehouse

Steinheimer, T.R.; Brooks, M.G.

1984-01-01

A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

Development of an extraction method for perchlorate in soils.

PubMed

Cañas, Jaclyn E; Patel, Rashila; Tian, Kang; Anderson, Todd A

2006-03-01

Perchlorate originates as a contaminant in the environment from its use in solid rocket fuels and munitions. The current US EPA methods for perchlorate determination via ion chromatography using conductivity detection do not include recommendations for the extraction of perchlorate from soil. This study evaluated and identified appropriate conditions for the extraction of perchlorate from clay loam, loamy sand, and sandy soils. Based on the results of this evaluation, soils should be extracted in a dry, ground (mortar and pestle) state with Milli-Q water in a 1 ratio 1 soil ratio water ratio and diluted no more than 5-fold before analysis. When sandy soils were extracted in this manner, the calculated method detection limit was 3.5 microg kg(-1). The findings of this study have aided in the establishment of a standardized extraction method for perchlorate in soil.

Method development for the analysis of 1,4-dioxane in drinking water using solid-phase extraction and gas chromatography-mass spectrometry.

PubMed

Grimmett, Paul E; Munch, Jean W

2009-01-01

1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The United States Environmental Protection Agency's (U.S. EPA) National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of an activated carbon solid-phase extraction of 500-mL or 100-mL water samples using dichloromethane as the elution solvent. The extracts are analyzed by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. In the NERL laboratory, recovery of 1,4-dioxane ranged from 94-110% in fortified laboratory reagent water and recoveries of 96-102% were demonstrated for fortified drinking water samples. The relative standard deviations for replicate analyses were less than 6% at concentrations exceeding the minimum reporting level.

Antioxidant and antimicrobial activities of bitter and sweet apricot (Prunus armeniaca L.) kernels.

PubMed

Yiğit, D; Yiğit, N; Mavi, A

2009-04-01

The present study describes the in vitro antimicrobial and antioxidant activity of methanol and water extracts of sweet and bitter apricot (Prunus armeniaca L.) kernels. The antioxidant properties of apricot kernels were evaluated by determining radical scavenging power, lipid peroxidation inhibition activity and total phenol content measured with a DPPH test, the thiocyanate method and the Folin method, respectively. In contrast to extracts of the bitter kernels, both the water and methanol extracts of sweet kernels have antioxidant potential. The highest percent inhibition of lipid peroxidation (69%) and total phenolic content (7.9 +/- 0.2 microg/mL) were detected in the methanol extract of sweet kernels (Hasanbey) and in the water extract of the same cultivar, respectively. The antimicrobial activities of the above extracts were also tested against human pathogenic microorganisms using a disc-diffusion method, and the minimal inhibitory concentration (MIC) values of each active extract were determined. The most effective antibacterial activity was observed in the methanol and water extracts of bitter kernels and in the methanol extract of sweet kernels against the Gram-positive bacteria Staphylococcus aureus. Additionally, the methanol extracts of the bitter kernels were very potent against the Gram-negative bacteria Escherichia coli (0.312 mg/mL MIC value). Significant anti-candida activity was also observed with the methanol extract of bitter apricot kernels against Candida albicans, consisting of a 14 mm in diameter of inhibition zone and a 0.625 mg/mL MIC value.

Identification and characterization of hydrocolloid from Cordia myxa leaf.

PubMed

Samavati, Vahid; Lorestani, Mohammad; Joolazadeh, Sajjad

2014-04-01

Hot water extraction technique was employed to extract the hydrocolloid from Cordia myxa leaf (PCM). The optimal conditions for extraction of PCM were determined using response surface methodology. A Box-Behnken design (BBD) was applied to evaluate the effects of three independent variables (extraction time (X1: 1-4 h), extraction temperature (X2: 55-95 °C), and water to raw material ratio (X3: 5-30 ml/g) on the extraction yield of PCM. The content of moisture, water-soluble and water-insoluble ash, crude protein and total phenol were determined in the extracted hydrocolloid by standard methods. The maximum hydrocolloid extraction yield (9.501±0.15%) was achieved by using extraction time of 4.94 h, extraction temperature of 94.91 °C and water to raw material ratio of 21.74 ml/g. The contents of moisture, crude protein, water-soluble and water-insoluble ash and total phenol were 21.63±0.94%, 14.27±0.55%, 3.07±0.16% and 2.61±0.19 mg galic acid/g, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Simplified multiple headspace extraction gas chromatographic technique for determination of monomer solubility in water.

PubMed

Chai, X S; Schork, F J; DeCinque, Anthony

2005-04-08

This paper reports an improved headspace gas chromatographic (GC) technique for determination of monomer solubilities in water. The method is based on a multiple headspace extraction GC technique developed previously [X.S. Chai, Q.X. Hou, F.J. Schork, J. Appl. Polym. Sci., in press], but with the major modification in the method calibration technique. As a result, only a few iterations of headspace extraction and GC measurement are required, which avoids the "exhaustive" headspace extraction, and thus the experimental time for each analysis. For highly insoluble monomers, effort must be made to minimize adsorption in the headspace sampling channel, transportation conduit and capillary column by using higher operating temperature and a short capillary column in the headspace sampler and GC system. For highly water soluble monomers, a new calibration method is proposed. The combinations of these technique modifications results in a method that is simple, rapid and automated. While the current focus of the authors is on the determination of monomer solubility in aqueous solutions, the method should be applicable to determination of solubility of any organic in water.

Determination of pyrazole and pyrrole pesticides in environmental water samples by solid-phase extraction using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography.

PubMed

Ma, Jiping; Lu, Xi; Xia, Yan; Yan, Fengli

2015-02-01

A solid-phase extraction (SPE) method using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography was developed for the determination of four pyrazole and pyrrole pesticides (fenpyroximate, chlorfenapyr, fipronil and flusilazole) in environmental water samples. Several parameters, such as extraction adsorbent, elution solvent and volume and sample loading flow rate were optimized to obtain high SPE recoveries and extraction efficiency. The calibration curves for the pesticides extracted were linear in the range of 0.05-10 μg L(-1) for chlorfenapyr and fenpyroximate and 0.05-20 μg L(-1) for fipronil and flusilazole, with the correlation coefficients (r(2)) between 0.9966 and 0.9990. The method gave good precisions (relative standard deviation %) from 2.9 to 10.1% for real spiked samples from reservoir water and seawater; method recoveries ranged 92.2-105.9 and 98.5-103.9% for real spiked samples from reservoir water and seawater, respectively. Limits of detection (S/N = 3) for the method were determined to be 8-19 ng L(-1). The optimized method was successfully applied to the determination of four pesticides of pyrazoles and pyrroles in real environmental water samples. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

DEVELOPMENT OF METHOD 535 FOR THE DETERMINATION OF CHLOROACETANILIDE AND OTHER ACETAMIDE HERBICIDE DEGRADATES IN DRINKING WATER BY SOLID PHASE EXTRACTION AND LIQUID CHROMATOGRAPHY/TANDEM MASS SPECTROMETRY

EPA Science Inventory

EPA Method 535 has been developed in order to provide a method for the analysis of "Alachlor ESA and other acetanilide degradation products" which are listed on U.S. EPA's 1998 Drinking Water Contaminant Candidate List. Method 535 uses solid phase extraction with a nonporous gr...

The Effect of Temperature on Pressurised Hot Water Extraction of Pharmacologically Important Metabolites as Analysed by UPLC-qTOF-MS and PCA

PubMed Central

Khoza, B. S.; Chimuka, L.; Mukwevho, E.; Steenkamp, P. A.; Madala, N. E.

2014-01-01

Metabolite extraction methods have been shown to be a critical consideration for pharmacometabolomics studies and, as such, optimization and development of new extraction methods are crucial. In the current study, an organic solvent-free method, namely, pressurised hot water extraction (PHWE), was used to extract pharmacologically important metabolites from dried Moringa oleifera leaves. Here, the temperature of the extraction solvent (pure water) was altered while keeping other factors constant using a homemade PHWE system. Samples extracted at different temperatures (50, 100, and 150°C) were assayed for antioxidant activities and the effect of the temperature on the extraction process was evaluated. The samples were further analysed by mass spectrometry to elucidate their metabolite compositions. Principal component analysis (PCA) evaluation of the UPLC-MS data showed distinctive differential metabolite patterns. Here, temperature changes during PHWE were shown to affect the levels of metabolites with known pharmacological activities, such as chlorogenic acids and flavonoids. Our overall findings suggest that, if not well optimised, the extraction temperature could compromise the “pharmacological potency” of the extracts. The use of MS in combination with PCA was furthermore shown to be an excellent approach to evaluate the quality and content of pharmacologically important extracts. PMID:25371697

Water isotope partitioning and ecohydrologic separation in mixed conifer forest explored with a centrifugation water extraction method

NASA Astrophysics Data System (ADS)

Bowers, W.; Mercer, J.; Pleasants, M.; Williams, D. G.

2017-12-01

Isotopic partitioning of water within soil into tightly and loosely bound fractions has been proposed to explain differences between isotopic water sources used by plants and those that contribute to streams and ground water, the basis for the "two water worlds" hypothesis. We examined the isotope ratio values of water in trees, bulk soil, mobile water collected from soil lysimeters, stream water, and GW at three different hillslopes in a mixed conifer forest in southeastern Wyoming, USA. Hillslopes differed in aspect and topographic position with corresponding differences in surface energy balance, snowmelt timing, and duration of soil moisture during the dry summer. The isotopic results support the partitioning of water within the soil; trees apparently used a different pool of water for transpiration than that recovered from soil lysimeters and the source was not resolved with the isotopic signature of the water that was extracted from bulk soil via cryogenic vacuum distillation. Separating and measuring the isotope ratios values in these pools would test the assumption that the tightly bound water within the soil has the same isotopic signature as the water transpired by the trees. We employed a centrifugation approach to separate water within the soil held at different tensions by applying stepwise increases in rotational velocity and pressures to the bulk soil samples. Effluent and the remaining water (cryogenically extracted) at each step were compared. We first applied the centrifugation method in a simple lab experiment using sandy loam soil and separate introductions of two isotopically distinct waters. We then applied the method to soil collected from the montane hillslopes. For the lab experiment, we predicted that effluents would have distinct isotopic signatures, with the last effluent and extracted water more closely representing the isotopic signature of the first water applied. For our field samples, we predicted that the isotopic signature of the water discharged in the last centrifuge step and final extraction would more closely represent the isotopic signature of water extracted from trees. Understanding the isotopic partitioning of water within soil is important for interpreting plant water isotope values within the context of the "two water worlds" hypothesis.

Development of a Solid Phase Extraction Method for Agricultural Pesticides in Large-Volume Water Samples

EPA Science Inventory

An analytical method using solid phase extraction (SPE) and analysis by gas chromatography/mass spectrometry (GC/MS) was developed for the trace determination of a variety of agricultural pesticides and selected transformation products in large-volume high-elevation lake water sa...

Mechanisms of post-supply contamination of drinking water in Bagamoyo, Tanzania.

PubMed

Harris, Angela R; Davis, Jennifer; Boehm, Alexandria B

2013-09-01

Access to household water connections remains low in sub-Saharan Africa, representing a public health concern. Previous studies have shown water stored in the home to be more contaminated than water at the source; however, the mechanisms of post-supply contamination remain unclear. Using water quality measurements and structured observations of households in Bagamoyo, Tanzania, this study elucidates the causal mechanisms of the microbial contamination of drinking water after collection from a communal water source. The study identifies statistically significant loadings of fecal indicator bacteria (FIB) occurring immediately after filling the storage container at the source and after extraction of the water from the container in the home. Statistically significant loadings of FIB also occur with various water extraction methods, including decanting from the container and use of a cup or ladle. Additionally, pathogenic genes of Escherichia coli were detected in stored drinking water but not in the source from which it was collected, highlighting the potential health risks of post-supply contamination. The results of the study confirm that storage containers and extraction utensils introduce microbial contamination into stored drinking water, and suggest that further research is needed to identify methods of water extraction that prevent microbial contamination of drinking water.

A review on green trend for oil extraction using subcritical water technology and biodiesel production.

PubMed

Abdelmoez, Weal; Ashour, Eman; Naguib, Shahenaz M

2015-01-01

It became a global agenda to develop clean alternative fuels which were domestically available, environmentally acceptable and technically feasible. Thus, biodiesel was destined to make a substantial contribution to the future energy demands of the domestic and industrial economies. Utilization of the non edible vegetable oils as raw materials for biodiesel production had been handled frequently for the past few years. The oil content of these seeds could be extracted by different oil extraction methods, such as mechanical extraction, solvent extraction and by subcritical water extraction technology SWT. Among them, SWT represents a new promising green extraction method. Therefore this review covered the current used non edible oil seeds for biodiesel production as well as giving a sharp focus on the efficiency of using the SWT as a promising extraction method. In addition the advantages and the disadvantages of the different biodiesel production techniques would be covered.

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.

Dispersive microextraction based on water-coated Fe₃O₄ followed by gas chromatography-mass spectrometry for determination of 3-monochloropropane-1,2-diol in edible oils.

PubMed

Zhao, Qin; Wei, Fang; Xiao, Neng; Yu, Qiong-Wei; Yuan, Bi-Feng; Feng, Yu-Qi

2012-06-01

In the present work, we developed a novel dispersive microextraction technique by combining the advantages of liquid-phase microextraction (LPME) and magnetic solid-phase extraction (MSPE). In this method, trace amount of water directly absorbed on bare Fe₃O₄ to form water-coated Fe₃O₄ (W-Fe₃O₄) and rapid extraction can be achieved while W-Fe₃O₄ dispersed in the sample solution. The analyte adsorbed W-Fe₃O₄ can be easily collected and isolated from sample solution by application of a magnet. It was worth noting that in the proposed method water was used as extractant and Fe₃O₄ served as the supporter and retriever of water. The performance of the method was evaluated by extraction of 3-monochloropropane-1,2-diol (3-MCPD) from edible oils. The extracted 3-MCPD was then derived by a silylanization reagent (1-trimethylsilylimidazole) before gas chromatography-mass spectrometry (GC-MS) analysis. Several parameters that affected the extraction and derivatization efficiency were investigated. Our results showed that the limit of detection for 3-MCPD was 1.1 ng/g. The recoveries in spiked oil samples were in the range of 70.0-104.9% with the RSDs less than 5.6% (intra-day) and 6.4% (inter-day). Taken together, the simple, rapid and cost-effective method developed in current study, offers a potential application for the extraction and preconcentration of hydrophilic analytes from complex fatty samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Extraction and characterization of bound extracellular polymeric substances from cultured pure cyanobacterium (Microcystis wesenbergii).

PubMed

Liu, Lizhen; Qin, Boqiang; Zhang, Yunlin; Zhu, Guangwei; Gao, Guang; Huang, Qi; Yao, Xin

2014-08-01

Preliminary characterization of bound extracellular polymeric substances (bEPS) of cyanobacteria is crucial to obtain a better understanding of the formation mechanism of cyanobacterial bloom. However, the characterization of bEPS can be affected by extraction methods. Five sets (including the control) of bEPS from Microcystis extracted by different methods were characterized using three-dimensional excitation and emission matrix (3DEEM) fluorescence spectroscopy combined chemical spectrophotometry; and the characterization results of bEPS samples were further compared. The agents used for extraction were NaOH, pure water and phosphate buffered saline (PBS) containing cationic exchange resins, and hot water. Extraction methods affected the fluorescence signals and intensities in the bEPS. Five fluorescence peaks were observed in the excitation and emission matrix fluorescence spectra of bEPS samples. Two peaks (peaks T₁ and T₂) present in all extractions were identified as protein-like fluorophores, two (peaks A and C) as humic-like fluorophores, and one (peak E) as a fulvic-like substance. Among these substances, the humic-like and fulvic-like fluorescences were only seen in the bEPS extracted with hot water. Also, NaOH solution extraction could result in strong fluorescence intensities compared to the other extraction methods. It was suggested that NaOH at pH10.0 was the most appropriate method to extract bEPS from Microcystis. In addition, dialysis could affect the yields and characteristics of extracted bEPS during the determination process. These results will help us to explore the issues of cyanobacterial blooms. Copyright © 2014. Published by Elsevier B.V.

METHOD 544. DETERMINATION OF MICROCYSTINS AND NODULARIN IN DRINKING WATER BY SOLID PHASE EXTRACTION AND LIQUID CHROMATOGRAPHY/TANDEM MASS SPECTROMETRY (LC/MS/MS)

EPA Science Inventory

Method 544 is an accurate and precise analytical method to determine six microcystins (including MC-LR) and nodularin in drinking water using solid phase extraction and liquid chromatography tandem mass spectrometry (SPE-LC/MS/MS). The advantage of this SPE-LC/MS/MS is its sensi...

A Simplified Method for Sampling and Analysis of High Volume Surface Water for Organic Contaminants Using XAD-2

USGS Publications Warehouse

Datta, S.; Do, L.V.; Young, T.M.

2004-01-01

A simple compressed-gas driven system for field processing and extracting water for subsequent analyses of hydrophobic organic compounds is presented. The pumping device is a pneumatically driven pump and filtration system that can easily clarify at 4L/min. The extraction device uses compressed gas to drive filtered water through two parallel XAD-2 resin columns, at about 200 mL/min. No batteries or inverters are required for water collection or processing. Solvent extractions were performed directly in the XAD-2 glass columns. Final extracts are cleaned-up on Florisil cartridges without fractionation and contaminants analyzed by GC-MS. Method detection limits (MDLs) and recoveries for dissolved organic contaminants, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and pesticides are reported along with results of surface water analysis for the San Francisco Bay, CA.

Electro-driven extraction of inorganic anions from water samples and water miscible organic solvents and analysis by ion chromatography.

PubMed

Nojavan, Saeed; Bidarmanesh, Tina; Memarzadeh, Farkhondeh; Chalavi, Soheila

2014-09-01

A simple electromembrane extraction (EME) procedure combined with ion chromatography (IC) was developed to quantify inorganic anions in different pure water samples and water miscible organic solvents. The parameters affecting extraction performance, such as supported liquid membrane (SLM) solvent, extraction time, pH of donor and acceptor solutions, and extraction voltage were optimized. The optimized EME conditions were as follows: 1-heptanol was used as the SLM solvent, the extraction time was 10 min, pHs of the acceptor and donor solutions were 10 and 7, respectively, and the extraction voltage was 15 V. The mobile phase used for IC was a combination of 1.8 mM sodium carbonate and 1.7 mM sodium bicarbonate. Under these optimized conditions, all anions had enrichment factors ranging from 67 to 117 with RSDs between 7.3 and 13.5% (n = 5). Good linearity values ranging from 2 to 1200 ng/mL with coefficients of determination (R(2) ) between 0.987 and 0.999 were obtained. The LODs of the EME-IC method ranged from 0.6 to 7.5 ng/mL. The developed method was applied to different samples to evaluate the feasibility of the method for real applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of two thin-film microextractions for the analysis of estrogens in aqueous tea extract and environmental water samples by high performance liquid chromatography-ultraviolet detection.

PubMed

Cai, Pei-Shan; Li, Dan; Chen, Jing; Xiong, Chao-Mei; Ruan, Jin-Lan

2015-04-15

Two thin-film microextractions (TFME), octadecylsilane (ODS)-polyacrylonitrile (PAN)-TFME and polar enhanced phase (PEP)-PAN-TFME have been proposed for the analysis of bisphenol-A, diethylstilbestrol and 17β-estradiol in aqueous tea extract and environmental water samples followed by high performance liquid chromatography-ultraviolet detection. Both thin-films were prepared by spraying. The influencing factors including pH, extraction time, desorption solvent, desorption volume, desorption time, ion strength and reusability were investigated. Under the optimal conditions, the two TFME methods are similar in terms of the analytical performance evaluated by standard addition method. The limits of detection for three estrogens in environmental water and aqueous tea extract matrix ranged from 1.3 to 1.6 and 2.8 to 7.1 ng mL(-1) by the two TFME methods, respectively. Both approaches were applied for the analysis of analytes in real aqueous tea extract and environmental water samples, presenting satisfactory recoveries ranged from 87.3% to 109.4% for the spiked samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Antimicrobial and Antibiofilm Activities of Citrus Water-Extracts Obtained by Microwave-Assisted and Conventional Methods.

PubMed

Caputo, Leonardo; Quintieri, Laura; Cavalluzzi, Maria Maddalena; Lentini, Giovanni; Habtemariam, Solomon

2018-06-17

Citrus pomace is a huge agro-food industrial waste mostly composed of peels and traditionally used as compost or animal feed. Owing to its high content of compounds beneficial to humans (e.g., flavonoids, phenol-like acids, and terpenoids), citrus waste is increasingly used to produce valuable supplements, fragrance, or antimicrobials. However, such processes require sustainable and efficient extraction strategies by solvent-free techniques for environmentally-friendly good practices. In this work, we evaluated the antimicrobial and antibiofilm activity of water extracts of three citrus peels (orange, lemon, and citron) against ten different sanitary relevant bacteria. Both conventional extraction methods using hot water (HWE) and microwave-assisted extraction (MAE) were used. Even though no extract fully inhibited the growth of the target bacteria, these latter (mostly pseudomonads) showed a significant reduction in biofilm biomass. The most active extracts were obtained from orange and lemon peel by using MAE at 100 °C for 8 min. These results showed that citrus peel water infusions by MAE may reduce biofilm formation possibly enhancing the susceptibility of sanitary-related bacteria to disinfection procedures.

Process for forming hydrogen and other fuels utilizing magma

DOEpatents

Galt, John K.; Gerlach, Terrence M.; Modreski, Peter J.; Northrup, Jr., Clyde J. M.

1978-01-01

The disclosure relates to a method for extracting hydrogen from magma and water by injecting water from above the earth's surface into a pocket of magma and extracting hydrogen produced by the water-magma reaction from the vicinity of the magma.

Multiclass method for the quantification of 92 veterinary antimicrobial drugs in livestock excreta, wastewater, and surface water by liquid chromatography with tandem mass spectrometry.

PubMed

Gao, Jinfang; Cui, Yonghui; Tao, Yanfei; Huang, Lingli; Peng, Dapeng; Xie, Shuyu; Wang, Xu; Liu, Zhenli; Chen, Dongmei; Yuan, Zonghui

2016-11-01

A simple multiresidue method was developed for detecting and quantifying 92 veterinary antimicrobial drugs from eight classes (β-lactams, quinolones, sulfonamides, tetracyclines, lincomycins, macrolides, chloramphenicols, and pleuromutilin) in livestock excreta and water by liquid chromatography with tandem mass spectrometry. The feces samples were extracted by ultrasound-assisted extraction with a mixture of acetonitrile/water (80:20, v/v) and edetate disodium, followed by a cleanup using solid-phase extraction with an amino cartridge. Water samples were purified with hydrophilic-lipophilic balance solid-phase extraction column. Urine samples were extracted with acetonitrile and edetate disodium. Detection of veterinary antimicrobial drugs was achieved by liquid chromatography with tandem mass spectrometry using both positive and negative electrospray ionization mode. The recovery values of veterinary antimicrobial drugs in feces, urine, and water samples were 75-99, 85-110, and 85-101% and associated relative standard deviations were less than 15, 10, and 8%, respectively. The limits of quantification in feces, urine, and water samples were 0.5-1, 0.5-1, and 0.01-0.05 μg/L, respectively. This method was applied to determine real samples obtained from local farms and provides reliable quantification and identification results of 92 veterinary antimicrobial drugs in livestock excreta and water. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of selected herbicides and their degradation products in water using solid-phase extraction and gas chromatography/mass spectrometry

USGS Publications Warehouse

Kish, J.L.; Thurman, E.M.; Scribner, E.A.; Zimmerman, L.R.

2000-01-01

A method for the extraction and analysis of eight herbicides and five degradation products using solid-phase extraction from natural water samples followed by gas chromatography/mass spectrometry is presented in this report. This method was developed for dimethenamid; flufenacet; fluometuron and its degradation products, demethylfluometuron (DMFM), 3-(trifluromethyl)phenylurea (TFMPU), 3-(trifluromethyl)-aniline (TFMA); molinate; norflurazon and its degradation product, demethylnorflurazon; pendamethalin; the degradation product of prometryn, deisopropylprometryn; propanil; and trifluralin. The eight herbicides are used primarily in the southern United States where cotton, rice, and soybeans are produced. The exceptions are dimethenamid and flufenacet, which are used on corn in the Midwest. Water samples received by the U.S. Geological Survey's Organic Geochemistry Research Group in Lawrence, Kansas, are filtered to remove suspended particulate matter and then passed through disposable solid-phase extraction columns containing octadecyl-bonded porous silica (C-18) to extract the compounds. The herbicides and their degradation products are removed from the column by ethyl acetate elution. The eluate is evaporated under nitrogen, and components then are separated, identified, and quantified by injecting an aliquot of the concentrated extract into a high-resolution, fused-silica capillary column of a gas chromatograph/mass spectrometer under selected-ion mode. Method detection limits ranged from 0.02 to 0.05 ?g/L for all compounds with the exception of TFMPU, which has a method detection limit of 0.32 ?g/L. The mean absolute recovery is 107 percent. This method for the determination of herbicides and their degradation products is valuable for acquiring information about water quality and compound fate and transport in water.

Extraction and LC determination of lysine clonixinate salt in water/oil microemulsions.

PubMed

Pineros, I; Ballesteros, P; Lastres, J L

2002-02-01

A new reversed-phase high performance liquid chromatography method has been developed and validated for the quantitative determination of lysine clonixinate salt in water/oil microemulsions. The mobile phase was acetonitrile-buffer phosphate pH 3.3. Detection was UV absorbance at 252 nm. The precision and accurately of the method were excellent. The established linearity range was 5-60 microg ml(-1) (r(2)=0.999). Microemulsions samples were dispersed with chloroform and extracted lysine clonixinate salt with water. This easy method employing chloroformic extraction has been done three times. The recovery of lysine clonixinate salt from spiked placebo and microemulsion were >90% over the linear range.

Assessment of the Extraction Methods for Monitoring Phthalate Emerging Contaminants in Groundwater and Tap Water

NASA Astrophysics Data System (ADS)

Cotto, I.; Padilla, I. Y.; De Jesús, N. H.; Torres, P. M.

2015-12-01

Trace organic contaminants such as phthalates, among other chemicals of emerging concerns, have not historically been considered as pollutants but are being detected in water, posing a potential risk to public health and the environment. One of the most common phthalates of particular concern is di-(2-ethylhexyl) phthalate (DEHP), a plasticizer normally found in plastics and consumer products, including: cosmetics, pharmaceuticals, medical devices, food packages, water bottles, and wiring cables. DEHP has been associated with preterm birth, a major cause of neonatal mortality and health complications. This study aims at monitoring the presence and concentration of DEHP and other phthalates in groundwater and tap water systems in Puerto Rico, which has one of the highest rates of preterm birth in the U.S. The Environmental Protection Agency (EPA) suggests a liquid-liquid extraction method that uses methylene chloride as the preferred organic solvent for the extractions. This work presents modified EPA methods that reduce the volume of sample and solvent used, lower the time of analysis, increase productivity, and decrease hazards and waste. Distribution coefficient of DEHP between methylene chloride and water are estimated and related to sample extraction efficiency. Research results indicate that DEHP is in fact distributed between water and methylene chloride with a distribution coefficient average value of 1.24. The study concludes that the sample and solvent volumes have influence on the efficiency but have not an effect on the distribution coefficient. The tests show higher extraction efficiencies for lower DEHP concentrations and higher extraction volumes. Results from the water analysis show presence of DEHP in 55% of groundwater and 44% of tap water samples, indicating a potential exposure through water.

[Evaluation for extraction process of Shenqi Tongmai Yizhi particles based on antioxidant capacity in vitro and its spectrum-effect relation].

PubMed

Zhang, Xiao-Li; Liu, Yu-Ling; Fan, Li-Jiao; Wang, Yue-Liang; Chen, Kai; Li, Hui

2016-05-01

Based on DPPH method, the antioxidant activities of Shenqi Tongmai Yizhi particles with different extraction processes were compared. The contribution to the anti-oxidant capacity in vitro was explored by means of grey relational analysis on different chemical compositions in the fingerprint. The results showed that the IC₅₀ concentration values of water extract, water extract from alcohol precipitation, alcohol extract, and alcohol and water extract were 0.801 4, 0.859 1, 0.796 1, 0.918 0 g•L⁻¹; and the alcohol extract is the best method to extract antioxidative components, with the highest antioxidant activity and lowest IC₅₀. When the mass concentration of the herbs reached a certain degree, its free radical clearance rate was similar to that of vitamin C control group. The order of different chemical contributions of constituents to the antioxidant activity in the fingerprint was 4>3>33>53>9>10>11>34>15>59>8>61>52>20>42>18>29. The preliminary exploration for the spectrum efficiency relations provides reference for studying traditional Chinese medicine compound processing method and the pharmacodyamic material basis. Copyright© by the Chinese Pharmaceutical Association.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Zaugg, Steven D.; Sandstrom, Mark W.; Smith, Steven G.; Fehlberg, Kevin M.

1995-01-01

A method for the isolation of 41 pesticides and pesticide metabolites in natural-water samples using C-18 solid-phase extraction and determination by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction columns containing octadecyl-bonded porous silica to extract the pesticides. The columns are dried using carbon dioxide or nitrogen gas, and adsorbed pesticides are removed from the columns by elution with 3.0 milliliters of hexane-isopropanol (3:1). Extracted pesticides are determined by capillary- column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 4 micrograms per liter (g/L) for most pesticides, with the exception of widely used corn herbicides--atrazine, alachlor, cyanazine, and metolachlor--which have upper concentration limits of 20 g/L. Single- operator method detection limits in reagent-water samples range from 0.001 to 0.018 g/L. Average short-term single-operator precision in reagent- water samples is 7 percent at the 0.1- and 1.0-g/L levels and 8 percent at the 0.01-g/L level. Mean recoveries in reagent-water samples are 73 percent at the 0.1- and 1.0-g/L levels and 83 percent at the 0.01-g/L level. The estimated holding time for pesticides after extraction on the solid-phase extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time.

Extending the applicability of pressurized hot water extraction to compounds exhibiting limited water solubility by pH control: curcumin from the turmeric rhizome.

PubMed

Euterpio, Maria Anna; Cavaliere, Chiara; Capriotti, Anna Laura; Crescenzi, Carlo

2011-11-01

Pressurized hot water extraction (PHWE, also known as subcritical water extraction) is commonly considered to be an environmentally friendly extraction technique that could potentially replace traditional methods that use organic solvents. Unfortunately, the applicability of this technique is often limited by the very low water solubility of the target compounds, even at high temperatures. In this paper, the scope for broadening the applicability of PHWE by adjusting the pH of the water used in the extraction is demonstrated in the extraction of curcumin (which exhibits very limited water solubility) from untreated turmeric (Curcuma longa L.) rhizomes. Although poor extraction yields were obtained, even at high temperatures when using degassed water or neutral phosphate buffer as the extraction medium, yields exceeding those obtained by Soxhlet extraction were achieved using highly acidic pH buffers due to curcumin protonation. The influence of the temperature, pH, and buffer concentration on the extraction yield were investigated in detail by means of a series of designed experiments. Optimized conditions for the extraction of curcumin from turmeric by PHWE were estimated at 197 °C using 62 g/L buffer concentration at pH 1.6. The relationships between these variables were subjected to statistical analysis using response surface methodology.

Simultaneous dispersive liquid-liquid microextraction derivatisation and gas chromatography mass spectrometry analysis of subcritical water extracts of sweet and sour cherry stems.

PubMed

Švarc-Gajić, Jaroslava; Clavijo, Sabrina; Suárez, Ruth; Cvetanović, Aleksandra; Cerdà, Víctor

2018-03-01

Cherry stems have been used in traditional medicine mostly for the treatment of urinary tract infections. Extraction with subcritical water, according to its selectivity, efficiency and other aspects, differs substantially from conventional extraction techniques. The complexity of plant subcritical water extracts is due to the ability of subcritical water to extract different chemical classes of different physico-chemical properties and polarities in a single run. In this paper, dispersive liquid-liquid microextraction (DLLME) with simultaneous derivatisation was optimised for the analysis of complex subcritical water extracts of cherry stems to allow simple and rapid preparation prior to gas chromatography-mass spectrometry (GC-MS). After defining optimal extracting and dispersive solvents, the optimised method was used for the identification of compounds belonging to different chemical classes in a single analytical run. The developed sample preparation protocol enabled simultaneous extraction and derivatisation, as well as convenient coupling with GC-MS analysis, reducing the analysis time and number of steps. The applied analytical protocol allowed simple and rapid chemical screening of subcritical water extracts and was used for the comparison of subcritical water extracts of sweet and sour cherry stems. Graphical abstract DLLME GC MS analysis of cherry stem extracts obtained by subcritical water.

Improvement of seawater salt quality by hydro-extraction and re-crystallization methods

NASA Astrophysics Data System (ADS)

Sumada, K.; Dewati, R.; Suprihatin

2018-01-01

Indonesia is one of the salt producing countries that use sea water as a source of raw materials, the quality of salt produced is influenced by the quality of sea water. The resulting average salt quality contains 85-90% NaCl. The Indonesian National Standard (SNI) for human salt’s consumption sodium chloride content is 94.7 % (dry base) and for industrial salt 98,5 %. In this study developed the re-crystallization without chemical and hydro-extraction method. The objective of this research to choose the best methods based on efficiency. The results showed that re-crystallization method can produce salt with NaCl content 99,21%, while hydro-extraction method content 99,34 % NaCl. The salt produced through both methods can be used as a consumption and industrial salt, Hydro-extraction method is more efficient than re-crystallization method because re-crystallization method requires heat energy.

Design and optimization of a semicontinuous hot-cold extraction of polyphenols from grape pomace.

PubMed

Monrad, Jeana K; Srinivas, Keerthi; Howard, Luke R; King, Jerry W

2012-06-06

Grape pomace contains appreciable amounts of polyphenolic compounds such as anthocyanins and procyanidins which can be recovered for use as food supplements. The extraction of these polyphenols from the pomace is usually accomplished at slightly elevated temperatures, frequently employing hydroethanolic solvents. Due to governmental regulations and the cost involved in using ethanol as a solvent, as well as the loss in polyphenolics due to thermal degradation, improved extraction techniques are required. In this study, a semicontinuous extraction apparatus employing only water was developed to maximize the recovery of anthocyanins and procyanidins from red grape pomace (Vitis vinifera). Water is preheated prior to its entry to the extraction cell containing the grape pomace sample, where it is allowed to then flow continuously through the unheated extraction vessel prior to its collection at ambient conditions. Extraction variables that impacted the polyphenolic recovery included pomace moisture content (crude or dried), sample mass, water flow rate, and extraction temperature. A response surface method was used to analyze the results from the extraction, and the optimal conditions were found to be 140 °C and 9 mL/min water flow rate. These conditions can produce an extract containing 130 mg/100 g DW of anthocyanins and 2077 mg/100 g DW of procyanidins. Higher yields of polyphenolics were observed using crude (wet) rather than dried pomace, hence avoiding the need to dry the pomace prior to extraction. The described semicontinuous extraction method using only water as the extraction solvent under subcritical conditions allowed the efficient extraction of polyphenols from red grape pomace without the attendant loss of polyphenolic content due to having to heat the extraction vessel prior to commencement of extraction.

Effect of Punica granatum L. Flower Water Extract on Five Common Oral Bacteria and Bacterial Biofilm Formation on Orthodontic Wire

PubMed Central

VAHID DASTJERDI, Elahe; ABDOLAZIMI, Zahra; GHAZANFARIAN, Marzieh; AMDJADI, Parisa; KAMALINEJAD, Mohammad; MAHBOUBI, Arash

2014-01-01

Background: Use of herbal extracts and essences as natural antibacterial compounds has become increasingly popular for the control of oral infectious diseases. Therefore, finding natural antimicrobial products with the lowest side effects seems necessary. The present study sought to assess the effect of Punica granatum L. water extract on five oral bacteria and bacterial biofilm formation on orthodontic wire. Methods: Antibacterial property of P. granatum L. water extract was primarily evaluated in brain heart infusion agar medium using well-plate method. The minimum inhibitory concentration and minimum bactericidal concentration were determined by macro-dilution method. The inhibitory effect on orthodontic wire bacterial biofilm formation was evaluated using viable cell count in biofilm medium. At the final phase, samples were fixed and analyzed by Scanning Electron Microscopy. Results: The growth inhibition zone diameter was proportional to the extract concentration. The water extract demonstrated the maximum antibacterial effect on Streptococcus sanguinis ATCC 10556 with a minimum inhibitory concentration of 6.25 mg/ml and maximum bactericidal effect on S. sanguinis ATCC 10556 and S. sobrinus ATCC 27607 with minimum bactericidal concentration of 25 mg/ml. The water extract decreased bacterial biofilm formation by S. sanguinis, S. sobrinus, S. salivarius, S. mutans ATCC 35608 and E. faecalis CIP 55142 by 93.7–100%, 40.6–99.9%, 85.2–86.5%, 66.4–84.4% and 35.5–56.3% respectively. Conclusion: Punica granatum L. water extract had significant antibacterial properties against 5 oral bacteria and prevented orthodontic wire bacterial biofilm formation. However, further investigations are required to generalize these results to the clinical setting. PMID:26171362

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.

The role of water in unconventional in situ energy resource extraction technologies: Chapter 7 in Food, energy, and water: The chemistry connection

USGS Publications Warehouse

Gallegos, Tanya J.; Bern, Carleton R.; Birdwell, Justin E.; Haines, Seth S.; Engle, Mark A.

2015-01-01

Global trends toward developing new energy resources from lower grade, larger tonnage deposits that are not generally accessible using “conventional” extraction methods involve variations of subsurface in situ extraction techniques including in situ oil-shale retorting, hydraulic fracturing of petroleum reservoirs, and in situ recovery (ISR) of uranium. Although these methods are economically feasible and perhaps result in a smaller above-ground land-use footprint, there remain uncertainties regarding potential subsurface impacts to groundwater. This chapter provides an overview of the role of water in these technologies and the opportunities and challenges for water reuse and recycling.

Method for analysis of psychopharmaceuticals in real industrial wastewater and groundwater with suspended organic particulate matter using solid phase extraction disks extraction and ultra-high performance liquid chromatography/time-of-flight mass spectrometry.

PubMed

Křesinová, Zdena; Linhartová, Lucie; Petrů, Klára; Krejčová, Lucie; Šrédlová, Kamila; Lhotský, Ondřej; Kameník, Zdeněk; Cajthaml, Tomáš

2016-04-01

A rapid and reliable analytical method was developed for the quantitative determination of psychopharmaceuticals, their precursors and by-products in real contaminated samples from a pharmaceutical company in Olomouc (Czech Republic), based on SPE disk extraction and detection by ultra performance liquid chromatography, combined with time-of-flight mass spectrometry. The target compounds were quantified in the real whole-water samples (water including suspended particles), both in the presence of suspended particulate matter (SPM) and high concentrations of other organic pollutants. A total of nine compounds were analyzed which consisted of three commonly used antidepressants (tricyclic antidepressants and antipsychotics), one antitussive agent and five by-products or precursors. At first, the SPE disk method was developed for the extraction of water samples (dissolved analytes, recovery 84-104%) and pressurised liquid extraction technique was verified for solid matrices (sludge samples, recovery 81-95%). In order to evaluate the SPE disk technique for whole water samples containing SPM, non contaminated groundwater samples were also loaded with different amounts (100 and 300mgL(-1)) of real contaminated sludge originating from the same locality. The recoveries from the whole-water samples obtained by SPE disk method ranged between 67 and 119% after the addition of the most contaminated sludge. The final method was applied to several real groundwater (whole-water) samples from the industrial area and high concentrations (up to 10(3)μgL(-1)) of the target compounds were detected. The results of this study document and indicate the feasibility of the SPE disk method for analysis of groundwater. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of GC-MS and FTIR methods for quantifying naphthenic acids in water samples.

PubMed

Scott, Angela C; Young, Rozlyn F; Fedorak, Phillip M

2008-11-01

The extraction of bitumen from the oil sands in Canada releases toxic naphthenic acids into the process-affected waters. The development of an ideal analytical method for quantifying naphthenic acids (general formula C(n)H(2n+Z)O(2)) has been impeded by the complexity of these mixtures and the challenges of differentiating naphthenic acids from other naturally-occurring organic acids. The oil sands industry standard FTIR method was compared with a newly-developed GC-MS method. Naphthenic acids concentrations were measured in extracts of surface and ground waters from locations within the vicinity of and away from the oil sands deposits and in extracts of process-affected waters. In all but one case, FTIR measurements of naphthenic acids concentrations were greater than those determined by GC-MS. The detection limit of the GC-MS method was 0.01 mg L(-1) compared to 1 mg L(-1) for the FTIR method. The results indicated that the GC-MS method is more selective for naphthenic acids, and that the FTIR method overestimates their concentrations.

Comparison of two different solvents employed for pressurised fluid extraction of stevioside from Stevia rebaudiana: methanol versus water.

PubMed

Pól, Jaroslav; Varadová Ostrá, Elena; Karásek, Pavel; Roth, Michal; Benesová, Karolínka; Kotlaríková, Pavla; Cáslavský, Josef

2007-08-01

Pressurised fluid extraction using water or methanol was employed for the extraction of stevioside from Stevia rebaudiana Bertoni. The extraction method was optimised in terms of temperature and duration of the static or the dynamic step. Extracts were analysed by liquid chromatography followed by UV and mass-spectrometric (MS) detections. Thermal degradation of stevioside was the same in both solvents within the range 70-160 degrees C. Methanol showed better extraction ability for isolation of stevioside from Stevia rebaudiana leaves than water within the range 110-160 degrees C. However, water represents the green alternative to methanol. The limit of detection of stevioside in the extract analysed was 30 ng for UV detection and 2 ng for MS detection.

Method of manipulating the chemical properties of water to improve the effectiveness of a desired chemical process

DOEpatents

Hawthorne, Steven B.; Miller, David J.; Yang, Yu; Lagadec, Arnaud Jean-Marie

1999-01-01

The method of the present invention is adapted to manipulate the chemical properties of water in order to improve the effectiveness of a desired chemical process. The method involves heating the water in the vessel to subcritical temperatures between 100.degree. to 374.degree. C. while maintaining sufficient pressure to the water to maintain the water in the liquid state. Various physiochemical properties of the water can be manipulated including polarity, solute solubility, surface tension, viscosity, and the disassociation constant. The method of the present invention has various uses including extracting organics from solids and semisolids such as soil, selectively extracting desired organics from nonaqueous liquids, selectively separating organics using sorbent phases, enhancing reactions by controlling the disassociation constant of water, cleaning waste water, and removing organics from water using activated carbon or other suitable sorbents.

Method of manipulating the chemical properties of water to improve the effectiveness of a desired process

DOEpatents

Hawthorne, Steven B.; Miller, David J.; Lagadec, Arnaud Jean-Marie; Hammond, Peter James; Clifford, Anthony Alan

2002-01-01

The method of the present invention is adapted to manipulate the chemical properties of water in order to improve the effectiveness of a desired process. The method involves heating the water in the vessel to subcritical temperatures between 100.degree. to 374.degree. C. while maintaining sufficient pressure to the water to maintain the water in the liquid state. Various physiochemical properties of the water can be manipulated including polarity, solute solubility, surface tension, viscosity, and the disassociation constant. The method of the present invention has various uses including extracting organics from solids and semisolids such as soil, selectively extracting desired organics from liquids, selectively separating organics using sorbent phases, enhancing reactions by controlling the disassociation constant of water, cleaning waste water, removing organics from water using activated carbon or other suitable sorbents, and degrading various compounds.

Development of a comprehensive screening method for more than 300 organic chemicals in water samples using a combination of solid-phase extraction and liquid chromatography-time-of-flight-mass spectrometry.

PubMed

Chau, Hong Thi Cam; Kadokami, Kiwao; Ifuku, Tomomi; Yoshida, Yusuke

2017-12-01

A comprehensive screening method for 311 organic compounds with a wide range of physicochemical properties (log Pow -2.2-8.53) in water samples was developed by combining solid-phase extraction with liquid chromatography-high-resolution time-of-flight mass spectrometry. Method optimization using 128 pesticides revealed that tandem extraction with styrene-divinylbenzene polymer and activated carbon solid-phase extraction cartridges at pH 7.0 was optimal. The developed screening method was able to extract 190 model compounds with average recovery of 80.8% and average relative standard deviations (RSD) of 13.5% from spiked reagent water at 0.20 μg L -1 , and 87.1% recovery and 10.8% RSD at 0.05 μg L -1 . Spike-recovery testing (0.20 μg L -1 ) using real sewage treatment plant effluents resulted in an average recovery and average RSD of 190 model compounds of 77.4 and 13.1%, respectively. The method was applied to the influent and effluent of five sewage treatment plants in Kitakyushu, Japan, with 29 out of 311 analytes being observed at least once. The results showed that this method can screen for a large number of chemicals with a wide range of physicochemical properties quickly and at low operational cost, something that is difficult to achieve using conventional analytical methods. This method will find utility in target screening of hazardous chemicals with a high risk in environmental waters, and for confirming the safety of water after environmental incidents.

A method of extracting impervious surface based on rule algorithm

NASA Astrophysics Data System (ADS)

Peng, Shuangyun; Hong, Liang; Xu, Quanli

2018-02-01

The impervious surface has become an important index to evaluate the urban environmental quality and measure the development level of urbanization. At present, the use of remote sensing technology to extract impervious surface has become the main way. In this paper, a method to extract impervious surface based on rule algorithm is proposed. The main ideas of the method is to use the rule-based algorithm to extract impermeable surface based on the characteristics and the difference which is between the impervious surface and the other three types of objects (water, soil and vegetation) in the seven original bands, NDWI and NDVI. The steps can be divided into three steps: 1) Firstly, the vegetation is extracted according to the principle that the vegetation is higher in the near-infrared band than the other bands; 2) Then, the water is extracted according to the characteristic of the water with the highest NDWI and the lowest NDVI; 3) Finally, the impermeable surface is extracted based on the fact that the impervious surface has a higher NDWI value and the lowest NDVI value than the soil.In order to test the accuracy of the rule algorithm, this paper uses the linear spectral mixed decomposition algorithm, the CART algorithm, the NDII index algorithm for extracting the impervious surface based on six remote sensing image of the Dianchi Lake Basin from 1999 to 2014. Then, the accuracy of the above three methods is compared with the accuracy of the rule algorithm by using the overall classification accuracy method. It is found that the extraction method based on the rule algorithm is obviously higher than the above three methods.

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).

A fast stir bar sorptive extraction method for the analysis of geosmin and 2-methylisoborneol in source and drinking water.

PubMed

Bauld, T; Teasdale, P; Stratton, H; Uwins, H

2007-01-01

The presence of unpleasant taste and odour in drinking water is an ongoing aesthetic concern for water providers worldwide. The need for a sensitive and robust method capable of analysis in both natural and treated waters is essential for early detection of taste and odour events. The purpose of this study was to develop and optimise a fast stir bar sorptive extraction (SBSE) method for the analysis of geosmin and 2-methylisoborneol (MIB) in both natural water and drinking water. Limits of detection with the optimised fast method (45 min extraction time at 60 degrees C using 24 microL stir bars) were 1.1 ng/L for geosmin and 4.2 ng/L for MIB. Relative standard deviations at the detection limits were under 17% for both compounds. Use of multiple stir bars can be used to decrease the detection limits further. The use of 25% NaCl and 5% methanol sample modifiers decreased the experimental recoveries. Likewise, addition of 1 mg/L and 1.5 mg/L NaOCI decreased the recoveries and this effect was not reversed by addition of 10% thiosulphate. The optimised method was used to measure geosmin concentrations in treated and untreated drinking water. MIB concentrations were below the detection limits in these waters.

Development of a magnetic solid-phase extraction coupled with high-performance liquid chromatography method for the analysis of polyaromatic hydrocarbons.

PubMed

Ma, Yan; Xie, Jiawen; Jin, Jing; Wang, Wei; Yao, Zhijian; Zhou, Qing; Li, Aimin; Liang, Ying

2015-07-01

A novel magnetic solid phase extraction coupled with high-performance liquid chromatography method was established to analyze polyaromatic hydrocarbons in environmental water samples. The extraction conditions, including the amount of extraction agent, extraction time, pH and the surface structure of the magnetic extraction agent, were optimized. The results showed that the amount of extraction agent and extraction time significantly influenced the extraction performance. The increase in the specific surface area, the enlargement of pore size, and the reduction of particle size could enhance the extraction performance of the magnetic microsphere. The optimized magnetic extraction agent possessed a high surface area of 1311 m(2) /g, a large pore size of 6-9 nm, and a small particle size of 6-9 μm. The limit of detection for phenanthrene and benzo[g,h,i]perylene in the developed analysis method was 3.2 and 10.5 ng/L, respectively. When applied to river water samples, the spiked recovery of phenanthrene and benzo[g,h,i]perylene ranged from 89.5-98.6% and 82.9-89.1%, respectively. Phenanthrene was detected over a concentration range of 89-117 ng/L in three water samples withdrawn from the midstream of the Huai River, and benzo[g,h,i]perylene was below the detection limit. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simplification and validation of a large volume polyurethane foam sampler for the analysis of persistent hydrophobic compounds in drinking water.

PubMed

Choi, J W; Lee, J H; Moon, B S; Kannan, K

2008-08-01

The use of a large volume polyurethane foam (PUF) sampler was validated for rapid extraction of persistent organic pollutants (POPs), such as polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), in raw water and treated water from drinking water plants. To validate the recovery of target compounds in the sampling process, a (37)Cl-labeled standard was spiked into the 1st PUF plug prior to filtration. An accelerated solvent extraction method, as a pressurized liquid extractor (PLE), was optimized to extract the PUF plug. For sample preparation, tandem column chromatography (TCC) clean-up was used for rapid analysis. The recoveries of labeled compounds in the analytical method were 80-110% (n = 9). The optimized PUF-PLE-TCC method was applied in the analysis of raw water and treated potable water from seven drinking water plants in South Korea. The sample volume used was between 18 and 102 L for raw water at a flow rate of 0.4-2 L min(-1), 95 and 107 L for treated water at a flow rate of 1.5-2.2 L min(-1). Limit of quantitation (LOQ) was a function of sample volume and it decreased with increasing sample volume. The LOQ of PCDD/Fs in raw waters analyzed by this method was 3-11 times lower than that described using large-size disk-type solid phase extraction (SPE) method. The LOQ of PCDD/F congeners in raw water and treated water were 0.022-3.9 ng L(-1) and 0.018-0.74 ng L(-1), respectively. Octachlorinated dibenzo-p-dioxin (OCDD) was found in some raw water samples, while their concentrations were well below the tentative criterion set by the Japanese Environmental Ministry for drinking water. OCDD was below the LOQ in the treated drinking water.

Phytochemical Comparison of the Water and Ethanol Leaf Extracts of the Cree medicinal plant, Sarracenia purpurea L. (Sarraceniaceae).

PubMed

Cieniak, Carolina; Walshe-Roussel, Brendan; Liu, Rui; Muhammad, Asim; Saleem, Ammar; Haddad, Pierre S; Cuerrier, Alain; Foster, Brian C; Arnason, John T

2015-01-01

The Cree of Eeyou Istchee in Northern Quebec identified Sarracenia purpurea L. as an important plant for the treatment of Type 2 diabetes. Traditionally the plant is used as a decoction (boiling water extract) of the leaf, however, in order to study the extract in a laboratory setting, an 80% ethanol extract was used. In this study, the phytochemistry of both extracts of the leaves was compared and quantified. Two S. purpurea leaf extracts were prepared, one a traditional hot water extract and the other an 80% ethanol extract. Using UPLC-ESI-MS, the extracts were phytochemically compared for 2 triterpenes, betulinic acid and ursolic acid, using one gradient method and for 10 additional substances, including the actives quercetin-3-O-galactoside and morroniside, using a different method. The concentrations of the nine phenolic substances present, as well as an active principle, the iridoid glycoside morroniside, were very similar between the two extracts, with generally slightly higher concentrations of phenolics in the ethanol extract as expected. However, two triterpenes, betulinic acid and ursolic acid, were 107 and 93 times more concentrated, respectively, in the ethanol extract compared to the water extract. The main phytochemical markers and most importantly the antidiabetic active principles, quercetin-3-O-galactoside and morroniside, were present in similar amounts in the two extracts, which predicts similar bioactivity.This article is open to POST-PUBLICATION REVIEW. Registered readers (see "For Readers") may comment by clicking on ABSTRACT on the issue's contents page.

[HPLC-ESI-MS(n) analysis of the water soluble extracts of Fructus Choerospondiatis].

PubMed

Shi, Run-ju; Dai, Yun; Fang, Min-feng; Zhao, Xin; Zheng, Jian-bin; Zheng, Xiao-hui

2007-03-01

To establish an HPLC-ESI-MS(n) method for analyzing the chemical ingredients in the water soluble extracts of Fructus Choerospondiatis. Water-solvable extracts of Fructus Choerospondiatis are obtained by heating recirculation. Multi-stage reaction mode (MRM) of the HPLC-ESI-MS(n) was used to determine the content of Gallic acid, the MS(n) technology was used to obtain the information of characteristic multistage fragment ions so as to identify the chemical structure of peaks in the total current spectrum. Eleven compounds were identified, and one of them is a new unknown ingredient. The method, which has high recovery and specificity, can offer the experimental evidences for the further research of the chemical ingredients extracted from the Fructus Choerospondiatis.

Characterisation of chamomile volatiles by simultaneous distillation solid-phase extraction in comparison to hydrodistillation and simultaneous distillation extraction.

PubMed

Krüger, Hans

2010-05-01

A new method for complete separation of steam-volatile organic compounds is described using the example of chamomile flowers. This method is based on the direct combination of hydrodistillation and solid-phase extraction in a circulation apparatus. In contrast to hydrodistillation and simultaneous distillation extraction (SDE), an RP-18 solid phase as adsorptive material is used rather than a water-insoluble solvent. Therefore, a prompt and complete fixation of all volatiles takes place, and the circulation of water-soluble bisabololoxides as well as water-soluble and thermolabile en-yne-spiroethers is inhibited. This so-called simultaneous distillation solid-phase extraction (SD-SPE) provides extracts that better characterise the real composition of the vapour phase, as well as the composition of inhalation vapours, than do SDE extracts or essential oils obtained by hydrodistillation. The data indicate that during inhalation therapy with chamomile, the bisabololoxides and spiroethers are more strongly involved in the inhaling activity than so far assumed. Georg Thieme Verlag KG Stuttgart New York.

Use of experimental design in the investigation of stir bar sorptive extraction followed by ultra-high-performance liquid chromatography-tandem mass spectrometry for the analysis of explosives in water samples.

PubMed

Schramm, Sébastien; Vailhen, Dominique; Bridoux, Maxime Cyril

2016-02-12

A method for the sensitive quantification of trace amounts of organic explosives in water samples was developed by using stir bar sorptive extraction (SBSE) followed by liquid desorption and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The proposed method was developed and optimized using a statistical design of experiment approach. Use of experimental designs allowed a complete study of 10 factors and 8 analytes including nitro-aromatics, amino-nitro-aromatics and nitric esters. The liquid desorption study was performed using a full factorial experimental design followed by a kinetic study. Four different variables were tested here: the liquid desorption mode (stirring or sonication), the chemical nature of the stir bar (PDMS or PDMS-PEG), the composition of the liquid desorption phase and finally, the volume of solvent used for the liquid desorption. On the other hand, the SBSE extraction study was performed using a Doehlert design. SBSE extraction conditions such as extraction time profiles, sample volume, modifier addition, and acetic acid addition were examined. After optimization of the experimental parameters, sensitivity was improved by a factor 5-30, depending on the compound studied, due to the enrichment factors reached using the SBSE method. Limits of detection were in the ng/L level for all analytes studied. Reproducibility of the extraction with different stir bars was close to the reproducibility of the analytical method (RSD between 4 and 16%). Extractions in various water sample matrices (spring, mineral and underground water) have shown similar enrichment compared to ultrapure water, revealing very low matrix effects. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2012-08-15

The present study demonstrates a simple, rapid and efficient method for the determination of chlorinated anilines (CAs) in environmental water samples using ultrasonication assisted emulsification microextraction technique based on solidification of floating organic droplet (USAEME-SFO) coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection. In this extraction method, 1-dodecanol was used as extraction solvent which is of lower density than water, low toxicity, low volatility, and low melting point (24 °C). After the USAEME, extraction solvent could be collected easily by keeping the extraction tube in ice bath for 2 min and the solidified organic droplet was scooped out using a spatula and transferred to another glass vial and allowed to thaw. Then, 10 μL of extraction solvent was diluted with mobile phase (1:1) and taken for HPLC-UV analysis. Parameters influencing the extraction efficiency, such as the kind and volume of extraction solvent, volume of sample, ultrasonication time, pH and salt concentration were thoroughly examined and optimized. Under the optimal conditions, the method showed good linearity in the concentration range of 0.05-500 ng mL(-1) with correlation coefficients ranging from 0.9948 to 0.9957 for the three target CAs. The limit of detection based on signal to noise ratio of 3 ranged from 0.01 to 0.1 ng mL(-1). The relative standard deviations (RSDs) varied from 2.1 to 6.1% (n=3) and the enrichment factors ranged from 44 to 124. The proposed method has also been successfully applied to analyze real water samples and the relative recoveries of environmental water samples ranged from 81.1 to 116.9%. Copyright © 2012 Elsevier B.V. All rights reserved.

Quantification of the xenoestrogens 4-tert.-octylphenol and bisphenol A in water and in fish tissue based on microwave assisted extraction, solid-phase extraction and liquid chromatography-mass spectrometry.

PubMed

Pedersen, S N; Lindholst, C

1999-12-09

Extraction methods were developed for quantification of the xenoestrogens 4-tert.-octylphenol (tOP) and bisphenol A (BPA) in water and in liver and muscle tissue from the rainbow trout (Oncorhynchus mykiss). The extraction of tOP and BPA from tissue samples was carried out using microwave-assisted solvent extraction (MASE) followed by solid-phase extraction (SPE). Water samples were extracted using only SPE. For the quantification of tOP and BPA, liquid chromatography mass spectrometry (LC-MS) equipped with an atmospheric pressure chemical ionisation interface (APCI) was applied. The combined methods for tissue extraction allow the use of small sample amounts of liver or muscle (typically 1 g), low volumes of solvent (20 ml), and short extraction times (25 min). Limits of quantification of tOP in tissue samples were found to be approximately 10 ng/g in muscle and 50 ng/g in liver (both based on 1 g of fresh tissue). The corresponding values for BPA were approximately 50 ng/g in both muscle and liver tissue. In water, the limit of quantification for tOP and BPA was approximately 0.1 microg/l (based on 100 ml sample size).

Removal of caffeine from green tea by microwave-enhanced vacuum ice water extraction.

PubMed

Lou, Zaixiang; Er, Chaojuan; Li, Jing; Wang, Hongxin; Zhu, Song; Sun, Juntao

2012-02-24

In order to selectively remove caffeine from green tea, a microwave-enhanced vacuum ice water extraction (MVIE) method was proposed. The effects of MVIE variables including extraction time, microwave power, and solvent to solid radio on the removal yield of caffeine and the loss of total phenolics (TP) from green tea were investigated. The optimized conditions were as follows: solvent (mL) to solid (g) ratio was 10:1, microwave extraction time was 6 min, microwave power was 350 W and 2.5 h of vacuum ice water extraction. The removal yield of caffeine by MVIE was 87.6%, which was significantly higher than that by hot water extraction, indicating a significant improvement of removal efficiency. Moreover, the loss of TP of green tea in the proposed method was much lower than that in the hot water extraction. After decaffeination by MVIE, the removal yield of TP tea was 36.2%, and the content of TP in green tea was still higher than 170 mg g(-1). Therefore, the proposed microwave-enhanced vacuum ice water extraction was selective, more efficient for the removal of caffeine. The main phenolic compounds of green tea were also determined, and the results indicated that the contents of several catechins were almost not changed in MVIE. This study suggests that MVIE is a new and good alternative for the removal of caffeine from green tea, with a great potential for industrial application. Copyright © 2011 Elsevier B.V. All rights reserved.

Metabolite extraction from adherently growing mammalian cells for metabolomics studies: optimization of harvesting and extraction protocols.

PubMed

Dettmer, Katja; Nürnberger, Nadine; Kaspar, Hannelore; Gruber, Michael A; Almstetter, Martin F; Oefner, Peter J

2011-01-01

Trypsin/ethylenediaminetetraacetic acid (EDTA) treatment and cell scraping in a buffer solution were compared for harvesting adherently growing mammalian SW480 cells for metabolomics studies. In addition, direct scraping with a solvent was tested. Trypsinated and scraped cell pellets were extracted using seven different extraction protocols including pure methanol, methanol/water, pure acetone, acetone/water, methanol/chloroform/water, methanol/isopropanol/water, and acid-base methanol. The extracts were analyzed by GC-MS after methoximation/silylation and derivatization with propyl chloroformate, respectively. The metabolic fingerprints were compared and 25 selected metabolites including amino acids and intermediates of energy metabolism were quantitatively determined. Moreover, the influence of freeze/thaw cycles, ultrasonication and homogenization using ceramic beads on extraction yield was tested. Pure acetone yielded the lowest extraction efficiency while methanol, methanol/water, methanol/isopropanol/water, and acid-base methanol recovered similar metabolite amounts with good reproducibility. Based on overall performance, methanol/water was chosen as a suitable extraction solvent. Repeated freeze/thaw cycles, ultrasonication and homogenization did not improve overall metabolite yield of the methanol/water extraction. Trypsin/EDTA treatment caused substantial metabolite leakage proving it inadequate for metabolomics studies. Gentle scraping of the cells in a buffer solution and subsequent extraction with methanol/water resulted on average in a sevenfold lower recovery of quantified metabolites compared with direct scraping using methanol/water, making the latter one the method of choice to harvest and extract metabolites from adherently growing mammalian SW480 cells.

Waterbodies Extraction from LANDSAT8-OLI Imagery Using Awater Indexs-Guied Stochastic Fully-Connected Conditional Random Field Model and the Support Vector Machine

NASA Astrophysics Data System (ADS)

Wang, X.; Xu, L.

2018-04-01

One of the most important applications of remote sensing classification is water extraction. The water index (WI) based on Landsat images is one of the most common ways to distinguish water bodies from other land surface features. But conventional WI methods take into account spectral information only form a limited number of bands, and therefore the accuracy of those WI methods may be constrained in some areas which are covered with snow/ice, clouds, etc. An accurate and robust water extraction method is the key to the study at present. The support vector machine (SVM) using all bands spectral information can reduce for these classification error to some extent. Nevertheless, SVM which barely considers spatial information is relatively sensitive to noise in local regions. Conditional random field (CRF) which considers both spatial information and spectral information has proven to be able to compensate for these limitations. Hence, in this paper, we develop a systematic water extraction method by taking advantage of the complementarity between the SVM and a water index-guided stochastic fully-connected conditional random field (SVM-WIGSFCRF) to address the above issues. In addition, we comprehensively evaluate the reliability and accuracy of the proposed method using Landsat-8 operational land imager (OLI) images of one test site. We assess the method's performance by calculating the following accuracy metrics: Omission Errors (OE) and Commission Errors (CE); Kappa coefficient (KP) and Total Error (TE). Experimental results show that the new method can improve target detection accuracy under complex and changeable environments.

Ultrathin-shell boron nitride hollow spheres as sorbent for dispersive solid-phase extraction of polychlorinated biphenyls from environmental water samples.

PubMed

Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Chen, Fan; Wu, Chi-Man Lawrence; Zhao, Rusong; Cheng, Chuange

2014-11-21

Boron nitride hollow spheres with ultrathin-shells were synthesized and used as sorbents for dispersive solid-phase extraction of aromatic pollutants at trace levels from environmental water samples. Polychlorinated biphenyls (PCBs) were selected as target compounds. Sample quantification and detection were performed by gas chromatography-tandem mass spectrometry. Extraction parameters influencing the extraction efficiency were optimized through response surface methodology using the Box-Behnken design. The proposed method achieved good linearity within the concentration range of 0.15-250 ng L(-1) PCBs, low limits of detection (0.04-0.09 ng L(-1), S/N=3:1), good repeatability of the extractions (relative standard deviation, <12%, n=6), and satisfactory recoveries between 84.9% and 101.0% under optimal conditions. Real environmental samples collected from rivers, local lakes, rain and spring waters were analyzed using the developed method. Results demonstrated that the hexagonal boron nitride-based material has significant potential as a sorbent for organic pollutant extraction from environmental water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

The effect of different conventional methods of extraction on Marantodes pumila var. pumila leaves in relation to free radical scavenging activity

NASA Astrophysics Data System (ADS)

Hamid, Noor Huda Abd; Latip, Jalifah; Markom, Masturah

2018-04-01

Marantodes pumila is one of the important herbs used in traditional medicine. However, there is no report on the optimum method for the preparation of M. pumila extract enriched with bioactive compounds. Therefore, this study aim to establish the suitable method in the preparation of M. pumila extracts enriched with antioxidative compounds. Different conventional extraction methods such as maceration, reflux and Soxhlet in solvents of different polarities i.e. ethanol, 50 % aqueous ethanol and water were employed to prepare extracts. Constituents of each extract were profiled using RP-HPLC followed by the free radical scavenging assay using 2,2 diphenyl-1-picrylhydrazyl (DPPH) to determine the antioxidant activity. Among all extraction methods, maceration in 50 % aqueous ethanol gave the highest total percentage yield (22.41 %) while all extraction methods were able to extract the marker compounds, gallic acid (GA) and methyl gallate (MGA). The free radical scavenging activity of extracts varied from IC50 11.93 µg/mL (50 % aqueous ethanol via reflux) to 64.15 µg/mL (water via maceration). All extracts showed better scavenging activity as compared to synthetic antioxidant, BHT. The variation in the IC50 values is expected due to the presence of different types and/or concentration of bioactive compounds in each extract. This study may provide a preliminary insight for the preparation of standardized extracts of M. pumila enriched with bioactive compounds.

A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extraction and gas chromatography-ion trap mass spectrometry

USGS Publications Warehouse

Hladik, M.L.; Smalling, K.L.; Kuivila, K.M.

2008-01-01

A method was developed for the analysis of over 60 pesticides and degradates in water by HLB solid-phase extraction and gas-chromatography/mass spectrometry. Method recoveries and detection limits were determined using two surface waters with different dissolved organic carbon (DOC) concentrations. In the lower DOC water, recoveries and detection limits were 80%-108% and 1-12 ng/L, respectively. In the higher DOC water, the detection limits were slightly higher (1-15 ng/L). Additionally, surface water samples from four sites were analyzed and 14 pesticides were detected with concentrations ranging from 4 to 1,200 ng/L. ?? 2008 Springer Science+Business Media, LLC.

Antioxidant and antibacterial activity of Thai medicinal plant (Capparis micracantha)

NASA Astrophysics Data System (ADS)

Laoprom, Nonglak; Sangprom, Araya; Chaisri, Patcharaporn

2018-04-01

This work aims to study the antioxidants capacity, Total phenolic content and antibacterial activity of Thai medicinal plant for the treatment of dermatitis-related inflammations, Capparis micracantha. Crude extract from stem of Thai medicinal plant was extracted with hexane, ethyl acetate, methanol and water. The antioxidant activities (IC50) was evaluated with 1,1-diphenyl-1-princylhydrazyl (DPPH) radical scavenging assay. Total phenolic content (TPC) was determined by using Folin-Ciocalteu method. Bacterial activities was tested with four human pathogenic bacteria; Escherichia coli, Listeria monocytogenes, Staphylococcus aureus and Stapylococcus epidermidis by using agar diffusion assay. Minimum Inhibition Concentration (MIC) and Minimum Bactericidal Concentration (MBC) were also determined by broth dilution method. For antioxidant activity, the methanol fraction from stem extract showed the highest activity with an IC50 of 2.4 mg/ml. Water extraction was the high TPC with 10,136.9 mg GAE/g dry weight. Methanol and water extraction showed the remarkable inhibition of bacterial growth was shown against L. monocytogenes and S. aureus. In addition, ethyl acetate, methanol and water fraction from stem extract against S. epidermidis. The present finding suggests that the extract of C. micracantha could be used to discover bioactive natural products that may serve as pharmaceutical products.

Extracting organic matter on Mars: A comparison of methods involving subcritical water, surfactant solutions and organic solvents

NASA Astrophysics Data System (ADS)

Luong, Duy; Court, Richard W.; Sims, Mark R.; Cullen, David C.; Sephton, Mark A.

2014-09-01

The first step in many life detection protocols on Mars involves attempts to extract or isolate organic matter from its mineral matrix. A number of extraction options are available and include heat and solvent assisted methods. Recent operations on Mars indicate that heating samples can cause the loss or obfuscation of organic signals from target materials, raising the importance of solvent-based systems for future missions. Several solvent types are available (e.g. organic solvents, surfactant based solvents and subcritical water extraction) but a comparison of their efficiencies in Mars relevant materials is missing. We have spiked the well characterised Mars analogue material JSC Mars-1 with a number of representative organic standards. Extraction of the spiked JSC Mars-1 with the three solvent methods provides insights into the relative efficiency of these methods and indicates how they may be used on future Mars missions.

Ultrasonic-energy enhance the ionic liquid-based dual microextraction to preconcentrate the lead in ground and stored rain water samples as compared to conventional shaking method.

PubMed

Nizamani, Sooraj; Kazi, Tasneem G; Afridi, Hassan I

2018-01-01

An efficient preconcentration technique based on ultrasonic-assisted ionic liquid-based dual microextraction (UA-ILDµE) method has been developed to preconcentrate the lead (Pb +2 ) in ground and stored rain water. In the current proposed method, Pb +2 was complexed with a chelating agent (dithizone), whereas an ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was used for extraction purpose. The ultrasonic irradiation and electrical shaking system were applied to enhance the dispersion and extraction of Pb +2 complex in aqueous samples. For second phase, dual microextraction (DµE phase), the enriched Pb +2 complex in ionic liquid, extracted back into the acidic aqueous solution and finally determined by flame atomic absorption spectrometry. Some major analytical parameters that influenced the extraction efficiency of developed method, such as pH, concentration of ligand, volume of ionic liquid and samples, time of shaking in thermostatic electrical shaker and ultrasonic bath, effect of back extracting HNO 3 volume, matrix effect, centrifugation time and rate were optimized. At the sample volume of 25mL, the calculated preconcentration factor was 62.2. The limit of detection of proposed procedure for Pb +2 ions was found to be 0.54μgL -1 . The validation of developed method was performed by the analysis of certified sample of water SRM 1643e and standard addition method in a real water sample. The extraction recovery of Pb +2 was enhanced≥2% with shaking time of 80s in ultrasonic bath as compared to used thermostatic electrical shaker, where for optimum recovery up to 10min was required. The developed procedure was successfully used for the enrichment of Pb +2 in ground and stored rain water (surface water) samples of an endemic region of Pakistan. The resulted data indicated that the ground water samples were highly contaminated with Pb +2 , while some of the surface water samples were also have higher values of Pb +2 than permissible limit of WHO. The concentration of Pb +2 in surface and ground water samples was found in the range of 17.5-24.5 and 25.6-99.1μgL - 1 respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Extraction of Polysaccharide from Spirulina and Evaluation of Its Activities.

PubMed

Wang, Bingyue; Liu, Qian; Huang, Yinghong; Yuan, Yueling; Ma, Qianqian; Du, Manling; Cai, Tiange; Cai, Yu

2018-01-01

Polysaccharide of Spirulina platensis (PSP) is a kind of water-soluble polysaccharide extracted from Spirulina platensis . It has been proved to have antitumor, antioxidation, antiaging, and antivirus properties. And it has a promising prospect for wide application. This study aims to identify an extraction process for high-purity polysaccharide in Spirulina (PSP) through a series of optimization methods and then evaluates its initial antiaging activities. Four kinds of extraction methods-hot-water extraction, alkali extraction, ultrasonic-assisted extraction, and freeze-thaw extraction-were compared to find the optimal one, which was further optimized by response surface methodology. PSP was obtained after the crude PSP was deproteinized and depigmented. The antiaging effects of PSP were preliminarily evaluated through in vitro cell experiments. The alkali extraction method was determined as the optimal method, with the optimized extraction process consisting of a solid-liquid ratio of 1 : 50, a pH value of 10.25, a temperature of 89.24°C, and a time of 9.99 h. The final PSP contained 71.65% of polysaccharide and 8.54% of protein. At a concentration of 50  μ g/mL, PSP exerted a significant promoting effect on the proliferation and traumatic fusion of human immortalized epidermal cells HaCaT. An extraction method for high-purity PSP with a high extraction rate was established, and in vitro results suggest antioxidation and antiaging activities.

Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

USGS Publications Warehouse

Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn

2000-01-01

A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

Alternative oil extraction methods from Echium plantagineum L. seeds using advanced techniques and green solvents.

PubMed

Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

2018-04-01

The edible oil processing industry involves large losses of organic solvent into the atmosphere and long extraction times. In this work, fast and environmentally friendly alternatives for the production of echium oil using green solvents are proposed. Advanced extraction techniques such as Pressurized Liquid Extraction (PLE), Microwave Assisted Extraction (MAE) and Ultrasound Assisted Extraction (UAE) were evaluated to efficiently extract omega-3 rich oil from Echium plantagineum seeds. Extractions were performed with ethyl acetate, ethanol, water and ethanol:water to develop a hexane-free processing method. Optimal PLE conditions with ethanol at 150 °C during 10 min produced a very similar oil yield (31.2%) to Soxhlet using hexane for 8 h (31.3%). UAE optimized method with ethanol at mild conditions (55 °C) produced a high oil yield (29.1%). Consequently, advanced extraction techniques showed good lipid yields and furthermore, the produced echium oil had the same omega-3 fatty acid composition than traditionally extracted oil. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effects of extraction methods on the yield, chemical structure and anti-tumor activity of polysaccharides from Cordyceps gunnii mycelia.

PubMed

Zhu, Zhen-Yuan; Dong, Fengying; Liu, Xiaocui; Lv, Qian; YingYang; Liu, Fei; Chen, Ling; Wang, Tiantian; Wang, Zheng; Zhang, Yongmin

2016-04-20

This study was to investigate the effects of different extraction methods on the yield, chemical structure and antitumor activity of polysaccharides from Cordyceps gunnii (C. gunnii) mycelia. Five extraction methods were used to extract crude polysaccharides (CPS), which include room-temperature water extraction (RWE), hot-water extraction (HWE), microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and cellulase-assisted extraction (CAE). Then Sephadex G-100 was used for purification of CPS. As a result, the antitumor activities of CPS and PPS on S180 cells were evaluated. Five CPS and purified polysaccharides (PPS) were obtained. The yield of CPS by microwave-assisted extraction (CPSMAE) was the highest and its anti-tumor activity was the best and its macromolecular polysaccharide (3000-1000kDa) ratio was the largest. The PPS had the same monosaccharide composition, but their obvious difference was in the antitumor activity and the physicochemical characteristics, such as intrinsic viscosity, specific rotation, scanning electron microscopy and circular dichroism spectra. Copyright © 2015 Elsevier Ltd. All rights reserved.

A sensitive gas chromatographic-tandem mass spectrometric method for detection of alkylating agents in water: application to acrylamide in drinking water, coffee and snuff.

PubMed

Pérez, Hermes Licea; Osterman-Golkar, Siv

2003-08-01

A sensitive analytical method for the analysis of acrylamide and other electrophilic agents in water has been developed. The amino acid L-valine served as a nucleophilic trapping agent. The method was applied to the analysis of acrylamide in 0.2-1 mL samples of drinking water or Millipore-filtered water, brewed coffee, or water extracts of snuff. The reaction product, N-(2-carbamoylethyl)valine, was incubated with pentafluorophenyl isothiocyanate to give a pentafluorophenylthiohydantoin (PFPTH) derivative. This derivative was extracted with diethyl ether, separated from excess reagent and impurities by a simple extraction procedure, and analyzed by gas chromatography-tandem mass spectrometry. (2H3)Acrylamide, added before the reaction with L-valine, was used as internal standard. Acrylamide and the related compound, N-methylolacrylamide, gave the same PFPTH derivative. The concentrations of acrylamides were < or = 0.4 nmol L(-1) (< or = 0.03 microg acrylamide L(-1)) in water, 200 to 350 nmol L(-1) in brewed coffee, and 10 to 34 nmol g(-1) snuff in portion bags, respectively. The precision (the coefficient of variation was 5%) and accuracy of the method were good. The detection limit was considerably lower than that of previously published methods for the analysis of acrylamide.

Simultaneous Microwave Extraction and Separation of Volatile and Non-Volatile Organic Compounds of Boldo Leaves. From Lab to Industrial Scale

PubMed Central

Petigny, Loïc; Périno, Sandrine; Minuti, Matteo; Visinoni, Francesco; Wajsman, Joël; Chemat, Farid

2014-01-01

Microwave extraction and separation has been used to increase the concentration of the extract compared to the conventional method with the same solid/liquid ratio, reducing extraction time and separate at the same time Volatile Organic Compounds (VOC) from non-Volatile Organic Compounds (NVOC) of boldo leaves. As preliminary study, a response surface method has been used to optimize the extraction of soluble material and the separation of VOC from the plant in laboratory scale. The results from the statistical analysis revealed that the optimized conditions were: microwave power 200 W, extraction time 56 min and solid liquid ratio of 7.5% of plants in water. Lab scale optimized microwave method is compared to conventional distillation, and requires a power/mass ratio of 0.4 W/g of water engaged. This power/mass ratio is kept in order to upscale from lab to pilot plant. PMID:24776762

Kinetics of the water/air phase transition of radon and its implication on detection of radon-in-water concentrations: practical assessment of different on-site radon extraction methods.

PubMed

Schubert, Michael; Paschke, Albrecht; Bednorz, Denise; Bürkin, Walter; Stieglitz, Thomas

2012-08-21

The on-site measurement of radon-in-water concentrations relies on extraction of radon from the water followed by its detection by means of a mobile radon-in-air monitor. Many applications of radon as a naturally occurring aquatic tracer require the collection of continuous radon concentration time series, thus necessitating the continuous extraction of radon either from a permanent water stream supplied by a water pump or directly from a water body or a groundwater monitoring well. Essentially, three different types of extraction units are available for this purpose: (i) a flow-through spray chamber, (ii) a flow-through membrane extraction module, and (iii) a submersible (usually coiled) membrane tube. In this paper we discuss the advantages and disadvantages of these three methodical approaches with particular focus on their individual response to instantaneously changing radon-in-water concentrations. After a concise introduction into theoretical aspects of water/air phase transition kinetics of radon, experimental results for the three types of extraction units are presented. Quantitative suggestions for optimizing the detection setup by increasing the water/air interface and by reducing the air volume circulating through the degassing unit and radon detector are made. It was shown that the flow-through spray chamber and flow-through membrane perform nearly similarly, whereas the submersible membrane tubing has a significantly larger delay in response to concentration changes. The flow-through spray chamber is most suitable in turbid waters and to applications where high flow rates of the water pump stream can be achieved (e.g., where the power supply is not constrained by field conditions). The flow-through membrane is most suited to radon extraction from clear water and in field conditions where the power supply to a water pump is limited, e.g., from batteries. Finally, the submersible membrane tube is most suitable if radon is to be extracted in situ without any water pumping, e.g., in groundwater wells with a low yield, or in long-term time series, in which short-term variations in the radon concentration are of no relevance.

GPR-Based Water Leak Models in Water Distribution Systems

PubMed Central

Ayala-Cabrera, David; Herrera, Manuel; Izquierdo, Joaquín; Ocaña-Levario, Silvia J.; Pérez-García, Rafael

2013-01-01

This paper addresses the problem of leakage in water distribution systems through the use of ground penetrating radar (GPR) as a nondestructive method. Laboratory tests are performed to extract features of water leakage from the obtained GPR images. Moreover, a test in a real-world urban system under real conditions is performed. Feature extraction is performed by interpreting GPR images with the support of a pre-processing methodology based on an appropriate combination of statistical methods and multi-agent systems. The results of these tests are presented, interpreted, analyzed and discussed in this paper.

Simultaneous detection of nine cyanotoxins in drinking water using dual solid-phase extraction and liquid chromatography-mass spectrometry.

PubMed

Yen, Hung-Kai; Lin, Tsair-Fuh; Liao, Pao-Chi

2011-08-01

A solid-phase extraction (SPE)-liquid chromatography (LC)-mass spectrometry (MS) method was developed to concentrate and detect nine cyanotoxins simultaneously, including six microcystins (MCs) congeners, nodularin (NOD), anatoxin-a (ATX) and cylindrospermopsin (CYN), in pure and natural waters. A dual cartridge SPE assembly was tested for the operating parameters of cyanotoxin extraction. A surrogate standard (SS), 1,9-diaminononane, was spiked in all the samples before the SPE extraction, and an internal standard (IS), 2,3,5-trimethylphenyl methyl carbamate, was spiked before LC/MS analysis. The method detection limit (MDL) was 2-100 ng/L for nine cyanotoxins in pure water and was increased by a factor of three to ten in a more complicated water matrix. The recoveries based on SS were between 83 and 104%, while those based on IS were 80-120%. The developed method was successfully employed in analyzing 33 water samples collected from eutrophic lakes, water treatment plants and distribution taps. MCs, NOD, and CYN were detected in the reservoir water, with concentrations as high as 36 μg/L. In addition, for the first time in Taiwan's tap water, CYN was detected at concentrations as high as 8.6 μg/L. Quality control data for the field samples shows that the analytical scheme developed is appropriate for monitoring cyanotoxins. Copyright © 2011 Elsevier Ltd. All rights reserved.

Application of liquid-liquid-liquid microextraction and high-performance liquid chromatography for the determination of alkylphenols and bisphenol-A in water.

PubMed

Lin, Che-Yi; Fuh, Ming-Ren; Huang, Shang-Da

2011-02-01

A method termed liquid-liquid-liquid microextraction (LLLME) was utilized to extract 4-t-butylphenol, 4-t-octylphenol, 4-n-nonylphenol, and bisphenol-A from water. The extracted target analytes were separated and quantified by high-performance liquid chromatography using a fluorescence detector. In LLLME, the donor phase (i.e. water sample) was made weakly acidic by adding monobasic potassium phosphate (KH(2) PO(4)); the organic phase adopted was 4-chlorotoluene; the acceptor phase (i.e. enriched extract) was 0.2 M tetraethylammonium hydroxide dissolved in ethylene glycol. This study solves a problem associated with the surface activity of long-chain alkylphenolate ions, permitting LLLME to extract long-chain alkylphenols. Experimental conditions such as acceptor phase composition, organic phase identity, acceptor phase volume, sample agitation, extraction time, and salt addition were optimized. The relative standard deviation (RSD, 2.0-5.8%), coefficient of determination (r(2) 0.9977-0.9999), and detection limit (0.017-0.0048 ng/mL) of the proposed method were achieved under the selected optimized conditions. The method was successfully applied to analyses of lake and tap water samples, and the relative recoveries of target analytes from the spiked lake and tap water samples were 92.8-106.3 and 93.6-105.6%, respectively. The results obtained with the proposed method confirm this microextraction technique to be reliable for the monitoring of alkylphenols and bisphenol-A in water samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of Two Methods for Determination of Strontium Isotopes in Pore Water at Yucca Mountain, Nevada

NASA Astrophysics Data System (ADS)

Marshall, B. D.; Futa, K.; Scofield, K. M.

2002-12-01

The proposed radioactive waste repository at Yucca Mountain, Nevada would be constructed in the high-silica rhyolite member of the Topopah Spring Tuff, an ash-flow tuff within the ~500-m-thick unsaturated zone. Dry-drilled rock cores from this unit have been packaged to preserve their water content. Two methods have been used to extract the strontium contained in the pore water for isotopic measurements. In the first method, samples of dried core were crushed, and the 0.25 to 2.4 mm size fractions were leached with ultra-pure water for about 1 hour to dissolve the salts left behind by the evaporated pore water. Concentrations of strontium in the pore water were calculated from determinations of porosity and saturation on adjacent core and the measured strontium concentration in the leachate. In the second method, pore water was extracted from sealed core using an ultracentrifuge, minimizing evaporation of water from the core at all steps in the process. The centrifugation of 150 to 200 g of welded tuff at 15,000 rpm for 6 hours typically results in the recovery of as much as 3 ml of pore water for analysis. Strontium isotope compositions were determined by thermal ionization mass spectrometry; 87Sr /86Sr ratios have a reproducibility of 0.00005. The ranges of 87Sr/86Sr ratios determined by the two methods are identical: 0.71215 to 0.71267 in the leachates (n = 35) and 0.71214 to 0.71266 in the extracted pore waters (n = 21). However, the calculated strontium concentrations in the leachates average 300 μg/L, whereas those in the extracted pore water average 1440 μg/L, indicating that a substantial portion of the pore-water salts remain in the crushed rock after leaching. The strontium data determined on extracted pore water shows that the leaching of pore-water salts results in accurate 87Sr/86Sr, but that a substantial correction to the strontium concentration is required due to the inefficiency of the leaching procedure and the small pore sizes in the welded tuffs. The strontium isotope data obtained on leachates can be used to constrain models of water-rock interaction and estimates of travel times in the unsaturated zone.

Method development for the analysis of organophosphate and pyrethroid insecticides at low parts per trillion levels in water.

PubMed

Wang, Dongli; Weston, Donald P; Lydy, Michael J

2009-06-15

In the current study, organophosphate and pyrethroid insecticides including diazinon, chlorpyrifos, bifenthrin, fenpropathrin, permethrin, lambda-cyhalothrin, cyfluthrin, cypermethrin, esfenvalerate and deltamethrin were analyzed in laboratory and field-collected water samples. Water samples were extracted and analyzed by gas chromatography/electron capture detector (GC/ECD) and gas chromatography/nitrogen-phosphorous detector (GC/NPD). Comparison of results from liquid-liquid extraction and subsequent normal phase solid-phase extraction cleanup (LLE-NPSPE), and reversed phase solid-phase extraction (RPSPE) showed that LLE-NPSPE was the better choice to extract trace amounts of pesticides from water. Pesticide recoveries from four spiked water samples using LLE-NPSPE ranged from 63.2 to 148.8% at four spiking concentrations. Method detection limits were 0.72-1.69 ng/L using four different water sources. The stability of the target pesticides in lake water was investigated at 4 degrees C for 1h, 1d, 4d, and 7d under three conditions: (1) water samples only; (2) with 20 mL hexane used as a keeper solvent; and (3) with acidification to pH 2 with HCl. Results showed that water storage without treatment resulted in slow degradation of some pesticides with storage time, storage using water acidification led to significant degradation and loss of diazinon and chlorpyrifos, while water storage with hexane as a keeper solvent showed good stability for all of the target pesticides over the 7d storage period.

Emerging organic pollutants in the vadose zone of a soil aquifer treatment system: Pore water extraction using positive displacement.

PubMed

Sopilniak, Alexander; Elkayam, Roy; Rossin, Anna Voloshenko; Lev, Ovadia

2018-01-01

Trace organic compounds in effluents, water streams and aquifers are amply reported. However, the mobile pool of Emerging Organic Contaminants (EOCs) in the deep parts of the vadose zone is hard to estimate, due to difficulties in extraction of sufficient quantity of pore water. Here, we present a new methodology for depth profiling of EOCs in pore water by Positive Displacement Extraction (PDE): Pore water extraction from unsaturated soil samples is carried out by withdrawal of soil cores by direct-push drilling and infiltrating the core by organics free water. We show that EOC concentrations in the water eluted in the plateau region of the inverse breakthrough curve is equal to their pore water concentrations. The method was previously validated for DOC extraction, and here the scope of the methodology is extended to pore water extraction for organic pollutants analysis. Method characteristics and validation were carried out with atrazine, simazine, carbamazepine, venlafaxine, O-desmethylvenlafaxine and caffeine in the concentration range of several ng to several μg/liter. Validation was carried out by laboratory experiments on three different soils (sandy, sandy-clayey and clayey). Field studies in the vadose zone of a SAT system provided 27 m deep EOC profiles with less than 1.5 m spatial resolution. During the percolation treatment, carbamazepine remained persistent, while the other studied EOCs were attenuated to the extent of 50-99%.The highest degradation rate of all studied EOCs was in the aerobic zone. EOC levels based on PDE and extraction by centrifugation were compared, showing a positive bias for centrifugation. Copyright © 2017 Elsevier Ltd. All rights reserved.

Ultra-trace analysis of furanic compounds in transformer/rectifier oils with water extraction and high-performance liquid chromatography.

PubMed

Lin, Monica; Lin, Kham; Lin, Amanda; Gras, Ronda; Luong, Jim

2016-07-01

A novel approach for the determination of parts-per-billion level of 5-hydroxymethyl-2-furaldehyde, furfuryl alcohol, furfural, 2-furyl methyl ketone, and 5-methylfurfural in transformer or rectifier oils has been successfully innovated and implemented. Various extraction methods including solid-phase extraction, liquid-liquid extraction using methanol, acetonitrile, and water were studied. Water was by far the most efficient solvent for use as an extraction medium. Separation of the analytes was conducted using a 4.6 mm × 250 mm × 3.5 μm Agilent Zorbax column while detection and quantitation were conducted with a variable wavelength UV detector. Detection limits of all furans were at 1 ppb v/v with linear ranges range from 5 to 1000 ppb v/v with correlation coefficients of 0.997 or better. A relative standard deviation of at most 2.4% at 1000 ppb v/v and 7.3% at 5 ppb v/v and a recovery from 43% to 90% depending on the analyte monitored were obtained. The method was purposely designed to be environmental friendly with water as an extraction medium. Also, the method uses 80% water and 20% acetonitrile with a mere 0.2 mL/min of acetonitrile in an acetonitrile/water mixture as mobile phase. The analytical technique has been demonstrated to be highly reliable with low cost of ownership, suitable for deployment in quality control labs or in regions where available analytical resources and solvents are difficult to procure. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid chromatographic determination of the cyanobacterial toxin beta-n-methylamino-L-alanine in algae food supplements, freshwater fish, and bottled water.

PubMed

Scott, Peter M; Niedzwiadek, Barbara; Rawn, Dorothea F K; Lau, Ben P-Y

2009-08-01

Beta-N-Methylamino-L-alanine (BMAA) is a neurotoxin originally found in cycad seeds and now known to be produced by many species of freshwater and marine cyanobacteria. We developed a method for its determination in blue-green algae (BGA) food supplements, freshwater fish, and bottled water by using a strong cation-exchange, solid-phase extraction column for cleanup after 0.3 M trichloroacetic acid extraction of BGA supplements and fish. Bottled water was applied directly onto the solid-phase extraction column. For analysis of carbonated water, sonication and pH adjustment to 1.5 were needed. To determine protein-bound BMAA, the protein pellet left after extraction of the BGA supplement and fish was hydrolyzed by boiling with 6 M hydrochloric acid; BMAA was cleaned up on a C18 column and a strong cation-exchange, solid-phase extraction column. Determination of BMAA was by liquid chromatography of the fluorescent derivative formed with 9-fluorenylmethyl chloroformate. The method was validated by recovery experiments using spiking levels of 1.0 to 10 microg/g for BGA supplements, 0.5 to 5.0 microg/g for fish, and 0.002 microg/g for bottled water; mean recoveries were in the range of 67 to 89% for BGA supplements and fish, and 59 to 92% for bottled water. Recoveries of BMAA from spiked extracts of hydrolyzed protein from BGA supplements and fish ranged from 66 to 83%. The cleanup developed provides a useful method for surveying foods and supplements for BMAA and protein-bound BMAA.

Determination of trace metals in drinking water using solid-phase extraction disks and X-ray fluorescence spectrometry.

PubMed

Hou, Xiandeng; Peters, Heather L; Yang, Zheng; Wagner, Karl A; Batchelor, James D; Daniel, Meredith M; Jones, Bradley T

2003-03-01

A convenient method is described for monitoring Cd, Ni, Cu, and Pb at trace levels in drinking water samples. These metals are preconcentrated on a chelating solid-phase extraction disk and then determined by X-ray fluorescence spectrometry. The method tolerates a wide pH range (pH 6-14) and a large amount of alkaline and alkaline earth elements. The preconcentration factor is well over 1600, assuming a 1 L water sample volume. The limits of detection for Cd, Ni, Cu, and Pb are 3.8, 0.6, 0.4, and 0.3 ng/mL, respectively. These are well below the federal maximum contaminant level values, which are 5, 100, 1300, and 15 ng/mL, respectively. The proposed method has many advantages including ease of operation, multielement capability, nondestructiveness, high sensitivity, and relative cost efficiency. The solid-phase extraction step can be conducted in the field and then the disks can be mailed to a laboratory for the analysis, eliminating the cost of transporting large volumes of water samples. Furthermore, the color of the used extraction disk provides an initial estimate of the degree of contamination for some transition metals (for example, Ni and Cu). Thus, the overall cost for analysis of metals in drinking water can be minimized by implementing the method, and small water supply companies with limited budgets will be better able to comply with the Safe Drinking Water Act.

Effects of oil extraction methods on physical and chemical properties of red salmon oils (Oncorhynchus nerka)

USDA-ARS?s Scientific Manuscript database

Four different red salmon oil extraction processes were used to extract oil from red salmon heads: RS1 involved a mixture of ground red salmon heads and water, no heat treatment, and centrifugation; RS2 involved ground red salmon heads (no water added), heat treatment, and centrifugation; RS3 involv...

Two-steps extraction of essential oil, polysaccharides and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits.

PubMed

Cheng, Zhenyu; Yang, Yingjie; Liu, Yan; Liu, Zhigang; Zhou, Hongli; Hu, Haobin

2014-08-05

A method for two-steps extraction of essential oil, polysaccharides and lignans from Schisandra chinensis Baill had been established. Firstly, S. chinensis was extracted by hydro-distillation, the extracted solution was separated from the water-insoluble residue and precipitated by adding dehydrated alcohol after the essential oil was collected, and then the precipitate as polysaccharide was collected. Finally, second extraction was performed to obtained lignans from the water-insoluble residue with ultrasonic-microwave assisted extraction (UMAE) method. Response surface methodology was employed to optimize the UMAE parameters, the optimal conditions were as follows: microwave power 430W, ethanol concentration 84%, particle size of sample 120-mesh sieves, ratio of water to raw material 15 and extraction time 2.1min. Under these optimized conditions, the total extraction yields of five lignans (Schisandrol A, Schisantherin A, Deoxyschisandrin, Schisandrin B and Schisandrin C) had reached 14.22±0.135mg/g. Compared with the traditional method of direct extraction of different bioactive components in respective procedure, the extraction yields of polysaccharides and the five lignans had reached 99% and 95%, respectively. The mean recoveries of the 5 lignan compounds and polysaccharides were 97.75-101.08% and their RSD value was less than 3.88%.The approach proposed in this study not only improved the extraction yield of lignans, but also elevated the utilization of Schisandra resources. Copyright © 2014 Elsevier B.V. All rights reserved.

Mixed functional monomers-based monolithic adsorbent for the effective extraction of sulfonylurea herbicides in water and soil samples.

PubMed

Pei, Miao; Zhu, Xiangyu; Huang, Xiaojia

2018-01-05

Effective extraction is a key step in the determination of sulfonylurea herbicides (SUHs) in complicated samples. According to the chemical properties of SUHs, a new monolithic adsorbent utilizing acrylamidophenylboronic acid and vinylimidazole as mixed functional monomers was synthesized. The new adsorbent was employed as the extraction phase of multiple monolithic fiber solid-phase microextraction (MMF-SPME) of SUHs, and the extracted SUHs were determined by high-performance liquid chromatography with diode array detection (HPLC-DAD). Results well evidence that the prepared adsorbent could extract SUHs in environmental waters and soil effectively through multiply interactions such as boronate affinity, dipole-dipole and π-π interactions. Under the optimized extraction conditions, the limits of detection for target SUHs in environmental water and soil samples were 0.018-0.17μg/L and 0.14-1.23μg/kg, respectively. At the same time, the developed method also displayed some analytical merits including wide linear dynamic ranges, good method reproducibility, satisfactory sensitivity and low consume of organic solvent. Finally, the developed were successfully applied to monitor trace SUHs in environmental water and soil samples. The recoveries at three fortified concentrations were in the range of 70.6-119% with RSD below 11% in all cases. The obtained results well demonstrate the excellent practical applicability of the developed MMF-SPME-HPLC-DAD method for the monitoring of SUHs in water and soil samples. Copyright © 2017 Elsevier B.V. All rights reserved.

[Determination of biphenyl ether herbicides in water using HPLC with cloud-point extraction].

PubMed

He, Cheng-Yan; Li, Yuan-Qian; Wang, Shen-Jiao; Ouyang, Hua-Xue; Zheng, Bo

2010-01-01

To determine residues of multiple biphenyl ether herbicides simultaneously in water using high performance liquid chromatography (HPLC) with cloud-point extraction. The residues of eight biphenyl ether herbicides (including bentazone, fomesafen, acifluorfen, aclonifen, bifenox, fluoroglycofenethy, nitrofen, oxyfluorfen) in water samples were extracted with cloud-point extraction of Triton X-114. The analytes were separated and determined using reverse phase HPLC with ultraviolet detector at 300 nm. Optimized conditions for the pretreatment of water samples and the parameters of chromatographic separation applied. There was a good linear correlation between the concentration and the peak area of the analytes in the range of 0.05-2.00 mg/L (r = 0.9991-0.9998). Except bentazone, the spiked recoveries of the biphenyl ether herbicides in the water samples ranged from 80.1% to 100.9%, with relative standard deviations ranging from 2.70% to 6.40%. The detection limit of the method ranged from 0.10 microg/L to 0.50 microg/L. The proposed method is simple, rapid and sensitive, and can meet the requirements of determination of multiple biphenyl ether herbicides simultaneously in natural waters.

A new method for fast extraction and determination of chlorophylls in natural water.

PubMed

Qiu, Nianwei; Wang, Xiushun; Zhou, Feng

2018-01-26

Algae collection and chlorophyll extraction are two troublesome steps in the traditional methods used for the determination of chlorophyll concentration in natural water. A new method was established in this study for fast collection and extraction of chlorophyll. Based on our results, the optimum centrifugation condition for collecting algae was determined as: 5000 g for 15 min at 4 °C, and the optimum dilution ratio of dimethyl sulfoxide: 90% acetone was 1:4. The specific steps were as follows: the algae in water samples were collected by centrifugation at 5000 g at 4 °C for 15 min. The precipitated algae were suspended with 2 mL DMSO. Then the sample was transferred to a 15 mL centrifuge tube, and the tube was incubated at 65 °C for 1-2 h in the dark until the sample turned white. After cooling, the chlorophyll extract was diluted with 8 mL 90% acetone, before centrifugation at 5000 g for 5 min. The absorbance values of the supernatants at 750, 664, 647 and 630 nm were used for the calculation of chlorophyll concentrations by the trichromatic equations. This new method saved the filter cost, simplified the extraction process, improved the algae acquisition efficiency, and accelerated the chlorophyll extraction rate.

Raft cultivation area extraction from high resolution remote sensing imagery by fusing multi-scale region-line primitive association features

NASA Astrophysics Data System (ADS)

Wang, Min; Cui, Qi; Wang, Jie; Ming, Dongping; Lv, Guonian

2017-01-01

In this paper, we first propose several novel concepts for object-based image analysis, which include line-based shape regularity, line density, and scale-based best feature value (SBV), based on the region-line primitive association framework (RLPAF). We then propose a raft cultivation area (RCA) extraction method for high spatial resolution (HSR) remote sensing imagery based on multi-scale feature fusion and spatial rule induction. The proposed method includes the following steps: (1) Multi-scale region primitives (segments) are obtained by image segmentation method HBC-SEG, and line primitives (straight lines) are obtained by phase-based line detection method. (2) Association relationships between regions and lines are built based on RLPAF, and then multi-scale RLPAF features are extracted and SBVs are selected. (3) Several spatial rules are designed to extract RCAs within sea waters after land and water separation. Experiments show that the proposed method can successfully extract different-shaped RCAs from HR images with good performance.

Development and validation of same-day monitoring methods for recreational water

EPA Pesticide Factsheets

When water is polluted, swimmers can become ill from exposure to waterborne pathogens. EPA scientists have developed a new DNA extraction method for determining the amount of pathogens present in water.

Development of Conductivity Method as an Alternative to Titration for Hydrolytic Resistance Testing Used for Evaluation of Glass Vials Used in Pharmaceutical Industry.

PubMed

Fujimori, Kiyoshi; Lee, Hans; Phillips, Joseph; Nashed-Samuel, Yasser

The European Pharmacopeia surface test to analyze the hydrolytic resistance is a common industrial method to understand and ensure the quality of produced glass vials. Hydrolytic resistance is evaluated by calculating the alkalinity of water extract from autoclaved vials by titration. As an alternative to this titration technique, a conductivity technique was assessed, which directly measures the ions in the water extract. A conductivity meter with a 12 mm diameter electrode was calibrated with a 100 μS/cm conductivity standard and carryover minimized by rinsing the probe in a water beaker per analysis. The limit of quantification at 1 μS/cm was determined as having a signal-to-noise ratio of 3 compared with the water blank. The conductivity method was selective for glass-composing elements (boron, sodium, aluminum, silicon, potassium, and calcium) within the vial extract. Accuracies of spiked conductivity standard within the range of 1 to 100 μS/cm were ±7% and had linearity with coefficient of determination (R 2 ) of ≥0.9999. Intraday precision had a relative standard deviation (RSD) (n = 5) of ≤6% for spiked conductivity standard within the range of 1 to 100 μS/cm. Interday precision had a RSD (n = 4) of ≤6% for 10 vials from three glass vial lots. Conductivity of water extracts from nine sets of seven lots of glass vials had a precise linear relationship [R 2 = 0.9876, RSD = 1% (n = 9)] with titration volumes of the same lots. Conductivity results in μS/cm could be converted to titration volumes in milliliters by a conversion factor of 0.0275. The simplicity, sample stability, and individual vial analysis of the conductivity technique were more advantageous than the current titration technique. The quality of glass vials used as primary containers in the pharmaceutical industry is of concern due to recent observations of glass flake-like delamination, or lamellae, under specific storage conditions. The current European Pharmacopoeia method to assess glass vial quality utilizes acid titration of vial extract pools to determine hydrolytic resistance or alkalinity. As an alternative to the European Pharmacopoeia method, the vial extracts were analyzed for conductivity, which directly determines the level of ions that were readily extracted from the vial surfaces. Lower quality glass would have greater surface defects that lead to higher ions extracted and higher conductivity value. The conductivity method was found to be suitable to measure the ions in water extracts and showed strong correlation with alkalinity. The advantage of the conductivity method over the alkalinity method was greater ease, lower volume requirements, stability, and flexibility in analysis. © PDA, Inc. 2017.

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.

Iodine speciation in coastal and inland bathing waters and seaweeds extracts using a sequential injection standard addition flow-batch method.

PubMed

Santos, Inês C; Mesquita, Raquel B R; Bordalo, Adriano A; Rangel, António O S S

2015-02-01

The present work describes the development of a sequential injection standard addition method for iodine speciation in bathing waters and seaweeds extracts without prior sample treatment. Iodine speciation was obtained by assessing the iodide and iodate content, the two inorganic forms of iodine in waters. For the determination of iodide, an iodide ion selective electrode (ISE) was used. The indirect determination of iodate was based on the spectrophotometric determination of nitrite (Griess reaction). For the iodate measurement, a mixing chamber was employed (flow batch approach) to explore the inherent efficient mixing, essential for the indirect determination of iodate. The application of the standard addition method enabled detection limits of 0.14 µM for iodide and 0.02 µM for iodate, together with the direct introduction of the target water samples, coastal and inland bathing waters. The results obtained were in agreement with those obtained by ICP-MS and a colorimetric reference procedure. Recovery tests also confirmed the accuracy of the developed method which was effectively applied to bathing waters and seaweed extracts. Copyright © 2014 Elsevier B.V. All rights reserved.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by graphitized carbon-based solid-phase extraction and high-performance liquid chromatography/mass spectrometry

USGS Publications Warehouse

Furlong, Edward T.; Anderson, Bruce D.; Werner, Stephen L.; Soliven, Paul P.; Coffey, Laura J.; Burkhardt, Mark R.

2001-01-01

In 1996, the U.S. Geological Survey National Water Quality Laboratory (NWQL) developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method to determine polar pesticide concentrations in surface- and ground-water samples. Subsequently, the NWQL developed a complementary analysis that uses high-performance liquid chromatography/mass spectrometry to detect, identify, and quantify polar pesticides and pesticide metabolites in filtered water at concentrations as low as 10 nanograms per liter. This new method was designed to improve sensitivity and selectivity over the prior method, and to reduce known interferences from natural organic matter.In this new method, pesticides are extracted from filtered water samples by useing a 0.5-gram graphitized carbon-based solid-phase extraction cartridge, eluted from the cartridge, and concentrations determined by using high-performance liquid chromatography with electrospray ionization-mass spectrometry. The upper concentration limit is 1.000 microgram per liter (μg/L) for most compounds. Single-operator method detection limits in organic-free water samples fortified with pesticides at a concentration of 0.025 μg/L ranged from 0.0019 to 0.022 μg/L for all compounds in the method. The grand mean (mean of mean recoveries for individual compounds) recoveries in organic-free water samples ranged from 72 to 89 percent, fortified with pesticides at three concentrations between 0.025 and 0.5 μg/L. Grand mean recoveries in ground- and surface-water samples ranged from 46 to 119 percent, also fortified with pesticides at three concentrations between 0.025 and 0.5 μg/L. Long-term recoveries from reagent water spikes were used to demonstrate that 38 of 65 compounds can be reported without qualification of the quantitative result across the analytical range of the method. The remaining 27 are reported with qualified estimates of concentration because of greater variability of recovery.

Hydrometallurgical recovery of germanium from coal gasification fly ash: pilot plant scale evaluation

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

Arroyo, F.; Fernandez-Pereira, C.; Olivares, J.

2009-04-15

In this article, a hydrometallurgical method for the selective recovery of germanium from fly ash (FA) has been tested at pilot plant scale. The pilot plant flowsheet comprised a first stage of water leaching of FA, and a subsequent selective recovery of the germanium from the leachate by solvent extraction method. The solvent extraction method was based on Ge complexation with catechol in an aqueous solution followed by the extraction of the Ge-catechol complex (Ge(C{sub 6}H{sub 4}O{sub 2}){sub 3}{sup 2-}) with an extracting organic reagent (trioctylamine) diluted in an organic solvent (kerosene), followed by the subsequent stripping of the organicmore » extract. The process has been tested on a FA generated in an integrated gasification with combined cycle (IGCC) process. The paper describes the designed 5 kg/h pilot plant and the tests performed on it. Under the operational conditions tested, approximately 50% of germanium could be recovered from FA after a water extraction at room temperature. Regarding the solvent extraction method, the best operational conditions for obtaining a concentrated germanium-bearing solution practically free of impurities were as follows: extraction time equal to 20 min; aqueous phase/organic phase volumetric ratio equal to 5; stripping with 1 M NaOH, stripping time equal to 30 min, and stripping phase/organic phase volumetric ratio equal to 5. 95% of germanium were recovered from water leachates using those conditions.« less

Toxicity of medicinal plants used in traditional medicine in Northern Peru

PubMed Central

Bussmann, R.W.; Malca, G.; Glenn, A.; Sharon, D.; Nilsen, B.; Parris, B.; Dubose, D; Ruiz, D.; Saleda, J.; Martinez, M.; Carillo, L.; Walker, K.; Kuhlman, A.; Townesmith, A.

2011-01-01

Aim The plant species reported here are traditionally used in Northern Peru for a wide range of illnesses. Most remedies are prepared as ethanol or aqueous extracts and then ingested. The aim of this study was to evaluate the potential toxicity of these extracts. Materials and methods The toxicity of ethanolic and water extracts of 341 plant species was determined using a Brine-Shrimp assay. Results Overall 24% of the species in water extract and 76% of the species in alcoholic extract showed elevated toxicity levels to brine-shrimp. Although in most cases multiple extracts of the same species showed very similar toxicity values, in some cases the toxicity of different extracts of the same species varied from non-toxic to highly toxic. Conclusions Traditional preparation methods take different toxicity levels in aqueous and ethanol extracts into account when choosing the appropriate solvent for the preparation of a remedy. PMID:21575699

A method to extract soil water for stable isotope analysis

USGS Publications Warehouse

Revesz, K.; Woods, P.H.

1990-01-01

A method has been developed to extract soil water for determination of deuterium (D) and 18O content. The principle of this method is based on the observation that water and toluene form an azeotropic mixture at 84.1??C, but are completely immiscible at ambient temperature. In a specially designed distillation apparatus, the soil water is distilled at 84.1??C with toluene and is separated quantitatively in the collecting funnel at ambient temperature. Traces of toluene are removed and the sample can be analyzed by mass spectrometry. Kerosene may be substituted for toluene. The accuracy of this technique is ?? 2 and ?? 0.2???, respectively, for ??D and ??18O. Reduced accuracy is obtained at low water contents. ?? 1990.

Method of analysis and quality-assurance practices by the U. S. Geological Survey Organic Geochemistry Research Group; determination of four selected mosquito insecticides and a synergist in water using liquid-liquid extraction and gas chrom

USGS Publications Warehouse

Zimmerman, L.R.; Strahan, A.P.; Thurman, E.M.

2001-01-01

A method of analysis and quality-assurance practices were developed for the determination of four mosquito insecticides (malathion, metho-prene, phenothrin, and resmethrin) and one synergist (piperonyl butoxide) in water. The analytical method uses liquid-liquid extraction (LLE) and gas chromatography/mass spectrometry (GC/MS). Good precision and accuracy were demonstrated in reagent water, urban surface water, and ground water. The mean accuracies as percentages of the true compound concentrations from water samples spiked at 10 and 50 nanograms per liter ranged from 68 to 171 percent, with standard deviations in concentrations of 27 nanograms per liter or less. The method detection limit for all compounds was 5.9 nanograms per liter or less for 247-milliliter samples. This method is valuable for acquiring information about the fate and transport of these mosquito insecticides and one synergist in water.

Optimization of cloud point extraction and solid phase extraction methods for speciation of arsenic in natural water using multivariate technique.

PubMed

Baig, Jameel A; Kazi, Tasneem G; Shah, Abdul Q; Arain, Mohammad B; Afridi, Hassan I; Kandhro, Ghulam A; Khan, Sumaira

2009-09-28

The simple and rapid pre-concentration techniques viz. cloud point extraction (CPE) and solid phase extraction (SPE) were applied for the determination of As(3+) and total inorganic arsenic (iAs) in surface and ground water samples. The As(3+) was formed complex with ammonium pyrrolidinedithiocarbamate (APDC) and extracted by surfactant-rich phases in the non-ionic surfactant Triton X-114, after centrifugation the surfactant-rich phase was diluted with 0.1 mol L(-1) HNO(3) in methanol. While total iAs in water samples was adsorbed on titanium dioxide (TiO(2)); after centrifugation, the solid phase was prepared to be slurry for determination. The extracted As species were determined by electrothermal atomic absorption spectrometry. The multivariate strategy was applied to estimate the optimum values of experimental factors for the recovery of As(3+) and total iAs by CPE and SPE. The standard addition method was used to validate the optimized methods. The obtained result showed sufficient recoveries for As(3+) and iAs (>98.0%). The concentration factor in both cases was found to be 40.

Efficient purification of paclitaxel from yews using high-performance displacement chromatography technique.

PubMed

Watchueng, Jean; Kamnaing, Pierre; Gao, Jin-Ming; Kiyota, Taira; Yeboah, Faustinus; Konishi, Yasuo

2011-05-20

Paclitaxel was purified using high-performance displacement chromatography (HPDC) technique, but not by the mechanism of HPDC. On small scale, paclitaxel was extracted with methanol from dry needles of Taxus canadensis and was enriched by extracting with chloroform after removing water-soluble hydrophilic components and hexane-soluble hydrophobic components. Then, 93-99% purity of paclitaxel was obtained using the HPDC technique. On large scale, taxanes were enriched by solvent partitioning between acetic acid/MeOH/H(2)O and hexane and extracted with CH(2)Cl(2). Taxanes except paclitaxel were further removed by extracting with methanol-water-trifluoroacetic acid (1.0:98.9:0.1, v/v/v). Applying HPDC technique to water-insoluble substances is problematic as this method requires a highly aqueous solvent system. In order to overcome this incompatibility, a system was set up where paclitaxel, although in low concentration, was extracted by methanol-water-trifluoroacetic acid (10.0:89.9:0.1, v/v/v). Recycling the extracting solvent to ensure minimal volume, the extracted paclitaxel was adsorbed on a C(18) trap column. A C(18) column of 4.6mm internal diameter was then connected to the trap column. The HPDC technique was thus carried out using an isocratic acetonitrile-water-trifluoroacetic acid (30.0:69.9:0.1, v/v/v) mobile phase consisting of a displacer cetylpyridinium trifluoroacetate (3mg/mL). Paclitaxel was co-eluted with the displacer and spontaneously crystallized. The crystal (114mg) showed 99.4% purity and only 10% of paclitaxel in the starting crude extract was lost during the enrichment/purification processes. This large scale purification method was successfully applied to purify paclitaxel from Chinese yew in small scale, suggesting general applicability of the method. This is the first report of purifying a water-insoluble natural product using HPDC technique. Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

Short term spatio-temporal variability of soil water-extractable calcium and magnesium after a low severity grassland fire in Lithuania.

NASA Astrophysics Data System (ADS)

Pereira, Paulo; Martin, David

2014-05-01

Fire has important impacts on soil nutrient spatio-temporal distribution (Outeiro et al., 2008). This impact depends on fire severity, topography of the burned area, type of soil and vegetation affected, and the meteorological conditions post-fire. Fire produces a complex mosaic of impacts in soil that can be extremely variable at small plot scale in the space and time. In order to assess and map such a heterogeneous distribution, the test of interpolation methods is fundamental to identify the best estimator and to have a better understanding of soil nutrients spatial distribution. The objective of this work is to identify the short-term spatial variability of water-extractable calcium and magnesium after a low severity grassland fire. The studied area is located near Vilnius (Lithuania) at 54° 42' N, 25° 08 E, 158 masl. Four days after the fire, it was designed in a burned area a plot with 400 m2 (20 x 20 m with 5 m space between sampling points). Twenty five samples from top soil (0-5 cm) were collected immediately after the fire (IAF), 2, 5, 7 and 9 months after the fire (a total of 125 in all sampling dates). The original data of water-extractable calcium and magnesium did not respected the Gaussian distribution, thus a neperian logarithm (ln) was applied in order to normalize data. Significant differences of water-extractable calcium and magnesium among sampling dates were carried out with the Anova One-way test using the ln data. In order to assess the spatial variability of water-extractable calcium and magnesium, we tested several interpolation methods as Ordinary Kriging (OK), Inverse Distance to a Weight (IDW) with the power of 1, 2, 3 and 4, Radial Basis Functions (RBF) - Inverse Multiquadratic (IMT), Multilog (MTG), Multiquadratic (MTQ) Natural Cubic Spline (NCS) and Thin Plate Spline (TPS) - and Local Polynomial (LP) with the power of 1 and 2. Interpolation tests were carried out with Ln data. The best interpolation method was assessed using the cross validation method. Cross-validation was obtained by taking each observation in turn out of the sample pool and estimating from the remaining ones. The errors produced (observed-predicted) are used to evaluate the performance of each method. With these data, the mean error (ME) and root mean square error (RMSE) were calculated. The best method was the one which had the lower RMSE (Pereira et al. in press). The results shown significant differences among sampling dates in the water-extractable calcium (F= 138.78, p< 0.001) and extractable magnesium (F= 160.66; p< 0.001). Water-extractable calcium and magnesium was high IAF decreasing until 7 months after the fire, rising in the last sampling date. Among the tested methods, the most accurate to interpolate the water-extractable calcium were: IAF-IDW1; 2 Months-IDW1; 5 months-OK; 7 Months-IDW4 and 9 Months-IDW3. In relation to water-extractable magnesium the best interpolation techniques were: IAF-IDW2; 2 Months-IDW1; 5 months- IDW3; 7 Months-TPS and 9 Months-IDW1. These results suggested that the spatial variability of these water-extractable is variable with the time. The causes of this variability will be discussed during the presentation. References Outeiro, L., Aspero, F., Ubeda, X. (2008) Geostatistical methods to study spatial variability of soil cation after a prescribed fire and rainfall. Catena, 74: 310-320. Pereira, P., Cerdà, A., Úbeda, X., Mataix-Solera, J. Arcenegui, V., Zavala, L. Modelling the impacts of wildfire on ash thickness in a short-term period, Land Degradation and Development, (In Press), DOI: 10.1002/ldr.2195

Fast trace determination of nine odorant and estrogenic chloro- and bromo-phenolic compounds in real water samples through automated solid-phase extraction coupled with liquid chromatography tandem mass spectrometry.

PubMed

Yuan, Su-Fen; Liu, Ze-Hua; Lian, Hai-Xian; Yang, Chuang-Tao; Lin, Qing; Yin, Hua; Lin, Zhang; Dang, Zhi

2018-02-01

A fast and reliable method was developed for simultaneous trace determination of nine odorous and estrogenic chloro- and bromo-phenolic compounds (CPs and BPs) in water samples using solid-phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS). For sample preparation, the extraction efficiencies of two widely applied cartridges Oasis HLB and Sep-Pak C18 were compared, and the Oasis HLB cartridge showed much better extraction performance; pH of water sample also plays important role on extraction, and pH = 2-3 was found to be most appropriate. For separation of the target compounds, small addition of ammonium hydroxide can obviously improve the detection sensitivity, and the optimized addition concentration was determined as 0.2%. The developed efficient method was validated and showed excellent linearity (R 2  > 0.995), low limit of detection (LOD, 1.9-6.2 ng/L), and good recovery efficiencies of 57-95% in surface and tap water with low relative standard deviation (RSD, 1.3-17.4%). The developed method was finally applied to one tap and one surface water samples and most of these nine targets were detected, but all of them were below their odor thresholds, and their estrogen equivalent (EEQ) were also very low.

[Determination of estrogen residues in drinking water by on-line solid phase extraction based on sol-gel technique coupled with high performance liquid chromatography].

PubMed

Li, Longfei; Su, Min; Shi, Xiaolei; Wang, Yana; Wang, Minmin; He, Jinxing

2014-02-01

A method for the determination of diethylstilbestrol (DES), hexestrol (HEX) and dienestrol (DS) residues in drinking water was established by on-line solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). The material synthesized on the base of sol-gel technology was employed as adsorbent. This material was prepared using 3-aminopropyltriethoxysilane (APTES) as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and acetic acid as the initiator. The synthesized adsorbent showed outstanding property for the estrogen extraction. The estrogen can be caught effectively from water samples and the extraction can be achieved rapidly. Some important parameters, such as pH of sample solution, eluent solvents, loading flow rate, which might influence extraction efficiency, were optimized. The results indicated that the limit of detection (S/N = 3) of the developed method could reach 0.07-0.13 microg/L under the conditions of pH 7.0 of sample solution, methanol and 1% (v/v) acetic acid aqueous solution as the eluent solvent and the loading flow rate of 2 mL/min. The recoveries of the three estrogens from the water samples at three spiked levels ranged from 82.31% to 99.43% with RSD of 1.61%-7.15%. The method was simple, rapid, and suitable to detect the trace residues of estrogens in drinking water.

Mixed hemimicelles solid-phase extraction based on sodium dodecyl sulfate (SDS)-coated nano-magnets for the spectrophotometric determination of Fingolomid in biological fluids

NASA Astrophysics Data System (ADS)

Azari, Zhila; Pourbasheer, Eslam; Beheshti, Abolghasem

2016-01-01

In this study, mixed hemimicelles solid-phase extraction (SPE) based on sodium dodecyl sulfate (SDS)-coated nano-magnets Fe3O4 was investigated as a novel method for the separation and determination of Fingolimod (FLM) in water, urine and plasma samples prior to spectrophotometeric determination. Due to the high surface area of these new sorbents and the excellent adsorption capacity after surface modification by SDS, satisfactory extraction recoveries can be produced. The main factors affecting the adsolubilization of analysts, such as pH, surfactant and adsorbent amounts, ionic strength, extraction time and desorption conditions were studied and optimized. Under the selected conditions, FLM has been quantitatively extracted. The accuracy of the method was evaluated by recovery measurements on spiked samples, and good recoveries of 96%, 95% and 88% were observed for water, urine and plasma respectively. Proper linear behaviors over the investigated concentration ranges of 2-26, 2-17 and 2-13 mg/L with good coefficients of determination, 0.998, 0.997 and 0.995 were achieved for water, urine and plasma samples, respectively. To the best of our knowledge, this is the first time that a mixed hemimicelles SPE method based on magnetic separation and nanoparticles has been used as a simple and sensitive method for monitoring of FLM in water and biological samples.

Method of removing and detoxifying a phosphorus-based substance

DOEpatents

Vandegrift, George F.; Steindler, Martin J.

1989-01-01

A method of removing organic phosphorus-based poisonous substances from water contaminated therewith and of subsequently destroying the toxicity of the substance is disclosed. Initially, a water-immiscible organic is immobilized on a supported liquid membrane. Thereafter, the contaminated water is contacted with one side of the supported liquid membrane to selectively dissolve the phosphorus-based substance in the organic extractant. At the same time, the other side of the supported liquid membrane is contacted with a hydroxy-affording strong base to react the phosphorus-based substance dissolved by the organic extractant with a hydroxy ion. This forms a non-toxic reaction product in the base. The organic extractant can be a water-insoluble trialkyl amine, such as trilauryl amine. The phosphorus-based substance can be phosphoryl or a thiophosphoryl.

Optimization of microwave assisted extraction of essential oils from Iranian Rosmarinus officinalis L. using RSM.

PubMed

Akhbari, Maryam; Masoum, Saeed; Aghababaei, Fahimeh; Hamedi, Sepideh

2018-06-01

In this study, the efficiencies of conventional hydro-distillation and novel microwave hydro-distillation methods in extraction of essential oil from Rosemary officinalis leaves have been compared. In order to attain the best yield and also highest quality of the essential oil in the microwave assisted method, the optimal values of operating parameters such as extraction time, microwave irradiation power and water volume to plant mass ratio were investigated using central composite design under response surface methodology. Optimal conditions for obtaining the maximum extraction yield in the microwave assisted method were predicted as follows: extraction time of 85 min, microwave power of 888 W, and water volume to plant mass ratio of 0.5 ml/g. The extraction yield at these predicted conditions was computed as 0.7756%. The qualities of the obtained essential oils under designed experiments were optimized based on total contents of four major compounds (α-pinene, 1,8-cineole, camphor and verbenone) which determined by gas chromatography equipped with mass spectroscopy (GC-MS). The highest essential oil quality (55.87%) was obtained at extraction time of 68 min; microwave irradiation power of 700 W; and water volume to plant mass ratio of zero.

Extraction and analysis methods for the determination of pyrethroid insecticides in surface water, sediments and biological tissues at environmentally relevant concentrations.

PubMed

Mekebri, A; Crane, D B; Blondina, G J; Oros, D R; Rocca, J L

2008-05-01

The aim of this study was to develop and validate chemical methods for measuring pyrethroid insecticides at environmentally relevant concentrations in different matrices. The analytes included six synthetic pyrethroids with the highest agricultural and commercial structural uses in California: bifenthrin, cyfluthrin, cypermethrin, esfenvalerate/fenvalerate, lambda-cyhalothrin, permethrin, and their corresponding stereoisomers, which includes enantiomers, diastereomers and racemic mixtures. Fortified water samples were extracted for analysis of synthetic pyrethroids using liquid-liquid extraction, while fortified sediment and fish tissue samples were extracted using pressurized fluid extraction followed by gel permeation chromatography (GPC) to remove matrix interferences. A florisil column was used for additional cleanup and fractionation of sediment and tissue extracts. Extracts were analyzed using dual column high resolution gas chromatography with electron capture detection (GC/ECD) and confirmation was obtained with gas chromatography mass spectrometry using a quadrupole ion trap detector in MS-MS mode. Method detection limits (MDLs) have been established for water (1-3 ng/L), sediment (0.5-4 ng/g dry weight) and tissue (1-3 ng/g fresh weight). Mean percent recoveries of fortified blanks and samples ranged from 75 to 115% with relative standard deviation (RSD) values less than 20% for all target compounds.

Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

PubMed

Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

2016-06-01

Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Calcium Alginate-Caged Multiwalled Carbon Nanotubes Dispersive Microsolid Phase Extraction Combined With Gas Chromatography-Flame Ionization Detection for the Determination of Polycyclic Aromatic Hydrocarbons in Water Samples.

PubMed

Abboud, Ayad Sami; Sanagi, Mohd Marsin; Ibrahim, Wan Aini Wan; Keyon, Aemi S Abdul; Aboul-Enein, Hassan Y

2018-02-01

In this study, caged calcium alginate-caged multiwalled carbon nanotubes dispersive microsolid phase extraction was described for the first time for the extraction of polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatographic analysis. Fluorene, phenanthrene and fluoranthene were selected as model compounds. The caged calcium alginate-caged multiwalled carbon nanotubes was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy and thermal gravimetry analyses. The effective parameters namely desorption solvent, solvent volume, extraction time, desorption time, the mass of adsorbent and sample volume were optimized. Under the optimum extraction conditions, the developed method showed good linearity in the range of 0.5-50 ng mL-1 (R2 ≥ 0.996), low limits of detection and quantification (0.42-0.22 ng mL-1) (0.73-1.38 ng mL-1) respectively, good relative recoveries (71.2-104.2%) and reproducibility (RSD 1.8-12.4%, n = 3) for the studied PAHs in water sample. With high enrichment factor (1,000), short extraction time (<30 min), low amounts of adsorbent (100 mg) and low amounts of solvent (0.1 mol) have proven that the microsolid phase extraction method based on calcium alginate-caged multiwalled carbon nanotubes are environmentally friendly and convenient extraction method to use as an alternative adsorbent in the simultaneous preconcentration of PAHs from environmental water samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Micelle-mediated extraction of elderberry blossom by whey protein and naturally derived surfactants.

PubMed

Śliwa, Karolina; Tomaszkiewicz-Potępa, Anna; Sikora, Elżbieta; Ogonowski, Jan

2013-01-01

Classical methods of the extraction of active ingredients from the plant material are expensive, complicated and often environmentally unfriendly. The micelle-mediated extraction method (MME) seems to be a good alternative. In this work, extractions of elderberry blossoms (Flos Sambuci) were performed using MME methods. Several popular surfactants and whey protein concentrate (WPC) was applied in the process. The obtained results were compared with those obtained in extraction by means of water. Antioxidant properties of the extracts were analyzed by using two different methods: reaction with di(phenyl)-(2,4,6-trinitrophenyl)iminoazanium (DPPH) reagent and Follin's method. Furthermore, the flavonoid content in the extracts was determined. The results confirmed that the MME method with using whey protein might be an alternative method for obtaining, rich in natural antioxidants, plant extracts.

QUANTITATION OF ESTROGENS IN GROUND WATER AND SWINE LAGOON SAMPLE USING SOLID PHASE EXTRACTION, PENTAFLUROBENZYL/TRIMETHYLSILYL DERIVATIZATIONS AND GAS CHROMATOGRAPHY NEGATIVE ION CHEMICAL IONIZATION/MASS SPECTROMETRY/MASS SPECTROMETRY

EPA Science Inventory

A method was developed for the confirmed identification and quantitation of 17B-estradiol, estrone, 17B-ethynylestrodial and 16a-hydroxy-17B-estradiol (estriol) in ground water and swine lagoon samples. Centrifuged and filtered samples were extracted using solid phase extraction...

The atmosphere of Mars - Resources for the exploration and settlement of Mars

NASA Technical Reports Server (NTRS)

Meyer, T. R.; Mckay, C. P.

1984-01-01

This paper describes methods of processing the Mars atmosphere to supply water, oxygen and buffer gas for a Mars base. Existing life support system technology is combined with innovative methods of water extraction, and buffer gas processing. The design may also be extended to incorporate an integrated greenhouse to supply food, oxygen and water recycling. It is found that the work required to supply one kilogram of an argon/nitrogen buffer gas is 9.4 kW-hr. To extract water from the dry Martian atmosphere can require up to 102.8 kW-hr per kilogram of water depending on the relative humidity of the air.

Faecal indicator bacteria enumeration in beach sand: a comparison study of extraction methods in medium to coarse sands.

PubMed

Boehm, A B; Griffith, J; McGee, C; Edge, T A; Solo-Gabriele, H M; Whitman, R; Cao, Y; Getrich, M; Jay, J A; Ferguson, D; Goodwin, K D; Lee, C M; Madison, M; Weisberg, S B

2009-11-01

The absence of standardized methods for quantifying faecal indicator bacteria (FIB) in sand hinders comparison of results across studies. The purpose of the study was to compare methods for extraction of faecal bacteria from sands and recommend a standardized extraction technique. Twenty-two methods of extracting enterococci and Escherichia coli from sand were evaluated, including multiple permutations of hand shaking, mechanical shaking, blending, sonication, number of rinses, settling time, eluant-to-sand ratio, eluant composition, prefiltration and type of decantation. Tests were performed on sands from California, Florida and Lake Michigan. Most extraction parameters did not significantly affect bacterial enumeration. anova revealed significant effects of eluant composition and blending; with both sodium metaphosphate buffer and blending producing reduced counts. The simplest extraction method that produced the highest FIB recoveries consisted of 2 min of hand shaking in phosphate-buffered saline or deionized water, a 30-s settling time, one-rinse step and a 10 : 1 eluant volume to sand weight ratio. This result was consistent across the sand compositions tested in this study but could vary for other sand types. Method standardization will improve the understanding of how sands affect surface water quality.

Evaluation of solvent effect on the extraction of phenolic compounds and antioxidant capacities from the berries: application of principal component analysis.

PubMed

Boeing, Joana Schuelter; Barizão, Erica Oliveira; E Silva, Beatriz Costa; Montanher, Paula Fernandes; de Cinque Almeida, Vitor; Visentainer, Jesuí Vergilio

2014-01-01

This study evaluated the effect of the solvent on the extraction of antioxidant compounds from black mulberry (Morus nigra), blackberry (Rubus ulmifolius) and strawberry (Fragaria x ananassa). Different extracts of each berry were evaluated from the determination of total phenolic content, anthocyanin content and antioxidant capacity, and data were applied to the principal component analysis (PCA) to gain an overview of the effect of the solvent in extraction method. For all the berries analyzed, acetone/water (70/30, v/v) solvent mixture was more efficient solvent in the extracting of phenolic compounds, and methanol/water/acetic acid (70/29.5/0.5, v/v/v) showed the best values for anthocyanin content. Mixtures of ethanol/water (50/50, v/v), acetone water/acetic acid (70/29.5/0.5, v/v/v) and acetone/water (50/50, v/v) presented the highest antioxidant capacities for black mulberries, blackberries and strawberries, respectively. Antioxidants extractions are extremely affected by the solvent combination used. In addition, the obtained extracts with the organic solvent-water mixtures were distinguished from the extracts obtained with pure organic solvents, through the PCA analysis.

Mesoporous silica based MCM-41 as solid-phase extraction sorbent combined with micro-liquid chromatography-quadrupole-mass spectrometry for the analysis of pharmaceuticals in waters.

PubMed

Dahane, S; Martínez Galera, M; Marchionni, M E; Socías Viciana, M M; Derdour, A; Gil García, M D

2016-05-15

This paper reports the first application of the silica based mesoporous material MCM-41 as a sorbent in solid phase extraction, to pre-concentrate pharmaceuticals of very different polarity (atenolol, nadolol, pindolol, timolol, bisoprolol, metoprolol, betaxolol, ketoprofen, naproxen, ibuprofen, diclofenac, tolfenamic acid, flufenamic acid and meclofenamic acid) in surface waters. The analytes were extracted from 100mL water samples at pH 2.0 (containing 10(-3) mol/L of sodium chloride) by passing the solution through a cartridge filled with 100 mg of MCM-41. Following elution, the pharmaceuticals were determined by micro-liquid chromatography and triple quadrupole-mass spectrometry. Two selected reaction monitoring transitions were monitored per compound, the most intense one being used for quantification and the second one for confirmation. Matrix effect was found in real waters for most analytes and was overcome using the standard addition method, which compared favorably with the matrix matched calibration method. The detection limits in solvent (acetonitrile:water 10:90, v/v) ranged from 0.01 to 1.48 μg/L and in real water extracts from 0.10 to 3.85 μg/L (0.001-0.0385 μg/L in the water samples). The quantitation limits in solvent were in the range 0.02-4.93 μg/L, whereas in real water extracts were between 0.45 and 10.00 μg/L (0.0045 and 0.1000 μg/L in the water samples). When ultrapure water samples were spiked at two concentration levels of each pharmaceutical (0.1 and 0.2 μg/L) and quantified using solvent based calibration graphs, recoveries were near 100%. However, recoveries for most pharmaceuticals were comparable or better than de described above, when river water samples (spiked at the same concentration levels) were quantified by the standard addition method and slightly worse using the matrix matched calibration method. Five real samples (two rivers, one dam and two fountain water samples) were analyzed by the developed method, atenolol, timolol, betaxolol, nadolol and diclofenac being found in some of them, at levels higher than their quantitation limits. Copyright © 2016 Elsevier B.V. All rights reserved.

Optimization of squalene produced from crude palm oil waste

NASA Astrophysics Data System (ADS)

Wandira, Irda; Legowo, Evita H.; Widiputri, Diah I.

2017-01-01

Squalene is a hydrocarbon originally and still mostly extracted from shark liver oil. Due to environmental issues over shark hunting, there have been efforts to extract squalene from alternative sources, such as Palm Fatty Acid Distillate (PFAD), one of crude palm oil (CPO) wastes. Previous researches have shown that squalene can be extracted from PFAD using saponification process followed with liquid-liquid extraction process although the method had yet to be optimized in order to optimize the amount of squalene extracted from PFAD. The optimization was done by optimizing both processes of squalene extraction method: saponification and liquid-liquid extraction. The factors utilized in the saponification process optimization were KOH concentration and saponification duration while during the liquid-liquid extraction (LLE) process optimization, the factors used were the volumes of distilled water and dichloromethane. The optimum percentage of squalene content in the extract (24.08%) was achieved by saponifying the PFAD with 50%w/v KOH for 60 minutes and subjecting the saponified PFAD to LLE, utilizing 100 ml of distilled water along with 3 times addition of fresh dichloromethane, 75 ml each; those factors would be utilized in the optimum squalene extraction method.

Effect of Ultrasound in Soybean Protein Extraction

NASA Astrophysics Data System (ADS)

Fukase, Hirokazu; Ohdaira, Etsuzo; Masuzawa, Nobuyoshi; Ide, Masao

1994-05-01

Application of ultrasound for accelerating the extraction of nutriments in food processing has been attempted. However, conditions of exposure to ultrasound were not clear in previous studies. This paper reports on the relationship between the ultrasonic pressure and the amount of extracted protein from soybeans. Experiments were conducted using a beaker, in which the ultrasonic fields were precisely measured. Soybean flakes suspended in water were put in the beaker and placed in a water tank. The amount of extracted protein in water upon ultrasonic exposure was calculated by the Kjeldahl method. It was found that the amount of extracted protein increased in proportion to ultrasonic pressure up to the total amount of soybean protein soluble in water. Furthermore, this paper describes the denaturation of the protein produced by the ultrasonic cavitation.

[Optimization of solid-phase extraction for enrichment of toxic organic compounds in water samples].

PubMed

Zhang, Ming-quan; Li, Feng-min; Wu, Qian-yuan; Hu, Hong-ying

2013-05-01

A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.

Low-density solvent based ultrasound-assisted emulsification microextraction and on-column derivatization combined with gas chromatography-mass spectrometry for the determination of carbamate pesticides in environmental water samples.

PubMed

Guo, Liang; Lee, Hian Kee

2012-04-27

A fast and efficient method for the determination of trace level of carbamate pesticides using a lower-density-than-water solvent for ultrasound-assisted emulsification microextraction coupled to on-column derivatization and analysis by GC-MS has been developed and studied. In this approach, a soft plastic Pasteur pipette was employed as a convenient extraction device. Fifty microliters of extraction solvent, of lower density than water, was injected into the sample solution held in the pipette. The latter was immediately immersed in an ultrasound water bath to form an emulsion. After 2 min extraction, the emulsion was fractionated into two layers by centrifugation. The upper layer (organic extract) could be collected conveniently by squeezing the bulb of the pipette, now held upside down, to move it into the narrow stem of the device, facilitating its retrieval for analysis. The extract was then combined with trimethylphenylammonium hydroxide and directly injected into a gas chromatography-mass spectrometry (GC-MS) system for on-column derivatization and analysis. The on-column derivatization provided an added convenience (since a separate step was not necessary). Parameters affecting the derivatization and extraction were investigated. Under the most favorable conditions, the method demonstrated high extraction efficiency with low limits of detection of between 0.01 and 0.1 μg/L, good linearity in the range of 0.05-50 μg/L, to 0.5-100 μg/L, and good repeatability (RSD below 9.2%, n=5). The proposed method was evaluated by determining carbamate pesticides in river water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Analytical method development using functionalized polysulfone membranes for the determination of chlorinated hydrocarbons in water.

PubMed

Nuhu, Abdulmumin A; Basheer, Chanbasha; Abu-Thabit, Nedal Y; Alhooshani, Khalid; Al-Arfaj, Abdul Rahman

2011-12-15

In this study, functionalized polysulfone membrane has been utilized as a sorbent for the extraction of chlorinated hydrocarbons (CHCs) in water samples. Two different functionalized polysulfones (i) phosphonic acid functionalized polysulfone (PPSU-A) with different forms (cross-linked and non cross-linked) membranes and (ii) phosphonic ester functionalized polysulfone (PPSU-E) with different forms (cross-linked and non cross-linked) were evaluated for the extraction of CHCs in water. A 10 ml of spiked water sample was extracted with 50mg piece of the functionalized membrane. After extraction, the membrane was desorbed by organic solvent and the extract was analyzed by gas chromatography-mass spectrometry. Eight CHCs, 1,3,5-trichlorobenzene (1,3,5-TCB), 1,2,3-trichlorobenzene (1,2,3-TCB), 1,1,2,3,4,4-hexachloro-1,3-butadiene (HCBD), 1,2,4-trichloro-3-methylbenzene (TCMB), 1,2,3,4-tetrachlorobenzene (1,2,3,4-TeCB), 1,2,4,5-tetrachlorobenzene (1,2,4,5-TeCB), pentachlorobenzene (PeCB) and hexachlorobenzene (HCB) were used as model compounds. Experimental parameters such as extraction time, desorption time, types of polymer membrane as well the nature of desorption solvent were optimized. Using optimum extraction conditions calibration curves were linear with coefficients of determination between 0.9954 and 0.9999 over wide range of concentrations (0.05-100 μgl(-1)). The method detection limits (at a signal-to-noise ratio of 3) were in the range of 0.4-3.9 ng l(-1). The proposed method was evaluated for the determination of CHCs in drinking water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of short chain chlorinated paraffins in water by stir bar sorptive extraction-thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry.

PubMed

Tölgyessy, P; Nagyová, S; Sládkovičová, M

2017-04-21

A simple, robust, sensitive and environment friendly method for the determination of short chain chlorinated paraffins (SCCPs) in water using stir bar sorptive extraction (SBSE) coupled to thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry (TD-GC-QqQ-MS/MS) was developed. SBSE was performed using 100mL of water sample, 20mL of methanol as a modifier, and a commercial sorptive stir bar (with 10mm×0.5mm PDMS layer) during extraction period of 16h. After extraction, the sorptive stir bar was thermally desorbed and online analysed by GC-MS/MS. Method performance was evaluated for MilliQ and surface water spiked samples. For both types of matrices, a linear dynamic range of 0.5-3.0μgL -1 with correlation coefficients >0.999 and relative standard deviations (RSDs) of the relative response factors (RRFs) <12% was established. The limits of quantification (LOQs) of 0.06 and 0.08μgL -1 , and the precision (repeatability) of 6.4 and 7.7% (RSDs) were achieved for MilliQ and surface water, respectively. The method also showed good robustness, recovery and accuracy. The obtained performance characteristics indicate that the method is suitable for screening and monitoring and compliance checking with environmental quality standards (EQS, set by the EU) for SCCPs in surface waters. Copyright © 2017 Elsevier B.V. All rights reserved.

Polydopamine-coated magnetic nanoparticles for isolation and enrichment of estrogenic compounds from surface water samples followed by liquid chromatography-tandem mass spectrometry determination.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Piovesana, Susy; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2016-06-01

Estrogens, phytoestrogens, and mycoestrogens may enter into the surface waters from different sources, such as effluents of municipal wastewater treatment plants, industrial plants, and animal farms and runoff from agricultural areas. In this work, a multiresidue analytical method for the determination of 17 natural estrogenic compounds, including four steroid estrogens, six mycoestrogens, and seven phytoestrogens, in river water samples has been developed. (Fe3O4)-based magnetic nanoparticles coated by polydopamine (Fe3O4@pDA) were used for dispersive solid-phase extraction, and the final extract was analyzed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry. The Fe3O4 magnetic nanoparticles were prepared by a co-precipitation procedure, coated by pDA, and characterized by scanning electron microscopy, infrared spectroscopy, and elemental analysis. The sample preparation method was optimized in terms of extraction recovery, matrix effect, selectivity, trueness, precision, method limits of detection, and method limits of quantification (MLOQs). For all the 17 analytes, recoveries were >70 % and matrix effects were below 30 % when 25 mL of river water sample was treated with 90 mg of Fe3O4@pDA nanoparticles. Selectivity was tested by spiking river water samples with 50 other compounds (mycotoxins, antibacterials, conjugated hormones, UV filters, alkylphenols, etc.), and only aflatoxins and some benzophenones showed recoveries >60 %. This method proved to be simple and robust and allowed the determination of natural estrogenic compounds belonging to different classes in surface waters with MLOQs ranging between 0.003 and 0.1 μg L(-1). Graphical Abstract Determination of natural estrogenic compounds in water by magnetic solid phase extraction followed by liquid chromatography-tandem mass spectrometry analysis.

Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group?Determination of acetamide herbicides and their degradation products in water using online solid-phase extraction and liquid chromatography/mass spectrometry

USGS Publications Warehouse

Lee, E.A.; Strahan, A.P.

2003-01-01

An analytical method for the determination of 6 acetamide herbicides (acetochlor, alachlor, dimethenamid, flufenacet, metolachlor, and propachlor) and 16 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is described in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using octadecylsilane as the solid-phase extraction media on online automated equipment followed by liquid chromatography/mass spectrometry. The method uses only 10 milliliters of sample per injection. Three different water-sample matrices, a reagent-water, a ground-water, and a surface-water sample spiked at 0.10 and 1.0 microgram per liter, were analyzed to determine method performance. Method detection limits ranged from 0.004 to 0.051 microgram per liter for the parent acetamide herbicides and their degradation products. Mean recoveries for the acetamide compounds in the ground- and surface-water samples ranged from 62.3 to 117.4 percent. The secondary amide of acetochlor/metolachlor ethanesulfonic acid (ESA) was recovered at an average rate of 43.5 percent. The mean recoveries for propachlor and propachlor oxanilic acid (OXA) were next lowest, ranging from 62.3 to 95.5 percent. Mean recoveries from reagent-water samples ranged from 90.3 to 118.3 percent for all compounds. Overall the mean of the mean recoveries of all compounds in the three matrices spiked at 0.10 and 1.0 microgram per liter ranged from 89.9 to 100.7 percent, including the secondary amide of acetochlor/metolachlor ESA and the propachlor compounds. The acetamide herbicides and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter. The upper concentration limit is 2.0 micrograms per liter for all compounds without dilution. With the exception of the secondary amide of acetochlor/metolachlor ESA, good precision and accuracy for the chloroacetanalide herbicides and their degradation compounds were demonstrated for the method in buffered reagent water, ground water, and surface water. The extraction method as used did not optimize the recovery of the secondary amide of acetochlor/metolachlor ESA.

GC-MS determination of parabens, triclosan and methyl triclosan in water by in situ derivatisation and stir-bar sorptive extraction.

PubMed

Casas Ferreira, Ana María; Möder, Monika; Fernández Laespada, María Esther

2011-01-01

Stir-bar sorptive extraction in combination with an in situ derivatisation reaction and thermal desorption-gas chromatography-mass spectrometry was successfully applied to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in water samples. This approach improves both the extraction efficiency and the sensitivity in the GC in a simple way since the derivatisation reaction occurs at the same time as the extraction procedure. The in situ derivatisation reaction was carried out with acetic anhydride under alkaline conditions. Thermal desorption parameters (cryofocusing temperature, desorption flow, desorption time, desorption temperature) were optimised using a Box-Behnken experimental design. All the analytes gave recoveries higher than 79%, except methylparaben (22%). The method afforded detection limits between 0.64 and 4.12 ng/L, with good reproducibility and accuracy values. The feasibility of the method for the determination of analytes in water samples was checked in tap water and untreated and treated wastewater.

Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

PubMed

Herrero Latorre, C; Barciela García, J; García Martín, S; Peña Crecente, R M

2013-12-04

Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

Development of a selective and pH-independent method for the analysis of ultra trace amounts of nitrite in environmental water samples after dispersive magnetic solid phase extraction by spectrofluorimetry.

PubMed

Daneshvar Tarigh, Ghazale; Shemirani, Farzaneh

2014-10-01

This paper describes an innovative and rapidly dispersive magnetic solid phase extraction spectrofluorimetry (DMSPE-FL) method for the analysis of trace amounts of nitrite in some environmental water samples. The method includes derivatization of aqueous nitrite with 2, 3-diaminonaphthalene (DAN), analysis of highly fluorescent 2, 3-naphthotriazole (NAT) derivative using spectrofluorimetry after DSPME. The novelty of our method is based on forming NAT that was independent with the pH-responsive and was adsorbed on MMWCNT by hydrophobic attractions in both acidic and basic media. The extraction efficiency of the sorbent was investigated by extraction of nitrite. The optimum extraction conditions for NO2(-) were obtained as of extraction time, 1.5 min; 10mg sorbent from 160 mL of the sample solution, and elution with 1 mL of acetone/KOH. Under the optimal conditions, the calibration curves were obtained in the range of 0.1-80 µg L(-1) (R(2)=0.999) and LOD (S/N=3) was obtained in 34 ng L(-1). Relative standard deviations (RSD) were 0.6 % (five replicates at 5 μg L(-1)). In addition, the feasibility of the method was demonstrated with extraction and determination of nitrite from some real samples containing tap, mineral, sea, rain, snow and ground waters, with the recovery in standard addition to real matrix of 94-102 % and RSDs of 1.8-10.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

Plant tissue analysis for explosive compounds in phytoremediation and phytoforensics.

PubMed

Karnjanapiboonwong, Adcharee; Mu, Ruipu; Yuan, Yuan; Shi, Honglan; Ma, Yinfa; Burken, Joel G

2012-01-01

Plant tissue analysis methods were evaluated for six explosive compounds to assess uptake and phytoforensic methods development to quantify explosives in plant to obtain the plant data for the evaluation of explosive contamination in soil and groundwater. Four different solvent mixtures containing acetonitrile or methanol were tested at variable extraction ratios to compare the extraction efficiency for six explosive compounds: 2,4,6-trinitrotoluene (TNT), pentaerythritoltetranitrate (PETN), hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), 2-amino-4,6-dinitrotoluene (2ADNT), and 2,4-Dinitroanisole (DNAN), in Laurel Willow (Salix pentandra) stem and range grass Big Bluestem (Andropogon gerardii) using LC-MS/MS. Plant tissues were spiked with 500 ng/g of explosives and extracted using ultrasonically-assisted solvent extraction. With the ratio of fresh plant mass to solvent volume of 1:20 for willow and 1:40 for big bluestem grass, results indicated that all explosives in willow except HMX were extracted at higher than 73.3% by using 20 mL of methanol, 50:50 (v/v) methanol:water, or acetonitrile, whereas HMX was extracted with the highest recovery of 61.3% by 20 mL of acetonitrile. In big bluestem grass, the most effective solvents were 20 mL of either methanol or 50:50 (v/v) methanol:water for PETN extraction with a recovery of higher than 101.2% and 20 mL of 50:50 (v/v) methanol:water for HMX, RDX, TNT, 2ADNT, and DNAN extraction with a recovery of 83.8%, 104.4%, 97.5%, 80.7%, and 108.2%, respectively. However, unlike methanol and acetonitrile, 50:50 (v/v) methanol:water provided no problem of leading or split peak in chromatogram; therefore, it was preferred in the test and performed a method validation. Results indicated that 50:50 (v/v) methanol:water provided good repeatability and recovery and method detection limits at 0.5-20 ng/g fresh weight or 8.8-61.3 ng/g dry weight. Overall, results suggested that solvent extraction efficiency of explosives in plant was influenced by plant species and solvent used, and method presented here was believed to provide the preliminary data with respect to the analysis of simultaneous explosives in plants with LC-MS/MS.

Subcritical water extraction of alkaloids in Sophora flavescens Ait. and determination by capillary electrophoresis with field-amplified sample stacking.

PubMed

Wang, Haiyan; Lu, Yuchao; Chen, Jie; Li, Junchao; Liu, Shuhui

2012-01-25

The extraction and determination of cytisine, sophocarpine, matrine, sophoridine and oxymatrine in Sophora flavescens Ait. were performed using subcritical water extraction and capillary electrophoresis with field-amplified sample stacking. The effects of extraction temperature, pressure, time and cycle number on the extraction yields were investigated systematically for accelerated solvent extraction with ethanol (ASE) and accelerated solvent extraction with water (subcritical water extraction, SWE). The extraction yields obtained using SWE, ASE, water ultrasonic extraction and chloroform soaking extraction methods were compared. The electrophoresis separation buffer was monosodium phosphate (pH 3.0; 110 mM)-isopropanol (85:15, v/v). The effect of phosphoric acid added to the sample matrix on the reproducibility of the peak heights of the analytes was also examined. Cytisine, sophoridine and oxymatrine showed good linearity (R(2)>0.999) within 0.125-4.0 μg/mL, and sophocarpine and matrine exhibited good linearity (R(2)>0.998) within 0.0625-2.0 μg/mL, with the detection limits in the range of 0.004-0.0013 μg/mL. The five alkaloid contents in medicinal plants from different sources and Sophora instant granule were determined and compared. Copyright © 2011 Elsevier B.V. All rights reserved.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of organophosphate pesticides in filtered water by gas chromatography with flame photometric detection

USGS Publications Warehouse

Jha, Virendra K.; Wydoski, Duane S.

2002-01-01

A method for the isolation of 20 parent organophosphate pesticides and 5 pesticide degradates from filtered natural-water samples is described. Seven of these compounds are reported permanently with an estimated concentration because of performance issues. Water samples are filtered to remove suspended particulate matter, and then 1 liter of filtrate is pumped through disposable solid-phase extraction columns that contain octadecyl-bonded porous silica to extract the compounds. The C-18 columns are dried with nitrogen gas, and method compounds are eluted from the columns with ethyl acetate. The extract is analyzed by dual capillary-column gas chromatography with flame photometric detection. Single-operator method detection limits in all three water-matrix samples ranged from 0.004 to 0.012 microgram per liter. Method performance was validated by spiking all compounds into three different matrices at three different concentrations. Eight replicates were analyzed at each concentration level in each matrix. Mean recoveries of method compounds spiked in surface-water samples ranged from 39 to 149 percent and those in ground-water samples ranged from 40 to 124 percent for all pesticides except dimethoate. Mean recoveries of method compounds spiked in reagent-water samples ranged from 41 to 119 percent for all pesticides except dimethoate. Dimethoate exhibited reduced recoveries (mean of 43 percent in low- and medium-concentration level spiked samples and 20 percent in high-concentration level spiked samples) in all matrices because of incomplete collection on the C-18 column. As a result, concen-trations of dimethoate and six other compounds (based on performance issues) in samples are reported in this method with an estimated remark code.

Analysis of hydrazine in drinking water by isotope dilution gas chromatography/tandem mass spectrometry with derivatization and liquid-liquid extraction.

PubMed

Davis, William E; Li, Yongtao

2008-07-15

A new isotope dilution gas chromatography/chemical ionization/tandem mass spectrometric method was developed for the analysis of carcinogenic hydrazine in drinking water. The sample preparation was performed by using the optimized derivatization and multiple liquid-liquid extraction techniques. Using the direct aqueous-phase derivatization with acetone, hydrazine and isotopically labeled hydrazine-(15)N2 used as the surrogate standard formed acetone azine and acetone azine-(15)N2, respectively. These derivatives were then extracted with dichloromethane. Prior to analysis using methanol as the chemical ionization reagent gas, the extract was dried with anhydrous sodium sulfate, concentrated through evaporation, and then fortified with isotopically labeled N-nitrosodimethylamine-d6 used as the internal standard to quantify the extracted acetone azine-(15)N2. The extracted acetone azine was quantified against the extracted acetone azine-(15)N2. The isotope dilution standard calibration curve resulted in a linear regression correlation coefficient (R) of 0.999. The obtained method detection limit was 0.70 ng/L for hydrazine in reagent water samples, fortified at a concentration of 1.0 ng/L. For reagent water samples fortified at a concentration of 20.0 ng/L, the mean recoveries were 102% with a relative standard deviation of 13.7% for hydrazine and 106% with a relative standard deviation of 12.5% for hydrazine-(15)N2. Hydrazine at 0.5-2.6 ng/L was detected in 7 out of 13 chloraminated drinking water samples but was not detected in the rest of the chloraminated drinking water samples and the studied chlorinated drinking water sample.

Ionic liquid-salt aqueous two-phase extraction based on salting-out coupled with high-performance liquid chromatography for the determination of sulfonamides in water and food.

PubMed

Han, Juan; Wang, Yun; Liu, Yan; Li, Yanfang; Lu, Yang; Yan, Yongsheng; Ni, Liang

2013-02-01

Ionic liquid-salt aqueous two-phase extraction coupled with high-performance liquid chromatography with ultraviolet detection was developed for the determination of sulfonamides in water and food samples. In the procedure, the analytes were extracted from the aqueous samples into the ionic liquid top phase in one step. Three sulfonamides, sulfamerazine, sulfamethoxazole, and sulfamethizole were selected here as model compounds for developing and evaluating the method. The effects of various experimental parameters in extraction step were studied using two optimization methods, one variable at a time and Box-Behnken design. The results showed that the amount of sulfonamides did not have effect on the extraction efficiency. Therefore, a three-level Box-Behnken experimental design with three factors, which combined the response surface modeling, was used to optimize sulfonamides extraction. Under the most favorable extraction parameters, the detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.15-0.3 ng/mL and 0.5-1.0 ng/mL from spiked samples, respectively, which are lower than or comparable with other reported approaches applied to the determination of the same compounds. Finally, the proposed method was successfully applied to the determination of sulfonamide compounds in different water and food samples and satisfactory recoveries of spiked target compounds in real samples were obtained.

Comparison of marine sampling methods for organic contaminants: Passive samplers, water extractions, and live oyster deployment.

PubMed

Raub, Kristin B; Vlahos, Penny; Whitney, Michael

2015-08-01

Laboratory and field trials evaluated the efficacy of three methods of detecting aquatic pesticide concentrations. Currently used pesticides: atrazine, metolachlor, and diazinon and legacy pesticide dieldrin were targeted. Pesticides were extracted using solid-phase extraction (SPE) of water samples, titanium plate passive samplers coated in ethylene vinyl acetate (EVA) and eastern oysters (Crassostrea viginica) as biosamplers. A laboratory study assessed the extraction efficiencies and precision of each method. Passive samplers yielded the highest precision of the three methods (RSD: 3-14% EVA plates; 19-60% oysters; and 25-56% water samples). Equilibrium partition coefficients were derived. A significant relationship was found between the concentration in oyster tissue and the ambient aquatic concentration. In the field (Housatonic River, CT (U.S.)) water sampling (n = 5) detected atrazine at 1.61-7.31 μg L(-1), oyster sampling (n = 2×15) detected dieldrin at n.d.-0.096 μg L(-1) SW and the passive samplers (n = 5×3) detected atrazine at 0.97-3.78 μg L(-1) SW and dieldrin at n.d.-0.68 μg L(-1) SW. Copyright © 2015 Elsevier Ltd. All rights reserved.

Microwave Extraction of Water from Lunar Regolith Simulant

NASA Technical Reports Server (NTRS)

Ethridge, Edwin C.; Kaukler, William

2007-01-01

Nearly a decade ago the DOD Clementine lunar orbital mission obtained data indicating that the permanently shaded regions at the lunar poles may have permanently frozen water in the lunar soil. Currently NASA's Robotic Lunar Exploration Program, RLEP-2, is planned to land at the lunar pole to determine if water is present. The detection and extraction of water from the permanently frozen permafrost is an important goal for NASA. Extraction of water from lunar permafrost has a high priority in the In-Situ Resource Utilization, ISRU, community for human life support and as a fuel. The use of microwave processing would permit the extraction of water without the need to dig, drill, or excavate the lunar surface. Microwave heating of regolith is potentially faster and more efficient than any other heating methods due to the very low thermal conductivity of the lunar regolith. Also, microwaves can penetrate into the soil permitting water removal from deep below the lunar surface. A cryogenic vacuum test facility was developed for evaluating the use of microwave heating and water extraction from a lunar regolith permafrost simulant. Water is obtained in a cryogenic cold trap even with soil conditions below 0 C. The results of microwave extraction of water experiments will be presented.

Faecal indicator bacteria enumeration in beach sand: A comparison study of extraction methods in medium to coarse sands

USGS Publications Warehouse

Boehm, A.B.; Griffith, J.; McGee, C.; Edge, T.A.; Solo-Gabriele, H. M.; Whitman, R.; Cao, Y.; Getrich, M.; Jay, J.A.; Ferguson, D.; Goodwin, K.D.; Lee, C.M.; Madison, M.; Weisberg, S.B.

2009-01-01

Aims: The absence of standardized methods for quantifying faecal indicator bacteria (FIB) in sand hinders comparison of results across studies. The purpose of the study was to compare methods for extraction of faecal bacteria from sands and recommend a standardized extraction technique. Methods and Results: Twenty-two methods of extracting enterococci and Escherichia coli from sand were evaluated, including multiple permutations of hand shaking, mechanical shaking, blending, sonication, number of rinses, settling time, eluant-to-sand ratio, eluant composition, prefiltration and type of decantation. Tests were performed on sands from California, Florida and Lake Michigan. Most extraction parameters did not significantly affect bacterial enumeration. anova revealed significant effects of eluant composition and blending; with both sodium metaphosphate buffer and blending producing reduced counts. Conclusions: The simplest extraction method that produced the highest FIB recoveries consisted of 2 min of hand shaking in phosphate-buffered saline or deionized water, a 30-s settling time, one-rinse step and a 10 : 1 eluant volume to sand weight ratio. This result was consistent across the sand compositions tested in this study but could vary for other sand types. Significance and Impact of the Study: Method standardization will improve the understanding of how sands affect surface water quality. ?? 2009 The Society for Applied Microbiology.

Application of modified hollow fiber liquid phase microextraction in conjunction with chromatography-electron capture detection for quantification of acrylamide in waste water samples at ultra-trace levels.

PubMed

Sobhi, Hamid Reza; Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali

2017-03-03

Herein, a simple and sensitive method was successfully developed for the extraction and quantification of acrylamide in water samples. Initially, acrylamide was derivatized through a bromination process. Subsequently, a modified hollow-fiber liquid-phase microextraction was applied for the extraction of the brominated acrylamide from a 10-ml portion of an aqueous sample. Briefly, in this method, the derivatized acrylamide (2,3-dibromopropionamide) was extracted from the aqueous sample into a thin layer of an organic solvent sustained in pores of a porous hollow fiber. Then, it was back-extracted using a small volume of organic acceptor solution (acetonitril, 25μl) located inside the lumen of the hollow fiber followed by gas chromatography-electron capture detection (GC-ECD). The optimal conditions were examined for the extraction of the analyte such as: the organic solvent: dihexyl ether+10% tri-n-octyl phosphine oxide; stirring rate: 750rpm; no salt addition and 30min extraction time. These optimal extraction conditions allowed excellent enrichment factor values for the method. Enrichment factor, detection limit (S/N=3) and dynamic linear range of 60, 2ngL -1 and 50-1000ngL -1 to be determined for the analyte. The relative standard deviations (RSD%) representing precision of the method were in the range of 2.2-5.8 based on the average of three measurements. Accuracy of the method was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 108%. Finally, the method proved to be simple, rapid, and cost-effective for routine screen of acrylamide-contaminated highly-complicated untreated waste water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Solid-phase microextraction-gas chromatography-mass spectrometry for the analysis of selective serotonin reuptake inhibitors in environmental water.

PubMed

Lamas, J Pablo; Salgado-Petinal, Carmen; García-Jares, Carmen; Llompart, María; Cela, Rafael; Gómez, Mariano

2004-08-13

The continuous contamination of surface waters by pharmaceuticals is of most environmental concern. Selective serotonin reuptake inhibitors (SSRIs) are drugs currently prescribed for the treatment of depressions and other psychiatric disorders and then, they are among the pharmaceuticals that can occur in environmental waters. Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry has been applied to the extraction of five SSRIs--venlafaxine, fluvoxamine, fluoxetine, citalopram and sertraline--from water samples. Some of the analytes were not efficiently extracted as underivatized compounds and so, an in situ acetylation step was introduced in the sample preparation procedure. Different parameters affecting extraction efficiency such as extraction mode, fiber coating and temperature were studied. A mixed-level fractional factorial design was also performed to simultaneously study the influence of other five experimental factors. Finally, a method based on direct SPME at 100 degrees C using polydimethylsiloxane-divinylbenzene fibers is proposed. The performance of the method was evaluated, showing good linearity and precision. The detection limits were in the sub-ng/mL level. Practical applicability was demonstrated through the analysis of real samples. Recoveries obtained for river water and wastewater samples were satisfactory in all cases. An important aspect of the proposed method is that no matrix effects were observed. Two of the target compounds, venlafaxine and citalopram, were detected and quantified in a sewage water sample.

Ultra-trace levels analysis of microcystins and nodularin in surface water by on-line solid-phase extraction with high-performance liquid chromatography tandem mass spectrometry.

PubMed

Balest, Lydia; Murgolo, Sapia; Sciancalepore, Lucia; Montemurro, Patrizia; Abis, Pier Paolo; Pastore, Carlo; Mascolo, Giuseppe

2016-06-01

An on-line solid phase extraction coupled with high-performance liquid chromatography in tandem with mass spectrometry (on-line SPE/HPLC/MS-MS) method for the determination of five microcystins and nodularin in surface waters at submicrogram per liter concentrations has been optimized. Maximum recoveries were achieved by carefully optimizing the extraction sample volume, loading solvent, wash solvent, and pH of the sample. The developed method was also validated according to both UNI EN ISO IEC 17025 and UNICHIM guidelines. Specifically, ten analytical runs were performed at three different concentration levels using a reference mix solution containing the six analytes. The method was applied for monitoring the concentrations of microcystins and nodularin in real surface water during a sampling campaign of 9 months in which the ELISA method was used as standard official method. The results of the two methods were compared showing good agreement when the highest concentration values of MCs were found. Graphical abstract An on-line SPE/HPLC/MS-MS method for the determination of five microcystins and nodularin in surface waters at sub μg L(-1) was optimized and compared with ELISA assay method for real samples.

Dual-cloud point extraction coupled to high performance liquid chromatography for simultaneous determination of trace sulfonamide antimicrobials in urine and water samples.

PubMed

Nong, Chunyan; Niu, Zongliang; Li, Pengyao; Wang, Chunping; Li, Wanyu; Wen, Yingying

2017-04-15

Dual-cloud point extraction (dCPE) was successfully developed for simultaneous extraction of trace sulfonamides (SAs) including sulfamerazine (SMZ), sulfadoxin (SDX), sulfathiazole (STZ) in urine and water samples. Several parameters affecting the extraction were optimized, such as sample pH, concentration of Triton X-114, extraction temperature and time, centrifugation rate and time, back-extraction solution pH, back-extraction temperature and time, back-extraction centrifugation rate and time. High performance liquid chromatography (HPLC) was applied for the SAs analysis. Under the optimum extraction and detection conditions, successful separation of the SAs was achieved within 9min, and excellent analytical performances were attained. Good linear relationships (R 2 ≥0.9990) between peak area and concentration for SMZ and STZ were optimized from 0.02 to 10μg/mL, for SDX from 0.01 to 10μg/mL. Detection limits of 3.0-6.2ng/mL were achieved. Satisfactory recoveries ranging from 85 to 108% were determined with urine, lake and tap water spiked at 0.2, 0.5 and 1μg/mL, respectively, with relative standard deviations (RSDs, n=6) of 1.5-7.7%. This method was demonstrated to be convenient, rapid, cost-effective and environmentally benign, and could be used as an alternative tool to existing methods for analysing trace residues of SAs in urine and water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Gold in natural water: A method of determination by solvent extraction and electrothermal atomization

USGS Publications Warehouse

McHugh, J.B.

1984-01-01

A method has been developed using electrothermal atomization to effectively determine the amount of gold in natural water within the nanogram range. The method has four basic steps: (1) evaporating a 1-L sample; (2) putting it in hydrobromic acid-bromine solution; (3) extracting the sample with methyl-isobutyl-ketone; and (4) determining the amount of gold using an atomic absorption spectrophotometer. The limit of detection is 0.001 ??g gold per liter. Results from three studies indicate, respectively, that the method is precise, effective, and free of interference. Specifically, a precision study indicates that the method has a relative standard deviation of 16-18%; a recovery study indicates that the method recovers gold at an average of 93%; and an interference study indicates that the interference effects are eliminated with solvent extraction and background correction techniques. Application of the method to water samples collected from 41 sites throughout the Western United States and Alaska shows a gold concentration range of < 0.001 to 0.036 ??g gold per liter, with an average of 0.005 ??g/L. ?? 1984.

Liquid chromatographic-diode-array detection multiresidue determination of rice herbicides in drinking and paddy-field water.

PubMed

Roehrs, Rafael; Zanella, Renato; Pizzuti, Ionara; Adaime, Martha B; Pareja, Lucía; Niell, Silvina; Cesio, María V; Heinzen, Horacio

2009-01-01

A sensitive, rapid, and simple multiresidue method for the simultaneous determination of six postemergence herbicides currently used in rice cultivation--metsulfuron methyl, bensulfuron methyl, pyrazosulfuron ethyl, bentazone, bispyribac sodium, and cyhalofop butyl--in drinking and paddy-field water is presented. Water samples were extracted with solid-phase extraction cartridges. Final determination was made by LC with diode-array detection. The extraction efficiencies of C18 and HLB cartridges were compared. The average recovery obtained for these compounds for the lowest spiked level (0.1 microg/L) varied from 70 to 122% for C18 and 75-119% for HLB, with RSDs of 11 and 8.3%, respectively. The method had good linearity, and the lower detection limit for the pesticides studied varied from 0.03 to 0.04 microg/L. The proposed method was also tested in paddy-field water, with recovery studies giving good results with low RSDs at 1.0 microg/L.

DETECTION OF GIARDIA IN ENVIRONMENTAL WATERS BY IMMUNO-PCR AMPLIFICATION METHODS

EPA Science Inventory

Genomic DNA was extracted either directly from Giardia muris cysts seeded into environmental surface waters or from cysts isolated by immunomagnetic beads (IMB).A 0.171-kbp segment of the giardin gene was PCR-amplified following "direct extraction" of Giardia DNA from seeded Caha...

DETECTION OF GIARDIA IN ENVIRONMENTAL WATERS BY IMMUNO-PCR AMPLIFICATION METHODS

EPA Science Inventory

Genomic DNA was extracted either directly from Giardia muris cysts seeded into environmental surface waters or from cysts isolated by immunomagnetic beads (IMB}. A 0.171-kbp segment of the giardin gene was PCR-amplified following "direct extraction" of Giardia DNA from seeded Cah...

A Novel Liquid-Liquid Extraction for the Determination of Sertraline in Tap Water and Waste Water at Trace Levels by GC-MS.

PubMed

Koçoğlu, Elif Seda; Bakırdere, Sezgin; Keyf, Seyfullah

2017-09-01

A simple, green and fast analytical method was developed for the determination of sertraline in tap and waste water samples at trace levels by using supportive liquid-liquid extraction with gas chromatography-mass spectrometry. Different parameters affecting extraction efficiency such as types and volumes of extraction and supporter solvents, extraction period, salt type and amount were optimized to get lower detection limits. Ethyl acetate was selected as optimum extraction solvent. In order to improve the precision, anthracene-D10 was used as an internal standard. The calibration plot of sertraline was linear from 1.0 to 1000 ng/mL with a correlation coefficient of 0.999. The limit of detection value under the optimum conditions was found to be 0.43 ng/mL. In real sample measurements, spiking experiments were performed to check the reliability of the method for these matrices. The spiking experiments yielded satisfactory recoveries of 91.19 ± 2.48%, 90.48 ± 5.19% and 95.46 ± 6.56% for 100, 250 and 500 ng/mL sertraline for tap water, and 85.80 ± 2.15% and 92.43 ± 4.02% for 250 and 500 ng/mL sertraline for waste water.

Analysis of DDT and its metabolites in soil and water samples obtained in the vicinity of a closed-down factory in Bangladesh using various extraction methods.

PubMed

Al Mahmud, M N U; Khalil, Farzana; Rahman, Md Musfiqur; Mamun, M I R; Shoeb, Mohammad; Abd El-Aty, A M; Park, Jong-Hyouk; Shin, Ho-Chul; Nahar, Nilufar; Shim, Jae-Han

2015-12-01

This study was conducted to monitor the spread of dichlorodiphenyltrichloroethane (DDT) and its metabolites (dichlorodiphenyldichloroethylene (DDE), dichlorodiphenyldichloroethane (DDD)) in soil and water to regions surrounding a closed DDT factory in Bangladesh. This fulfillment was accomplished using inter-method and inter-laboratory validation studies. DDTs (DDT and its metabolites) from soil samples were extracted using microwave-assisted extraction (MAE), supercritical fluid extraction (SFE), and solvent extraction (SE). Inter-laboratory calibration was assessed by SE, and all methods were validated by intra- and inter-day accuracy (expressed as recovery %) and precision (expressed as relative standard deviation (RSD)) in the same laboratory, at three fortified concentrations (n = 4). DDTs extracted from water samples by liquid-liquid partitioning and all samples were analyzed by gas chromatography (GC)-electron capture detector (ECD) and confirmed by GC/mass spectrometry (GC/MS). Linearities expressed as determination coefficients (R (2)) were ≥0.995 for matrix-matched calibrations. The recovery rate was in the range of 72-120 and 83-110%, with <15% RSD in soil and water, respectively. The limit of quantification (LOQ) was 0.0165 mg kg(-1) in soil and 0.132 μg L(-1) in water. Greater quantities of DDTs were extracted from soil using the MAE and SE techniques than with the SFE method. Higher amounts of DDTs were discovered in the southern (2.2-936 × 10(2) mg kg(-1)) or southwestern (86.3-2067 × 10(2) mg kg(-1)) direction from the factory than in the eastern direction (1.0-48.6 × 10(2) mg kg(-1)). An exception was the soil sample collected 50 ft (15.24 m) east (2904 × 10(2) mg kg(-1)) of the factory. The spread of DDTs in the water bodies (0.59-3.01 μg L(-1)) was approximately equal in all directions. We concluded that DDTs might have been dumped randomly around the warehouse after the closing of the factory.

Extraction of pesticides, dioxin-like PCBs and PAHs in water based commodities using liquid-liquid microextraction and analysis by gas chromatography-mass spectrometry.

PubMed

Dasgupta, Soma; Banerjee, Kaushik; Utture, Sagar; Kusari, Parijat; Wagh, Sameer; Dhumal, Kondiba; Kolekar, Sanjay; Adsule, Pandurang G

2011-09-23

Water based samples such as flavored drinks, juices and drinking water may contain contaminants at ultra trace level belonging to different chemical classes. A novel, simple, low-cost and fast method was developed and validated for trace residue extraction of pesticides, dioxin-like PCBs and PAHs from water and water based samples followed by analysis through gas chromatography (GC) coupled with time-of-flight mass spectrometry (ToFMS). The extraction solvent type, volume; sample volume and other extraction conditions were optimized. This was achieved by extracting 10 mL sample with 250 μL chloroform by vortexing (1 min, standing time of 2 min) followed by centrifugation (6000 rpm, 5 min). The bottom organic layer (200 μL) was pipetted out, evaporated to near dryness and reconstituted in 20 μL of ethyl acetate+cyclohexane (1:9) mixture resulting in an enrichment factor of 400. The recoveries of all compounds were within 76-120% (±10%) with the method detection limit (MDL) ranging from 1 to 250 ng/L depending on the analyte response. The MDLs were 400 times lower than the instrument quantification limits that ranged from 0.4 to 100 ng/mL. The method was further validated in water based drinks (e.g. apple, lemon, pineapple, orange, grape and pomegranate juice). For the juices with suspended pulp, the extraction was carried out with 400 μL chloroform. The extract was analyzed by GC-ToFMS at both 1D and GC×GC modes to chromatographically separate closely eluting interfering compounds the effect of which could not be minimized otherwise. The resulting peak table was filtered to identify a range of compounds belonging to specific classes viz. polycyclic aromatic hydrocarbons, chlorinated, brominated, and nitro compounds. User developed scripts were employed on the basis of identification of the molecular ion and isotope clusters or other spectral characteristics. The method performed satisfactorily in analyzing both incurred as well as market samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Regional water-quality analysis of 2,4-D and dicamba in river water using gas chromatography-isotope dilution mass spectrometry

USGS Publications Warehouse

Thurman, E.M.; Zimmerman, L.R.; Aga, D.S.; Gilliom, R.J.

2001-01-01

Gas chromatography with isotope dilution mass spectrometry (GC-MS) and enzyme-linked immunosorbent assay (ELISA) were used in regional National Water Quality Assessment studies of the herbicides, 2,4-D and dicamba, in river water across the United States. The GC-MS method involved solid-phase extraction, derivatized with deutemted 2,4-D, and analysis by selected ion monitoring. The ELISA method was applied after preconcentration with solid-phase extraction. The ELISA method was unreliable because of interference from humic substances that were also isolated by solid-phase extraction. Therefore, GC-MS was used to analyzed 80 samples from river water from 14 basins. The frequency of detection of dicamba (28%) was higher than that for 2,4-D (16%). Concentrations were higher for dicamba than for 2,4-D, ranging from less than the detection limit (<0.05 ??g/L) to 3.77 ??g/L, in spite of 5 times more annual use of 2,4-D as compared to dicamba. These results suggest that 2,4-D degrades more rapidly in the environment than dicamba.

Automatic sub-pixel coastline extraction based on spectral mixture analysis using EO-1 Hyperion data

NASA Astrophysics Data System (ADS)

Hong, Zhonghua; Li, Xuesu; Han, Yanling; Zhang, Yun; Wang, Jing; Zhou, Ruyan; Hu, Kening

2018-06-01

Many megacities (such as Shanghai) are located in coastal areas, therefore, coastline monitoring is critical for urban security and urban development sustainability. A shoreline is defined as the intersection between coastal land and a water surface and features seawater edge movements as tides rise and fall. Remote sensing techniques have increasingly been used for coastline extraction; however, traditional hard classification methods are performed only at the pixel-level and extracting subpixel accuracy using soft classification methods is both challenging and time consuming due to the complex features in coastal regions. This paper presents an automatic sub-pixel coastline extraction method (ASPCE) from high-spectral satellite imaging that performs coastline extraction based on spectral mixture analysis and, thus, achieves higher accuracy. The ASPCE method consists of three main components: 1) A Water- Vegetation-Impervious-Soil (W-V-I-S) model is first presented to detect mixed W-V-I-S pixels and determine the endmember spectra in coastal regions; 2) The linear spectral mixture unmixing technique based on Fully Constrained Least Squares (FCLS) is applied to the mixed W-V-I-S pixels to estimate seawater abundance; and 3) The spatial attraction model is used to extract the coastline. We tested this new method using EO-1 images from three coastal regions in China: the South China Sea, the East China Sea, and the Bohai Sea. The results showed that the method is accurate and robust. Root mean square error (RMSE) was utilized to evaluate the accuracy by calculating the distance differences between the extracted coastline and the digitized coastline. The classifier's performance was compared with that of the Multiple Endmember Spectral Mixture Analysis (MESMA), Mixture Tuned Matched Filtering (MTMF), Sequential Maximum Angle Convex Cone (SMACC), Constrained Energy Minimization (CEM), and one classical Normalized Difference Water Index (NDWI). The results from the three test sites indicated that the proposed ASPCE method extracted coastlines more efficiently than did the compared methods, and its coastline extraction accuracy corresponded closely to the digitized coastline, with 0.39 pixels, 0.40 pixels, and 0.35 pixels in the three test regions, showing that the ASPCE method achieves an accuracy below 12.0 m (0.40 pixels). Moreover, in the quantitative accuracy assessment for the three test sites, the ASPCE method shows the best performance in coastline extraction, achieving a 0.35 pixel-level at the Bohai Sea, China test site. Therefore, the proposed ASPCE method can extract coastline more accurately than can the hard classification methods or other spectral unmixing methods.

Phytochemical screening, anti-oxidant activity and in vitro anticancer potential of ethanolic and water leaves extracts of Annona muricata (Graviola).

PubMed

Gavamukulya, Yahaya; Abou-Elella, Faten; Wamunyokoli, Fred; AEl-Shemy, Hany

2014-09-01

To determine the phytochemical composition, antioxidant and anticancer activities of ethanolic and water leaves extracts of Annona muricata (A. muricata) from the Eastern Uganda. Phytochemical screening was conducted using standard qualitative methods and a Chi-square goodness of fit test was used to assign the relative abundance of the different phytochemicals. The antioxidant activity was determined using the 2, 2-diphenyl-2-picrylhydrazyl and reducing power methods whereas the in vitro anticancer activity was determined using three different cell lines. Phytochemical screening of the extracts revealed that they were rich in secondary class metabolite compounds such as alkaloids, saponins, terpenoids, flavonoids, coumarins and lactones, anthraquinones, tannins, cardiac glycosides, phenols and phytosterols. Total phenolics in the water extract were (683.69±0.09) μg/mL gallic acid equivalents (GAE) while it was (372.92±0.15) μg/mL GAE in the ethanolic extract. The reducing power was 216.41 μg/mL in the water extract and 470.51 μg/mL GAE in the ethanolic extract. In vitro antioxidant activity IC50 was 2.0456 mg/mL and 0.9077 mg/mL for ethanolic and water leaves extracts of A. muricata respectively. The ethanolic leaves extract was found to be selectively cytotoxic in vitro to tumor cell lines (EACC, MDA and SKBR3) with IC50 values of 335.85 μg/mL, 248.77 μg/mL, 202.33 μg/mL respectively, while it had no cytotoxic effect on normal spleen cells. The data also showed that water leaves extract of A. muricata had no anticancer effect at all tested concentrations. The results showed that A. muricata was a promising new antioxidant and anticancer agent. Copyright © 2014 Hainan Medical College. Published by Elsevier B.V. All rights reserved.

Data for the geochemical investigation of UMTRAP designated site at Durango, Colorado

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

Markos, G.; Bush, K.J.

1983-09-01

This report contains the methods of collection and the data used in the geochemical investigation of the former tailings and raffinate pond sites at Durango, Colorado. The methods of data interpretation and results of the investigation are described in the report, ''Geochemical Investigation of UMTRAP Designated Site at Durango, Colorado''. Data are from a one-time sampling of waters and solid material from the background, the area adjacent to the site, and the site. The solid samples are water extracted to remove easily soluble salts and acid extracted to remove carbonates and hydroxides. The waters, extracts, and solid samples were analyzedmore » for selected major and trace elements. A few samples were analyzed for radioisotopes.« less

Different activities of Schinus areira L.: anti-inflammatory or pro-inflammatory effect.

PubMed

Davicino, R; Mattar, A; Casali, Y; Anesini, C; Micalizzi, B

2010-12-01

The anti-inflammatory drugs possess many serious side effects at doses commonly prescribed. It is really important to discover novel regulators of inflammation from natural sources with minimal adverse effects. Schinus areira L. is a plant native from South America and is used in folk medicine as an anti-inflammatory herb. For this study, the activity of aqueous extracts on inflammation and the effect on superoxide anion production in mice macrophages were assayed. Aqueous extracts were prepared by soaking herbs in cold water (cold extract), boiling water (infusion), and simmering water (decoction). Cold extract possess an anti-inflammatory activity. Decoction and infusion showed pro-inflammatory activity. Cold extract increased the production of superoxide anion. It has been proposed to use diverse methods to obtain extracts of S. areira L. with different effects. Cold extract, decoction, and infusion could be utilized as extracts or as pharmacological preparations for topical application.

Comparison of ambient solvent extraction methods for the analysis of fatty acids in non-starch lipids of flour and starch

PubMed Central

Bahrami, Niloufar; Yonekura, Lina; Linforth, Robert; Carvalho da Silva, Margarida; Hill, Sandra; Penson, Simon; Chope, Gemma; Fisk, Ian Denis

2014-01-01

BACKGROUND Lipids are minor components of flours, but are major determinants of baking properties and end-product quality. To the best of our knowledge, there is no single solvent system currently known that efficiently extracts all non-starch lipids from all flours without the risk of chemical, mechanical or thermal damage. This paper compares nine ambient solvent systems (monophasic and biphasic) with varying polarities: Bligh and Dyer (BD); modified Bligh and Dyer using HCl (BDHCL); modified BD using NaCl (BDNaCl); methanol–chloroform–hexane (3:2:1, v/v); Hara and Radin (hexane–isopropanol, 3:2, v/v); water-saturated n-butanol; chloroform; methanol and hexane for their ability to extract total non-starch lipids (separated by lipid classes) from wheat flour (Triticum aestivum L.). Seven ambient extraction protocols were further compared for their ability to extract total non-starch lipids from three alternative samples: barley flour (Hordeum vulgare L.), maize starch (Zea mays L.) and tapioca starch (Manihot esculenta Crantz). RESULTS For wheat flour the original BD method and those containing HCl or NaCl tended to extract the maximum lipid and a significant correlation between lipid extraction yield (especially the glycolipids and phospholipids) and the polarity of the solvent was observed. For the wider range of samples BD and BD HCl repeatedly offered the maximum extraction yield and using pooled standardized (by sample) data from all flours, total non-starch lipid extraction yield was positively correlated with solvent polarity (r = 0.5682, P < 0.05) and water ratio in the solvent mixture (r = 0.5299, P < 0.05). CONCLUSION In general, BD-based methods showed better extraction yields compared to methods without the addition of water and, most interestingly, there was much greater method dependence of lipid yields in the starches when compared to the flour samples, which is due to the differences in lipid profiles between the two sample types (flours and starches). PMID:24132804

Ultrasound-Assisted Extraction of Stilbenes from Grape Canes.

PubMed

Piñeiro, Zulema; Marrufo-Curtido, Almudena; Serrano, Maria Jose; Palma, Miguel

2016-06-16

An analytical ultrasound-assisted extraction (UAE) method has been optimized and validated for the rapid extraction of stilbenes from grape canes. The influence of sample pre-treatment (oven or freeze-drying) and several extraction variables (solvent, sample-solvent ratio and extraction time between others) on the extraction process were analyzed. The new method allowed the main stilbenes in grape canes to be extracted in just 10 min, with an extraction temperature of 75 °C and 60% ethanol in water as the extraction solvent. Validation of the extraction method was based on analytical properties. The resulting RSDs (n = 5) for interday/intraday precision were less than 10%. Furthermore, the method was successfully applied in the analysis of 20 different grape cane samples. The result showed that grape cane byproducts are potentially sources of bioactive compounds of interest for pharmaceutical and food industries.

Deep eutectic solvents as efficient solvent system for the extraction of κ-carrageenan from Kappaphycus alvarezii.

PubMed

Das, Arun Kumar; Sharma, Mukesh; Mondal, Dibyendu; Prasad, Kamalesh

2016-01-20

Three different deep eutectic solvents (DESs) prepared by the complexation of choline chloride with urea, ethylene glycol and glycerol along with their hydrated counterparts were used for the selective extraction of κ-carrageenan from Kappaphycus alvarezii. Upon comparison of the quality of the polysaccharide with the one obtained using water as extraction media as well as the one extracted using widely practiced conventional method, it was found that, the physicochemical as well as rheological properties of κ-carrageenan obtained using DESs as solvents was at par to the one obtained using conventional method and was superior in quality when compared to κ-carrageenan obtained using water as solvent. Considering the tedious nature of the extraction method employed in conventional extraction process, the DESs can be considered as suitable alternative solvents for the facile extraction of the polysaccharide directly from the seaweed. However, among the hydrated and non-hydrated DESs, the hydrated ones were found to be more effective in comparison to their non-hydrated counterparts. Copyright © 2015 Elsevier Ltd. All rights reserved.

Ionic liquid-impregnated agarose film two-phase micro-electrodriven membrane extraction (IL-AF-μ-EME) for the analysis of antidepressants in water samples.

PubMed

Mohamad Hanapi, Nor Suhaila; Sanagi, Mohd Marsin; Ismail, Abd Khamim; Wan Ibrahim, Wan Aini; Saim, Nor'ashikin; Wan Ibrahim, Wan Nazihah

2017-03-01

The aim of this study was to investigate and apply supported ionic liquid membrane (SILM) in two-phase micro-electrodriven membrane extraction combined with high performance liquid chromatography-ultraviolet detection (HPLC-UV) for pre-concentration and determination of three selected antidepressant drugs in water samples. A thin agarose film impregnated with 1-hexyl-3-methylimidazolium hexafluorophosphate, [C 6 MIM] [PF 6 ], was prepared and used as supported ionic liquid membrane between aqueous sample solution and acceptor phase for extraction of imipramine, amitriptyline and chlorpromazine. Under the optimized extraction conditions, the method provided good linearity in the range of 1.0-1000μgL -1 , good coefficients of determination (r 2 =0.9974-0.9992) and low limits of detection (0.1-0.4μgL -1 ). The method showed high enrichment factors in the range of 110-150 and high relative recoveries in the range of 88.2-111.4% and 90.9-107.0%, for river water and tap water samples, respectively with RSDs of ≤7.6 (n=3). This method was successfully applied to the determination of the drugs in river and tap water samples. It is envisaged that the SILM improved the perm-selectivity by providing a pathway for targeted analytes which resulted in rapid extraction with high degree of selectivity and high enrichment factor. Copyright © 2017 Elsevier B.V. All rights reserved.

Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

PubMed

Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

2013-12-15

A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Micro-solid phase extraction of benzene, toluene, ethylbenzene and xylenes from aqueous solutions using water-insoluble β-cyclodextrin polymer as sorbent.

PubMed

Nojavan, Saeed; Yazdanpanah, Mina

2017-11-24

Water-insoluble β-cyclodextrin polymer was synthesized by chemical cross-linking using epichlorohydrin (EPI) as a cross-linker agent. The produced water-insoluble polymer was used as a sorbent for the micro-solid phase extraction (μ-SPE) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water samples. The μ-SPE device consisted of a sealed tea bag envelope containing 15mg of sorbent. For the evaluation of the extraction efficiency, parameters such as extraction and desorption time, desorption solvent and salt concentration were investigated. At an extraction time of 30min in the course of the extraction process, analytes were extracted from a 10mL aqueous sample solution. The analytes were desorbed by ultrasonication in 200μL of acetonitrile for 20min. Analysis of the analytes was done by a gas chromatography-flame ionization detector (GC-FID) system. The enrichment factor (EF) was found to be in the range 23.0-45.4 (EF max =50.0). The method provided linearity ranges of between 0.5 and 500.0ng/mL (depending on the analytes), with good coefficients of determination (r 2 ) ranging between 0.997 and 0.999 under optimized conditions. Detection limits for BTEX were in the range of between 0.15 and 0.60ng/mL, while corresponding recoveries were in the range of 46.0-90.0%. The relative standard deviation of the method for the analytes at 100.0ng/mL concentration level ranged from 5.5 to 11.2% (n=5). The proposed method was concluded to be a cost effective and environmentally-friendly extraction technique with ease of operation and minimal usage of organic solvent. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwave Extraction of Lunar Water for Rocket Fuel

NASA Technical Reports Server (NTRS)

Ethridge, Edwin C.; Donahue, Benjamin; Kaukler, William

2008-01-01

Nearly 50% of the lunar surface is oxygen, present as oxides in silicate rocks and soil. Methods for reduction of these oxides could liberate the oxygen. Remote sensing has provided evidence of significant quantities of hydrogen possibly indicating hundreds of millions of metric tons, MT, of water at the lunar poles. If the presence of lunar water is verified, water is likely to be the first in situ resource exploited for human exploration and for LOX-H2 rocket fuel. In-Situ lunar resources offer unique advantages for space operations. Each unit of product produced on the lunar surface represents 6 units that need not to be launched into LEO. Previous studies have indicated the economic advantage of LOX for space tugs from LEO to GEO. Use of lunar derived LOX in a reusable lunar lander would greatly reduce the LEO mass required for a given payload to the moon. And Lunar LOX transported to L2 has unique advantages for a Mars mission. Several methods exist for extraction of oxygen from the soil. But, extraction of lunar water has several significant advantages. Microwave heating of lunar permafrost has additional important advantages for water extraction. Microwaves penetrate and heat from within not just at the surface and excavation is not required. Proof of concept experiments using a moon in a bottle concept have demonstrated that microwave processing of cryogenic lunar permafrost simulant in a vacuum rapidly and efficiently extracts water by sublimation. A prototype lunar water extraction rover was built and tested for heating of simulant. Microwave power was very efficiently delivered into a simulated lunar soil. Microwave dielectric properties (complex electric permittivity and magnetic permeability) of lunar regolith simulant, JSC-1A, were measured down to cryogenic temperatures and above room temperature. The microwave penetration has been correlated with the measured dielectric properties. Since the microwave penetration depth is a function of temperature and frequency, an extraction system can be designed for water removal from different depths.

Multi-laboratory survey of qPCR enterococci analysis method performance

EPA Pesticide Factsheets

Quantitative polymerase chain reaction (qPCR) has become a frequently used technique for quantifying enterococci in recreational surface waters, but there are several methodological options. Here we evaluated how three method permutations, type of mastermix, sample extract dilution and use of controls in results calculation, affect method reliability among multiple laboratories with respect to sample interference. Multiple samples from each of 22 sites representing an array of habitat types were analyzed using EPA Method 1611 and 1609 reagents with full strength and five-fold diluted extracts. The presence of interference was assessed three ways: using sample processing and PCR amplifications controls; consistency of results across extract dilutions; and relative recovery of target genes from spiked enterococci in water sample compared to control matrices with acceptable recovery defined as 50 to 200%. Method 1609, which is based on an environmental mastermix, was found to be superior to Method 1611, which is based on a universal mastermix. Method 1611 had over a 40% control assay failure rate with undiluted extracts and a 6% failure rate with diluted extracts. Method 1609 failed in only 11% and 3% of undiluted and diluted extracts analyses. Use of sample processing control assay results in the delta-delta Ct method for calculating relative target gene recoveries increased the number of acceptable recovery results. Delta-delta tended to bias recoveries fr

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

NASA Astrophysics Data System (ADS)

Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

2018-01-01

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

Coupling of multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction with pulse glow discharge-ion mobility spectrometry for analysis of triazine herbicides in water and soil samples.

PubMed

Zou, Nan; Yuan, Chunhao; Liu, Shaowen; Han, Yongtao; Li, Yanjie; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

2016-07-29

An analytical method based on stir bar sorptive extraction (SBSE) coupled with pulse glow discharge-ion mobility spectrometry (PGD-IMS) was developed for analysis of three triazine pesticide residues in water and soil samples. An injection port with sealing device and stir bars hold device were designed and constructed to directly position the SBSE fiber including the extracted samples into the heating device, making desorption and detection of analytes proceeded simultaneously. The extraction conditions such as SBSE solid phase material, extraction time, extraction temperature, pH value and salt concentration were optimized. Mixture of MWCNTs-COOH and PDMS were shown to be effective in enriching the triazines. The LODs and LOQs of three triazines were found to be 0.006-0.015μgkg(-1) and 0.02-0.05μgkg(-1), and the linear range was 0.05-10μgL(-1) with determination coefficients from 0.9987 to 0.9993. The SBSE-PGD-IMS method was environmentally friendly without organic solvent consumption in the entire experimental procedures, and it was demonstrated to be a commendable rapid analysis technique for analysis of triazine pesticide residues in environmental samples on site. The proposed method was applied for the analysis of real ground water, surface water and soil samples. Copyright © 2016 Elsevier B.V. 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.

Effect of gamma irradiation on the extraction yield, antioxidant, and antityrosinase activities of pistachio green hull extract

NASA Astrophysics Data System (ADS)

Abolhasani, Ali; Barzegar, Mohsen; Sahari, Mohammad Ali

2018-03-01

In this study, the antioxidant activity and tyrosinase inhibitory of non-irradiated and irradiated pistachio green hull (PGH) extracts were investigated. After irradiation of PGH by different doses of gamma ray (0, 10, 20, 30 and 40 kGy), their phenolic compounds were extracted by water. Antioxidant activities of extracts were examined by DPPH• and FRAP methods. The results showed that irradiation not only do not have negative effects on antioxidant activity but also it can increase the amount of total phenolic compounds of water extract in comparison with non-irradiated sample. Water extract of irradiated PGH at the dose of 30 kGy, showed the highest antioxidant activity in the DPPH° test with EC50 equal to 289.0 ± 1.2 μg/ml. Irradiated (30 kGy) and non-irradiated water extracts had the highest antityrosinase activities with IC50 of 10.8 ± 1.1 and 11.9 ± 1.2 μg phenolic/ml, respectively. In addition, it was found that the water extract of irradiated PGH can prevent enzymatic browning in sliced raw potatoes. According to the antityrosinase potential of PGH extract, it may be suggested as an antibrowning agent in some foodstuffs or cosmetic products.

Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

PubMed

Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

2016-05-15

A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of intracellular and extracellular microcystin variants in sediments and pore waters by accelerated solvent extraction and high performance liquid chromatography-tandem mass spectrometry.

PubMed

Zastepa, Arthur; Pick, Frances R; Blais, Jules M; Saleem, Ammar

2015-05-04

The fate and persistence of microcystin cyanotoxins in aquatic ecosystems remains poorly understood in part due to the lack of analytical methods for microcystins in sediments. Existing methods have been limited to the extraction of a few extracellular microcystins of similar chemistry. We developed a single analytical method, consisting of accelerated solvent extraction, hydrophilic-lipophilic balance solid phase extraction, and reversed phase high performance liquid chromatography-tandem mass spectrometry, suitable for the extraction and quantitation of both intracellular and extracellular cyanotoxins in sediments as well as pore waters. Recoveries of nine microcystins, representing the chemical diversity of microcystins, and nodularin (a marine analogue) ranged between 75 and 98% with one, microcystin-RR (MC-RR), at 50%. Chromatographic separation of these analytes was achieved within 7.5 min and the method detection limits were between 1.1 and 2.5 ng g(-1) dry weight (dw). The robustness of the method was demonstrated on sediment cores collected from seven Canadian lakes of diverse geography and trophic states. Individual microcystin variants reached a maximum concentration of 829 ng g(-1) dw on sediment particles and 132 ng mL(-1) in pore waters and could be detected in sediments as deep as 41 cm (>100 years in age). MC-LR, -RR, and -LA were more often detected while MC-YR, -LY, -LF, and -LW were less common. The analytical method enabled us to estimate sediment-pore water distribution coefficients (K(d)), MC-RR had the highest affinity for sediment particles (log K(d)=1.3) while MC-LA had the lowest affinity (log K(d)=-0.4), partitioning mainly into pore waters. Our findings confirm that sediments serve as a reservoir for microcystins but suggest that some variants may diffuse into overlying water thereby constituting a new route of exposure following the dissipation of toxic blooms. The method is well suited to determine the fate and persistence of different microcystins in aquatic systems. Copyright © 2015 Elsevier B.V. All rights reserved.

Detergentless ultrasound-assisted extraction of trace elements from edible oils using lipase as an extractant.

PubMed

Kara, Derya; Fisher, Andrew; Hill, Steve

2015-11-01

A new method for the extraction and preconcentration of trace elements (Al, Ba, Cd, Cu, Fe, Mn, Mo, Ni, Ti, V and Zn) from edible oils by producing detergentless micro-emulsions via an ultrasound-assisted extraction using a water phase containing Lipase at pH 3 as an extractant was developed. The trace elements in the water phase post-extraction were determined against matrix matched standards using ICP-MS. In the first step of the work, the parameters that affect extraction, such as pH, the volume of 1% lipase in the water phase and the ultrasonic and centrifugation times were optimized. Under the optimal conditions, the detection limits (µg kg(-1)) were 0.46, 0.03, 0.007, 0.028, 0.67, 0.038, 0.022, 0.14, 0.17, 0.05 and 0.07 for Al, Ba, Cd, Cu, Fe, Mn, Mo, Ni, Ti, V and Zn respectively for edible oils (3 Sb/m). A certified reference material (EnviroMAT HU-1 Used oil) was analysed to check the accuracy of the developed method. Results obtained were in agreement with certified values with a t-test showing that no significant differences at the 95% confidence levels were found. The proposed method was applied to different edible oils such as sunflower oil, rapeseed oil, olive oil and salmon oil. Copyright © 2015 Elsevier B.V. All rights reserved.

Dispersive liquid-phase microextraction with solidification of floating organic droplet coupled with high-performance liquid chromatography for the determination of Sudan dyes in foodstuffs and water samples.

PubMed

Chen, Bo; Huang, Yuming

2014-06-25

Dispersive liquid-phase microextraction with solidification of floating organic drop (SFO-DLPME) is one of the most interesting sample preparation techniques developed in recent years. In this paper, a new, rapid, and efficient SFO-DLPME coupled with high-performance liquid chromatography (HPLC) was established for the extraction and sensitive detection of banned Sudan dyes, namely, Sudan I, Sudan II, Sudan III, and Sudan IV, in foodstuff and water samples. Various factors, such as the type and volume of extractants and dispersants, pH and volume of sample solution, extraction time and temperature, ion strength, and humic acid concentration, were investigated and optimized to achieve optimal extraction of Sudan dyes in one single step. After optimization of extraction conditions using 1-dodecanol as an extractant and ethanol as a dispersant, the developed procedure was applied for extraction of the target Sudan dyes from 2 g of food samples and 10 mL of the spiked water samples. Under the optimized conditions, all Sudan dyes could be easily extracted by the proposed SFO-DLPME method. Limits of detection of the four Sudan dyes obtained were 0.10-0.20 ng g(-1) and 0.03 μg L(-1) when 2 g of foodstuff samples and 10 mL of water samples were adopted, respectively. The inter- and intraday reproducibilities were below 4.8% for analysis of Sudan dyes in foodstuffs. The method was satisfactorily used for the detection of Sudan dyes, and the recoveries of the target for the spiked foodstuff and water samples ranged from 92.6 to 106.6% and from 91.1 to 108.6%, respectively. These results indicated that the proposed method is simple, rapid, sensitive, and suitable for the pre-concentration and detection of the target dyes in foodstuff samples.

Determination of phthalic acid esters in water samples by hollow fiber liquid-phase microextraction prior to gas chromatography tandem mass spectrometry.

PubMed

González-Sálamo, Javier; González-Curbelo, Miguel Ángel; Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel

2018-06-01

A new hollow fiber liquid-phase microextraction (HF-LPME) method has been developed for the extraction of a group of phthalic acid esters (PAEs) of interest from different water samples prior to gas chromatography tandem mass spectrometry analysis. HF-LPME was carried out using 1-octanol as extraction solvent followed by a back extraction step with cyclohexane. The different parameters that affect HF-LPME such as sample pH, ionic strength, extraction time, stirring rate, extraction temperature and back extraction conditions were investigated. The optimized conditions involved the extraction of 10 mL of sample without pH adjustment or addition of salt during 75 min under a stirring of 850 rpm at 60 °C and subsequent desorption with 200 μL of cyclohexane for 10 min in an ultrasonic bath. The method was validated in terms of calibration and recovery studies using dibutyl phthalate-d 4 as internal standard. The developed procedure gave satisfactory recovery (74-120%) and relative standard deviation values (<20%) for the studied PAEs in mineral, tap, pond and waste water samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

[The determination of the herbicide glyphosate and its chief metabolite aminomethylphosphonic acid (AMPA) in drinking water with the aid of HPLC].

PubMed

Gauch, R; Leuenberger, U; Müller, U

1989-01-01

A method for the determination of glyphosate and its major metabolite aminomethylphosphonic acid (AMPA) is described. With a detection limit of 0.02 microgram/l, the method suitably fulfills the requirements of the Swiss legislation (tolerance value of 0.1 micrograms/l water). The compounds are derivatized directly in the original water sample with 9-fluorenylmethyl chloroformate (FMOCC1) in order to obtain extractable and fluorescent derivatives. These are extracted with organic solvents and determined by HPLC using a fluorescence detector. Neither of the compounds could be detected in 151 tap water samples from the Canton of Berne.

Determination of traces of silver in waters by anion exchange and atomic absorption spectrophotometry

USGS Publications Warehouse

Chao, T.T.; Fishman, M. J.; Ball, J.W.

1969-01-01

A method has been developed for the accurate determination of 0.1-1 ??g of silver per liter of water. The method permits stabilization of silver in water without loss to container walls. Optimum conditions have been established for the complete recovery of silver from water with an anion-exchange column, for quantitative elution of silver from the resin, and for measurement of silver by atomic absorption spectrophotometry after chelation with ammonium pyrrolidine dithiocarbamate and extraction of the chelate with MIBK. Silver in the 1-10 ??g 1 range can be determined by extraction without pre-concentration on an ion-exchange resin. ?? 1969.

Combination of artificial neural network and genetic algorithm method for modeling of methylene blue adsorption onto wood sawdust from water samples.

PubMed

Khajeh, Mostafa; Sarafraz-Yazdi, Ali; Natavan, Zahra Bameri

2016-03-01

The aim of this research was to develop a low price and environmentally friendly adsorbent with abundant of source to remove methylene blue (MB) from water samples. Sawdust solid-phase extraction coupled with high-performance liquid chromatography was used for the extraction and determination of MB. In this study, an experimental data-based artificial neural network model is constructed to describe the performance of sawdust solid-phase extraction method for various operating conditions. The pH, time, amount of sawdust, and temperature were the input variables, while the percentage of extraction of MB was the output. The optimum operating condition was then determined by genetic algorithm method. The optimized conditions were obtained as follows: 11.5, 22.0 min, 0.3 g, and 26.0°C for pH of the solution, extraction time, amount of adsorbent, and temperature, respectively. Under these optimum conditions, the detection limit and relative standard deviation were 0.067 μg L(-1) and <2.4%, respectively. The Langmuir and Freundlich adsorption models were applied to describe the isotherm constant and for the removal and determination of MB from water samples. © The Author(s) 2013.

A sensitive multi-residue method for the determination of 35 micropollutants including pharmaceuticals, iodinated contrast media and pesticides in water.

PubMed

Valls-Cantenys, Carme; Scheurer, Marco; Iglesias, Mònica; Sacher, Frank; Brauch, Heinz-Jürgen; Salvadó, Victoria

2016-09-01

A sensitive, multi-residue method using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to determine a representative group of 35 analytes, including corrosion inhibitors, pesticides and pharmaceuticals such as analgesic and anti-inflammatory drugs, five iodinated contrast media, β-blockers and some of their metabolites and transformation products in water samples. Few other methods are capable of determining such a broad range of contrast media together with other analytes. We studied the parameters affecting the extraction of the target analytes, including sorbent selection and extraction conditions, their chromatographic separation (mobile phase composition and column) and detection conditions using two ionisation sources: electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI). In order to correct matrix effects, a total of 20 surrogate/internal standards were used. ESI was found to have better sensitivity than APCI. Recoveries ranging from 79 to 134 % for tap water and 66 to 144 % for surface water were obtained. Intra-day precision, calculated as relative standard deviation, was below 34 % for tap water and below 21 % for surface water, groundwater and effluent wastewater. Method quantification limits (MQL) were in the low ng L(-1) range, except for the contrast agents iomeprol, amidotrizoic acid and iohexol (22, 25.5 and 17.9 ng L(-1), respectively). Finally, the method was applied to the analysis of 56 real water samples as part of the validation procedure. All of the compounds were detected in at least some of the water samples analysed. Graphical Abstract Multi-residue method for the determination of micropollutants including pharmaceuticals, iodinated contrast media and pesticides in waters by LC-MS/MS.

A SUSTAINABLE METHOD OF WATER EXTRACTION FOR SCHOOL-COMMUNITY GARDENS IN NIGER, WEST AFRICA

EPA Science Inventory

The challenge of this project is significant in the developing world, specifically in the Air Massif region of Niger, the poorest country in the world. A sustainable water extraction system is needed to irrigate community gardens. These gardens produce a basic need, food, for ...

Extraction optimization and influences of drying methods on antioxidant activities of polysaccharide from cup plant (Silphium perfoliatum L.)

PubMed Central

Li, Ran; Duan, Meng-Ying; Wu, Hong-Xin

2017-01-01

Response surface methodology (RSM) was used to investigate the extraction condition of polysaccharide from cup plant (Silphium perfoliatum L.) (named CPP). Water to raw material ratio (10–30 mL/g), extraction time (40–80 min) and extraction temperature (60–100°C) were set as the 3 independent variables, and their effects on the extraction yield of CPP were measured. In addition, the effects of drying methods including hot air drying (HD), vacuum drying (VD) and freeze drying (FD) on the antioxidant activities of CPP were evaluated. The results showed that the optimal condition to extract CPP was: water to raw material ratio (15 mL/g), extraction time (61 min), and extraction temperature (97°C), a maximum CPP yield of 6.49% was obtained under this condition. CPP drying with FD method showed stronger reducing power (0.943 at 6 mg/mL) and radical scavenging capacities against DPPH radical (75.71% at 1.2 mg/mL) and ABTS radical (98.06 at 1.6 mg/mL) than CPP drying with HD and VD methods. Therefore, freeze drying served as a good method for keeping the antioxidant activities of polysaccharide from cup plant. The polysaccharide from cup plant has potential to use as a natural antioxidant. PMID:28837625

A METHOD FOR AUTOMATED ANALYSIS OF 10 ML WATER SAMPLES CONTAINING ACIDIC, BASIC, AND NEUTRAL SEMIVOLATILE COMPOUNDS LISTED IN USEPA METHOD 8270 BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GAS CHROMATOGRAPHY/MASS SPECTROMETRY

EPA Science Inventory

Data is presented showing the progress made towards the development of a new automated system combining solid phase extraction (SPE) with gas chromatography/mass spectrometry for the single run analysis of water samples containing a broad range of acid, base and neutral compounds...

Concentration of organic compounds in natural waters with solid-phase dispersion based on advesicle modified silica prior to liquid chromatography.

PubMed

Parisis, Nikolaos A; Giokas, Dimosthenis L; Vlessidis, Athanasios G; Evmiridis, Nicholaos P

2005-12-02

The ability of vesicle-coated silica to aid the extraction of organic compounds from water prior to liquid chromatographic analysis is presented for the first time. The method is based on the formation of silica supported cationic multi-lamellar vesicles of gemini surfactants inherently ensuring the presence of hydrophilic and hydrophobic sites for the partitioning of analytes bearing different properties. Method development is illustrated by studying the adsolubilization of UV absorbing chemicals from swimming pool water. Due to the requirement for external energy input (intense shearing) a method based on solid-phase dispersion (SPD) was applied producing better results than off-line solid-phase extraction (SPE). Meticulous investigation of the experimental parameters was conducted in order to elucidate the mechanisms behind the proposed extraction pattern. Analyte recoveries were quantitative under the optimum experimental conditions offering recoveries higher than 96% with RSD values below 5%.

A comparison of methods for concentrating mutagens in drinking water--recovery aspects and their implications for the chemical character of major unidentified mutagens.

PubMed

Wigilius, B; Borén, H; Carlberg, G E; Grimvall, A; Möller, M

1985-12-01

A comparison of techniques for concentrating mutagenic compounds in drinking water has shown that XAD-2 adsorption and dichloromethane extraction have acceptable and almost identical enrichment properties, while purging at an elevated temperature is inappropriate in this context. Quantitatively, the most important drinking water mutagens could only be adsorbed (extracted) after acidification of the water, and even then recovery was far from complete. Recovery experiments with known mutagens from pulp mill effluents have shown that none of the major chlorination-stage mutagens identified thus far can explain the mutagenic activity of extracts from neutral or acidified chlorinated drinking water.

Phytochemical screening and in-vitro evaluation of pharmacological activities of peels of Musa sapientum and Carica papaya fruit.

PubMed

Siddique, Sarmad; Nawaz, Shamsa; Muhammad, Faqir; Akhtar, Bushra; Aslam, Bilal

2018-06-01

Aqueous, absolute and 80% ethanolic extract of fruit peels of Musa sapientum and Carica papaya were investigated for their antibacterial activity, measured by disc diffusion method and antioxidant activity, measured by four different methods. Papaya and banana peels were found to contain terpenoids, tannins, alkaloids, saponins steroid, phenols, fixed oils and fats. 80% ethanolic extract of banana peel was found to contain highest total phenolic content (TPC), total flavonoid content (TFC) and antioxidant activity but in papaya peel, highest TPC and reducing activity was shown by water extract while, TFC and radical scavenging activity was given by 80% ethanolic extract. In banana, water extract showed highest antibacterial activity against tested bacteria while in case of papaya, absolute ethanolic extract showed highest antibacterial activity. The present study revealed that peels of banana and papaya fruits are potentially good source of antioxidant and antibacterial agents.

Determination of pharmaceutical residues in drinking water in Poland using a new SPE-GC-MS(SIM) method based on Speedisk extraction disks and DIMETRIS derivatization.

PubMed

Caban, Magda; Lis, Ewa; Kumirska, Jolanta; Stepnowski, Piotr

2015-12-15

The presence of pharmaceuticals in drinking water, even at very low concentrations, has raised concerns among stakeholders such as drinking-water regulators, governments, water suppliers and the public, with regard to the potential risks to humans. Despite this, the occurrence and the fate of pharmaceuticals in drinking waters of many countries (e.g. in Poland) remains unknown. There is a lack of sufficiently sensitive and reliable analytical methods for such analyses and a need for more in-depth hydrogeological analysis of the possible sources of drug residues in drinking water. In this paper, a multi-residual method for the simultaneous determination of seventeen human pharmaceuticals in drinking waters has been developed. Large-volume extractions using Speedisk extraction disks, and derivatization prior to GC-MS-SIM analysis using a new silylating agent DIMETRIS were applied. The method detection limits (MDLs) ranged from 0.9 to 5.7ng/L and the absolute recoveries of the target compounds were above 80% for most analytes. The developed method was successfully applied in the analysis of the target compounds in drinking water collected in Gdansk (Poland), and of the 17 pharmaceuticals, 6 compounds were detected at least once. During the investigation, the geomorphology of the site region was taken into account, possible sources of pharmaceuticals in the analysed drinking water samples were investigated, and the presence of the drugs in ground and surface waters, raw and treated drinking waters was determined. Concentrations were also compared with those observed in other countries. As a result, this study has not only developed a new analytical method for determining pharmaceuticals in drinking waters as well as rendering missing information for Poland (a country with one of the highest consumptions of pharmaceuticals in Europe), but it also presents a modelled in-depth hydrogeological analysis of the real sources of drugs in drinking waters. Copyright © 2015 Elsevier B.V. All rights reserved.

Improved solvent-free microwave extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim.

PubMed

Wang, Ziming; Ding, Lan; Li, Tiechun; Zhou, Xin; Wang, Lu; Zhang, Hanqi; Liu, Li; Li, Ying; Liu, Zhihong; Wang, Hongju; Zeng, Hong; He, Hui

2006-01-13

Solvent-free microwave extraction (SFME) is a recently developed green technique which is performed in atmospheric conditions without adding any solvent or water. SFME has already been applied to extraction of essential oil from fresh plant materials or dried materials prior moistened. The essential oil is evaporated by the in situ water in the plant materials. In this paper, it was observed that an improved SFME, in which a kind of microwave absorption solid medium, such as carbonyl iron powders (CIP), was added and mixed with the sample, can be applied to extraction of essential oil from the dried plant materials without any pretreatment. Because the microwave absorption capacity of CIP is much better than that of water, the extraction time while using the improved SFME is no more than 30 min using a microwave power of 85 W. Compared to the conventional SFME, the advantages of improved SFME were to speed up the extraction rate and need no pretreatment. Improved SFME has been compared with conventional SFME, microwave-assisted hydrodistillation (MAHD) and conventional hydrodistillation (HD) for the extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim. By using GC-MS system the compositions of essential oil extracted by applying four kinds of extraction methods were identified. There was no obvious difference in the quality of essential oils obtained by the four kinds of extraction methods.

Analysis of Polyphenolic Compounds in Extracts from Leaves of Some Malus domestica Cultivars: Antiradical and Antimicrobial Analysis of These Extracts

PubMed Central

Sowa, Alina; Zgórka, Grażyna; Szykuła, Aleksandra; Franiczek, Roman; Żbikowska, Beata; Gamian, Andrzej

2016-01-01

In this study, methanol, ethyl acetate, water extracts, and precipitate were obtained from leaves of Malus domestica cultivars: Golden delicious, Jonagold, Elstar, Ligol, and Mutsu. Antiradical activity of these extracts was measured using the ABTS+∙ radical, and antimicrobial activity was measured with the disk-diffusion method. Phenolic compounds were measured with the colorimetric method and identified with high performance liquid chromatography (HPLC). The highest antiradical activity was observed for the Jonagold variety, and in particular strong activity was noted for ethyl acetate extracts. Antimicrobial activity was observed against strains of Staphylococcus aureus, Enterococcus faecalis, and the fungus Candida glabrata. Particularly susceptible to the extracts activity appeared to be Staphylococcus aureus, but the growth of Candida glabrata was inhibited in the presence of ethyl acetate extracts. With the HPLC method we identified a high amount of phloridzin (above 500 mg per g of ethyl acetate extracts), lower amounts of hyperoside, isoquercitrin, and quercitrin, and traces of p-hydroxybenzoic and chlorogenic acids. The contribution of phloridzin to antiradical activity of methanol and ethyl acetate extracts was very high (above 90%). In water extract the contribution of phloridzin was between 38.9 and 55.2%, chlorogenic acid 22.7 and 36.1%, and hyperoside 12.2 and 13.3%. PMID:28097143

Analysis of Polyphenolic Compounds in Extracts from Leaves of Some Malus domestica Cultivars: Antiradical and Antimicrobial Analysis of These Extracts.

PubMed

Sowa, Alina; Zgórka, Grażyna; Szykuła, Aleksandra; Franiczek, Roman; Żbikowska, Beata; Gamian, Andrzej; Sroka, Zbigniew

2016-01-01

In this study, methanol, ethyl acetate, water extracts, and precipitate were obtained from leaves of Malus domestica cultivars: Golden delicious, Jonagold, Elstar, Ligol, and Mutsu. Antiradical activity of these extracts was measured using the ABTS +∙ radical, and antimicrobial activity was measured with the disk-diffusion method. Phenolic compounds were measured with the colorimetric method and identified with high performance liquid chromatography (HPLC). The highest antiradical activity was observed for the Jonagold variety, and in particular strong activity was noted for ethyl acetate extracts. Antimicrobial activity was observed against strains of Staphylococcus aureus , Enterococcus faecalis , and the fungus Candida glabrata . Particularly susceptible to the extracts activity appeared to be Staphylococcus aureus , but the growth of Candida glabrata was inhibited in the presence of ethyl acetate extracts. With the HPLC method we identified a high amount of phloridzin (above 500 mg per g of ethyl acetate extracts), lower amounts of hyperoside, isoquercitrin, and quercitrin, and traces of p -hydroxybenzoic and chlorogenic acids. The contribution of phloridzin to antiradical activity of methanol and ethyl acetate extracts was very high (above 90%). In water extract the contribution of phloridzin was between 38.9 and 55.2%, chlorogenic acid 22.7 and 36.1%, and hyperoside 12.2 and 13.3%.

Application of a dispersive solid-phase extraction method using an amino-based silica-coated nanomagnetic sorbent for the trace quantification of chlorophenoxyacetic acids in water samples.

PubMed

Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali; Sobhi, Hamid Reza

2017-09-01

Herein, an amino-based silica-coated nanomagnetic sorbent was applied for the effective extraction of two chlorophenoxyacetic acids (2-methyl-4-chlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic acid) from various water samples. The sorbent was successfully synthesized and subsequently characterized by scanning electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy. The analytes were extracted by the sorbent mainly through ionic interactions. Once the extraction of analytes was completed, they were desorbed from the sorbent and detected by high-performance liquid chromatography with ultraviolet detection. A number of factors affecting the extraction and desorption of the analytes were investigated in detail and the optimum conditions were established. Under the optimum conditions, the calibration curves were linear over the concentration range of 1-250, and based on a signal-to-noise ratio of 3, the method detection limits were determined to be 0.5 μg/L for both analytes. Additionally, a preconcentration factor of 314 was achieved for the analytes. The average relative recoveries obtained from the fortified water samples varied in the range of 91-108% with relative standard deviations of 2.9-8.3%. Finally, the method was determined to be robust and effective for environmental water analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sample Enrichment for Bioanalytical Assessment of Disinfected Drinking Water: Concentrating the Polar, the Volatiles, and the Unknowns.

PubMed

Stalter, Daniel; Peters, Leon I; O'Malley, Elissa; Tang, Janet Yat-Man; Revalor, Marion; Farré, Maria José; Watson, Kalinda; von Gunten, Urs; Escher, Beate I

2016-06-21

Enrichment methods used in sample preparation for the bioanalytical assessment of disinfected drinking water result in the loss of volatile and hydrophilic disinfection byproducts (DBPs) and hence likely tend to underestimate biological effects. We developed and evaluated methods that are compatible with bioassays, for extracting nonvolatile and volatile DBPs from chlorinated and chloraminated drinking water to minimize the loss of analytes. For nonvolatile DBPs, solid-phase extraction (SPE) with TELOS ENV as solid phase performed superior compared to ten other sorbents. SPE yielded >70% recovery of nonpurgeable adsorbable organic halogens (AOX). For volatile DBPs, cryogenic vacuum distillation performed unsatisfactorily. Purge and cold-trap with crushed ice serving as condensation nuclei achieved recoveries of 50-100% for trihalomethanes and haloacetonitriles and approximately 60-90% for purged AOX from tap water. We compared the purgeable versus the nonpurgeable fraction by combining purge-and-trap extraction with SPE. The purgeable DBP fraction enriched with the purge-and-trap method exerted a lower oxidative stress response in mammalian cells than the nonpurgeable DBPs enriched with SPE after purging, while contributions of both fractions to bacterial cytotoxicity was more variable. 37 quantified DBPs explained almost the entire AOX in the purge-and-trap extracts, but <16% in the SPE extracts demonstrating that the nonpurgeable fraction is dominated by unknown DBPs.

Batch experiments versus soil pore water extraction--what makes the difference in isoproturon (bio-)availability?

PubMed

Folberth, Christian; Suhadolc, Metka; Scherb, Hagen; Munch, Jean Charles; Schroll, Reiner

2009-10-01

Two approaches to determine pesticide (bio-)availability in soils (i) batch experiments with "extraction with an excess of water" (EEW) and (ii) the recently introduced "soil pore water (PW) extraction" of pesticide incubated soil samples have been compared with regard to the sorption behavior of the model compound isoproturon in soils. A significant correlation between TOC and adsorbed pesticide amount was found when using the EEW approach. In contrast, there was no correlation between TOC and adsorbed isoproturon when using the in situ PW extraction method. Furthermore, sorption was higher at all concentrations in the EEW method when comparing the distribution coefficients (K(d)) for both methods. Over all, sorption in incubated soil samples at an identical water tension (-15 kPa) and soil density (1.3 g cm(-3)) appears to be controlled by a complex combination of sorption driving soil parameters. Isoproturon bioavailability was found to be governed in different soils by binding strength and availability of sorption sites as well as water content, whereas the dominance of either one of these factors seems to depend on the individual composition and characteristics of the respective soil sample. Using multiple linear regression analysis we obtained furthermore indications that the soil pore structure is affected by the EEW method due to disaggregation, resulting in a higher availability of pesticide sorption sites than in undisturbed soil samples. Therefore, it can be concluded that isoproturon sorption is overestimated when using the EEW method, which should be taken into account when using data from this approach or similar batch techniques for risk assessment analysis.

METHOD 544. DETERMINATION OF MICROCYSTINS AND ...

EPA Pesticide Factsheets

Method 544 is an accurate and precise analytical method to determine six microcystins (including MC-LR) and nodularin in drinking water using solid phase extraction and liquid chromatography tandem mass spectrometry (SPE-LC/MS/MS). The advantage of this SPE-LC/MS/MS is its sensitivity and ability to speciate the microcystins. This method development task establishes sample preservation techniques, sample concentration and analytical procedures, aqueous and extract holding time criteria and quality control procedures. Draft Method 544 undergone a multi-laboratory verification to ensure other laboratories can implement the method and achieve the quality control measures specified in the method. It is anticipated that Method 544 may be used in UCMR 4 to collect nationwide occurrence data for selected microcystins in drinking water. The purpose of this research project is to develop an accurate and precise analytical method to concentrate and determine selected MCs and nodularin in drinking water.

Antimicrobial activity of crude epicarp and seed extracts from mature avocado fruit (Persea americana) of three cultivars.

PubMed

Raymond Chia, Teck Wah; Dykes, Gary A

2010-07-01

The epicarp and seed of Persea Americana Mill. var. Hass (Lauraceae), Persea Americana Mill. var. Shepard, and Persea americana Mill. var Fuerte cultivars of mature avocados (n = 3) were ground separately and extracted with both absolute ethanol and distilled water. Extracts were analyzed for antimicrobial activity using the microtiter broth microdilution assay against four Gram-positive bacteria, six Gram-negative bacteria, and one yeast. Antimicrobial activity against two molds was determined by the hole plate method. The ethanol extracts showed antimicrobial activity (104.2-416.7 microg/mL) toward both Gram-positive and Gram-negative bacteria (except Escherichia coli), while inhibition of the water extracts was only observed for Listeria monocytogenes (93.8-375.0 microg/mL) and Staphylococcus epidermidis (354.2 microg/mL). The minimum concentration required to inhibit Zygosaccharomyces bailii was 500 microg/mL for the ethanol extracts, while no inhibition was observed for the water extracts. No inhibition by either ethanol or water extracts was observed against Penicillium spp. and Aspergillus flavus.

Molecular Dynamics Simulation of Mahkota Dewa (Phaleria Macrocarpa) Extract in Subcritical Water Extraction Process

NASA Astrophysics Data System (ADS)

Hashim, N. A.; Mudalip, S. K. Abdul; Harun, N.; Che Man, R.; Sulaiman, S. Z.; Arshad, Z. I. M.; Shaarani, S. M.

2018-05-01

Mahkota Dewa (Phaleria Macrocarpa), a good source of saponin, flavanoid, polyphenol, alkaloid, and mangiferin has an extensive range of medicinal effects. The intermolecular interactions between solute and solvents such as hydrogen bonding considered as an important factor that affect the extraction of bioactive compounds. In this work, molecular dynamics simulation was performed to elucidate the hydrogen bonding exists between Mahkota Dewa extracts and water during subcritical extraction process. A bioactive compound in the Mahkota Dewa extract, namely mangiferin was selected as a model compound. The simulation was performed at 373 K and 4.0 MPa using COMPASS force field and Ewald summation method available in Material Studio 7.0 simulation package. The radial distribution functions (RDF) between mangiferin and water signify the presence of hydrogen bonding in the extraction process. The simulation of the binary mixture of mangiferin:water shows that strong hydrogen bonding was formed. It is suggested that, the intermolecular interaction between OH2O••HMR4(OH1) has been identified to be responsible for the mangiferin extraction process.

Numerical method based on transfer function for eliminating water vapor noise from terahertz spectra.

PubMed

Huang, Y; Sun, P; Zhang, Z; Jin, C

2017-07-10

Water vapor noise in the air affects the accuracy of optical parameters extracted from terahertz (THz) time-domain spectroscopy. In this paper, a numerical method was proposed to eliminate water vapor noise from the THz spectra. According to the Van Vleck-Weisskopf function and the linear absorption spectrum of water molecules in the HITRAN database, we simulated the water vapor absorption spectrum and real refractive index spectrum with a particular line width. The continuum effect of water vapor molecules was also considered. Theoretical transfer function of a different humidity was constructed through the theoretical calculation of the water vapor absorption coefficient and the real refractive index. The THz signal of the Lacidipine sample containing water vapor background noise in the continuous frequency domain of 0.5-1.8 THz was denoised by use of the method. The results show that the optical parameters extracted from the denoised signal are closer to the optical parameters in the dry nitrogen environment.

Static headspace gas chromatography-mass spectrometry for the one-step derivatisation and extraction of eleven aldehydes in drinking water.

PubMed

Serrano, María; Gallego, Mercedes; Silva, Manuel

2013-09-13

Low-molecular-mass aldehydes (LMMAs) are water disinfection by-products formed by the reaction of ozone and/or chlorine with natural organic matter in water. LMMAs are mutagenic and carcinogenic compounds, which are detected at ng/L levels in water. An analytical method that allows simultaneous derivatisation and extraction of LMMAs in water has been developed using the classical static headspace technique coupled with gas chromatography-mass spectrometry (HS-GC-MS). Important parameters controlling the derivatisation of LMMAs with o-2,3,4,5,6-pentafluorobenzylhydroxylamine, oxime-products extraction and headspace generation were optimised to obtain the highest sensitivity, completing the entire process in 20min. For the first time the derivatisation reaction was carried out at alkaline pH adjusted with sodium hydrogen carbonate which exerts a significant enhancement effect on the derivatisation efficiency of the aldehydes; up to 20-fold with respect to those obtained in weak acid media as recommended by EPA Method 556.1. The addition of 200μL of n-hexane, as a chemical modifier, favoured the volatilisation of oxime-products, increasing the sensitivity of the method. The proposed method allows the achieving of detection limits from 2 to 80ng/L and has excellent precision (RSD average value of 6.4%) and accuracy (recovery ranging from 97% to 99%) for LMMA quantifications in drinking water samples. Finally, the HS-GC-MS method was validated relative to EPA Method 556.1 for the analysis of drinking water samples subjected to several disinfection treatments. Copyright © 2013 Elsevier B.V. All rights reserved.

Evaluation of a method for assaying sulfonamide antimicrobial residues in cheese: hot-water extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Berardi, Giorgio; Bogialli, Sara; Curini, Roberta; Di Corcia, Antonio; Laganá, Aldo

2006-06-28

Several sulfonamide antimicrobials (SAAs) are largely used in veterinary medicine. A rapid, specific, and sensitive procedure for determining 12 SAAs in cheese is presented. The method is based on the matrix solid-phase dispersion technique followed by liquid chromatography (LC)-tandem mass spectrometry (MS) equipped with an electrospray ion source. Target compounds were extracted from Mozzarella, Asiago, Parmigiano, Emmenthal, and Camembert cheese samples by 6 mL of water modified with 10% methanol and heated at 120 degrees C. The addition of methanol to hot water served to improve remarkably extraction yields of the most lipophilic SAAs, that is, sulfadimethoxine and sulfaquinoxaline. After acidification and filtration, 100 microL of the aqueous extract was injected in the LC column. MS data acquisition was performed in the multireaction monitoring mode, selecting two precursor-to-product ion transitions for each target compound. Methanol-modified hot water appeared to be an efficient extractant, because absolute recovery ranged between 67 and 88%. Using sulfamoxole as surrogate analyte, recovery of the 12 analytes spiked in the five types of cheese considered at the 50 ng/g level ranged between 75 and 105% with RSD not higher than 11%. Statistical analysis of the mean recovery data showed that the extraction efficiency was not affected by the type of cheese analyzed. This result indicates this method could be applied to other cheese types not considered here. The accuracy of the method was determined at three spike levels, that is, 20, 50, and 100 ng/g, and varied between 73 and 102% with relative standard deviations ranging between 4 and 12%. On the basis of a signal-to-noise ratio of 10, limits of quantification were estimated to be <1 ng/g.

Electrokinetic electrode system for extraction of soil contaminants from unsaturated soils

DOEpatents

Lindgren, Eric R.; Mattson, Earl D.

1995-01-01

There is presented an electrokinetic electrode assembly for use in extraction of soil contaminants from unsaturated soil in situ. The assembly includes a housing for retaining a liquid comprising an electrolyte solution, pure water, and soil water, the housing being in part of porous material capable of holding a vacuum. An electrode is mounted in the housing. The housing is provided with a vacuum orifice for effecting a vacuum within the housing selectively to control flow of soil water through the housing into the chamber and to control outflow of the liquid from the chamber. The assembly further includes conduit means for removing the liquid from the housing and returning the electrolyte solution to the housing, and a conduit for admitting pure water to the housing. There is further presented an electrode system and method for extraction of soil contaminants, the system and method utilizing at least two electrode assemblies as described above.

Electrokinetic electrode system for extraction of soil contaminants from unsaturated soils

DOEpatents

Lindgren, E.R.; Mattson, E.D.

1995-07-25

An electrokinetic electrode assembly is described for use in extraction of soil contaminants from unsaturated soil in situ. The assembly includes a housing for retaining a liquid comprising an electrolyte solution, pure water, and soil water, the housing being in part of porous material capable of holding a vacuum. An electrode is mounted in the housing. The housing is provided with a vacuum orifice for effecting a vacuum within the housing selectively to control flow of soil water through the housing into the chamber and to control outflow of the liquid from the chamber. The assembly further includes conduit means for removing the liquid from the housing and returning the electrolyte solution to the housing, and a conduit for admitting pure water to the housing. An electrode system and method are also revealed for extraction of soil contaminants. The system and method utilize at least two electrode assemblies as described above. 5 figs.

Methods for Estimating Water Withdrawals for Mining in the United States, 2005

USGS Publications Warehouse

Lovelace, John K.

2009-01-01

The mining water-use category includes groundwater and surface water that is withdrawn and used for nonfuels and fuels mining. Nonfuels mining includes the extraction of ores, stone, sand, and gravel. Fuels mining includes the extraction of coal, petroleum, and natural gas. Water is used for mineral extraction, quarrying, milling, and other operations directly associated with mining activities. For petroleum and natural gas extraction, water often is injected for secondary oil or gas recovery. Estimates of water withdrawals for mining are needed for water planning and management. This report documents methods used to estimate withdrawals of fresh and saline groundwater and surface water for mining during 2005 for each county and county equivalent in the United States, Puerto Rico, and the U.S. Virgin Islands. Fresh and saline groundwater and surface-water withdrawals during 2005 for nonfuels- and coal-mining operations in each county or county equivalent in the United States, Puerto Rico, and the U.S. Virgin Islands were estimated. Fresh and saline groundwater withdrawals for oil and gas operations in counties of six states also were estimated. Water withdrawals for nonfuels and coal mining were estimated by using mine-production data and water-use coefficients. Production data for nonfuels mining included the mine location and weight (in metric tons) of crude ore, rock, or mineral produced at each mine in the United States, Puerto Rico, and the U.S. Virgin Islands during 2004. Production data for coal mining included the weight, in metric tons, of coal produced in each county or county equivalent during 2004. Water-use coefficients for mined commodities were compiled from various sources including published reports and written communications from U.S. Geological Survey National Water-use Information Program (NWUIP) personnel in several states. Water withdrawals for oil and gas extraction were estimated for six States including California, Colorado, Louisiana, New Mexico, Texas, and Wyoming, by using data from State agencies that regulate oil and gas extraction. Total water withdrawals for mining in a county were estimated by summing estimated water withdrawals for nonfuels mining, coal mining, and oil and gas extraction. The results of this study were distributed to NWUIP personnel in each State during 2007. NWUIP personnel were required to submit estimated withdrawals for numerous categories of use in their States to a national compilation team for inclusion in a national report describing water use in the United States during 2005. NWUIP personnel had the option of submitting the estimates determined by using the methods described in this report, a modified version of these estimates, or their own set of estimates or reported data. Estimated withdrawals resulting from the methods described in this report may not be included in the national report; therefore the estimates are not presented herein in order to avoid potential inconsistencies with the national report. Water-use coefficients for specific minerals also are not presented to avoid potential disclosure of confidential production data provided by mining operations to the U.S. Geological Survey.

Characterization of gold kiwifruit pectin from fruit of different maturities and extraction methods.

PubMed

Yuliarti, Oni; Matia-Merino, Lara; Goh, Kelvin K T; Mawson, John; Williams, Martin A K; Brennan, Charles

2015-01-01

Studies on gold kiwifruit pectins are limited. In this work, the characterization of pectin isolated from two different stages of maturity of gold kiwifruit, namely early harvested fruit (EHF) and main harvested fruit (MHF) isolated by three methods (acid, water, enzymatic) was carried out. Pectins isolated from MHF were higher in galacturonic acid content (52-59% w/w) and weight-average molecular weights (Mw, 1.7-3.8 × 10(6)g/mol) compared with EHF pectins (29-49% w/w and 0.2-1.7 × 10(6)g/mol respectively). Enzymatic treatment gave the highest yield but lowest in Mw, viscosity and mechanical spectra for both maturities. The pectin of both maturities was classified as high-methoxyl pectin with the degree of esterification ranged from 82% to 90%. Water-extracted MHF pectin molecules had the highest RMS radius (182.7 nm) and Mw (3.75 × 10(6)g/mol). The water extraction method appeared to retain the native state of pectin molecules compared with acid and enzymatic extraction methods based on the Mw and viscosity data. Copyright © 2014 Elsevier Ltd. All rights reserved.

A comparative study of Averrhoabilimbi extraction method

NASA Astrophysics Data System (ADS)

Zulhaimi, H. I.; Rosli, I. R.; Kasim, K. F.; Akmal, H. Muhammad; Nuradibah, M. A.; Sam, S. T.

2017-09-01

In recent year, bioactive compound in plant has become a limelight in the food and pharmaceutical market, leading to research interest to implement effective technologies for extracting bioactive substance. Therefore, this study is focusing on extraction of Averrhoabilimbi by different extraction technique namely, maceration and ultrasound-assisted extraction. Fewplant partsof Averrhoabilimbiweretaken as extraction samples which are fruits, leaves and twig. Different solvents such as methanol, ethanol and distilled water were utilized in the process. Fruit extractsresult in highest extraction yield compared to other plant parts. Ethanol and distilled water have significant role compared to methanol in all parts and both extraction technique. The result also shows that ultrasound-assisted extraction gave comparable result with maceration. Besides, the shorter period on extraction process gives useful in term of implementation to industries.

Analysis of the herbicide diuron, three diuron degradates, and six neonicotinoid insecticides in water-Method details and application to two Georgia streams

USGS Publications Warehouse

Hladik, Michelle; Calhoun, Daniel L.

2012-01-01

A method for the determination of the widely used herbicide diuron, three degradates of diuron, and six neonicotinoid insecticides in environmental water samples is described. Filtered water samples were extracted by using solid-phase extraction (SPE) with no additional cleanup steps. Quantification of the pesticides from the extracted water samples was done by using liquid chromatography with tandem mass spectrometry (LC/MS/MS). Recoveries in test water samples fortified at 20 nanograms per liter (ng/L) for each compound ranged from 75 to 97 percent; relative standard deviations ranged from 5 to 10 percent. Method detection limits (MDLs) in water ranged from 3.0 to 6.2 ng/L using LC/MS/MS. The method was applied to water samples from two streams in Georgia, Sope Creek and the Chattahoochee River. Diuron and 3,4-dichloroaniline (3,4-DCA) were detected in 100 and 80 percent, respectively, of the samples from the Chattahoochee River, whereas Sope creek had detection frequencies of 15 percent for diuron and 31 percent for 3,4-DCA. Detection frequencies for the neonicotinoid insecticide, imidacloprid, were 60 percent for the Chattahoochee River and 85 percent for Sope Creek. Field matrix-spike recoveries for each compound, when averaged over four water samples, ranged from 79 to 100 percent. The average percentage difference between replicate pairs for all compounds detected in the field samples was 10.1 (± 4.5) percent.

A novel method for rapid determination of total solid content in viscous liquids by multiple headspace extraction gas chromatography.

PubMed

Xin, Li-Ping; Chai, Xin-Sheng; Hu, Hui-Chao; Barnes, Donald G

2014-09-05

This work demonstrates a novel method for rapid determination of total solid content in viscous liquid (polymer-enriched) samples. The method is based multiple headspace extraction gas chromatography (MHE-GC) on a headspace vial at a temperature above boiling point of water. Thus, the trend of water loss from the tested liquid due to evaporation can be followed. With the limited MHE-GC testing (e.g., 5 extractions) and a one-point calibration procedure (i.e., recording the weight difference before and after analysis), the total amount of water in the sample can be determined, from which the total solid contents in the liquid can be calculated. A number of black liquors were analyzed by the new method which yielded results that closely matched those of the reference method; i.e., the results of these two methods differed by no more than 2.3%. Compared with the reference method, the MHE-GC method is much simpler and more practical. Therefore, it is suitable for the rapid determination of the solid content in many polymer-containing liquid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Analysis of polycyclic aromatic hydrocarbons in sediment reference materials by microwave-assisted extraction.

PubMed

Shu, Y Y; Lao, R C; Chiu, C H; Turle, R

2000-12-01

The microwave-assisted extraction (MAE) of polycyclic aromatic hydrocarbons (PAHs) from harbor sediment reference material EC-1, marine sediment reference material HS-2 and PAH-spiked river bed soil was conducted. The extraction conditions for EC-1 were carried out at 70 degrees C and 100 degrees C under pressure in closed vessels with cyclohexane acetone (1:1), cyclohexane-water (3:1), hexane acetone (1:1), and hexane-water (3:1) for 10 min. A comparison between MAE and a 16-h Soxhlet extraction (SX) method showed that both techniques gave comparable results with certified values. MAE has advantages over the currently used Soxhlet technique due to a faster extraction time and lower quantity of solvent used. The consumption of organic solvent of the microwave method was less than one-tenth compared to Soxhlet.

Optimisation of extraction and sludge dewatering efficiencies of bio-flocculants extracted from Abelmoschus esculentus (okra).

PubMed

Lee, Chai Siah; Chong, Mei Fong; Robinson, John; Binner, Eleanor

2015-07-01

The production of natural biopolymers as flocculants for water treatment is highly desirable due to their inherent low toxicity and low environmental footprint. In this study, bio-flocculants were extracted from Hibiscus/Abelmoschus esculentus (okra) by using a water extraction method, and the extract yield and its performance in sludge dewatering were evaluated. Single factor experimental design was employed to obtain the optimum conditions for extraction temperature (25-90 °C), time (0.25-5 h), solvent loading (0.5-5 w/w) and agitation speed (0-225 rpm). Results showed that extraction yield was affected non-linearly by all experimental variables, whilst the sludge dewatering ability was only influenced by the temperature of the extraction process. The optimum extraction conditions were obtained at 70 °C, 2 h, solvent loading of 2.5 w/w and agitation at 200 rpm. Under the optimal conditions, the extract yield was 2.38%, which is comparable to the extraction of other polysaccharides (0.69-3.66%). The bio-flocculants displayed >98% removal of suspended solids and 68% water recovery during sludge dewatering, and were shown to be comparable with commercial polyacrylamide flocculants. This work shows that bio-flocculants could offer a feasible alternative to synthetic flocculants for water treatment and sludge dewatering applications, and can be extracted using only water as a solvent, minimising the environmental footprint of the extraction process. Copyright © 2015 Elsevier Ltd. All rights reserved.

Improved detection of multiple environmental antibiotics through an optimized sample extraction strategy in liquid chromatography-mass spectrometry analysis.

PubMed

Yi, Xinzhu; Bayen, Stéphane; Kelly, Barry C; Li, Xu; Zhou, Zhi

2015-12-01

A solid-phase extraction/liquid chromatography/electrospray ionization/multi-stage mass spectrometry (SPE-LC-ESI-MS/MS) method was optimized in this study for sensitive and simultaneous detection of multiple antibiotics in urban surface waters and soils. Among the seven classes of tested antibiotics, extraction efficiencies of macrolides, lincosamide, chloramphenicol, and polyether antibiotics were significantly improved under optimized sample extraction pH. Instead of only using acidic extraction in many existing studies, the results indicated that antibiotics with low pK a values (<7) were extracted more efficiently under acidic conditions and antibiotics with high pK a values (>7) were extracted more efficiently under neutral conditions. The effects of pH were more obvious on polar compounds than those on non-polar compounds. Optimization of extraction pH resulted in significantly improved sample recovery and better detection limits. Compared with reported values in the literature, the average reduction of minimal detection limits obtained in this study was 87.6% in surface waters (0.06-2.28 ng/L) and 67.1% in soils (0.01-18.16 ng/g dry wt). This method was subsequently applied to detect antibiotics in environmental samples in a heavily populated urban city, and macrolides, sulfonamides, and lincomycin were frequently detected. Antibiotics with highest detected concentrations were sulfamethazine (82.5 ng/L) in surface waters and erythromycin (6.6 ng/g dry wt) in soils. The optimized sample extraction strategy can be used to improve the detection of a variety of antibiotics in environmental surface waters and soils.

Multiresidue analysis of 24 Water Framework Directive priority substances by on-line solid phase extraction-liquid chromatography tandem mass spectrometry in environmental waters.

PubMed

Rubirola, Adrià; Boleda, Mª Rosa; Galceran, Mª Teresa

2017-04-14

This paper reports the development of a fully multiresidue and automated on-line solid phase extraction (SPE) - liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of 24 priority substances (PS) belonging to different classes (pesticides, hormones or pharmaceuticals) included in the Directive 2013/39/UE and the recent Watch List (Decision 2015/495) in water samples (drinking water, surface water, and effluent wastewaters). LC-MS/MS conditions and on-line SPE parameters such as sorbent type, sample and wash volumes were optimized. The developed method is highly sensitive (limits of detection between 0.1 and 1.4ngL -1 ) and precise (relative standard deviations lower than 8%). As part of the method validation studies, linearity, accuracy and matrix effects were assessed. The main advantage of this method over traditional off-line procedures is the minimization of tedious sample preparation increasing productivity and sample throughput. The optimized method was applied to the analysis of water samples and the results revealed the presence of 16 PS in river water and effluent water of wastewater treatment plants. Copyright © 2017 Elsevier B.V. All rights reserved.

Influence of extraction solvent on antioxidant capacity value of oleaster measured by ORAC method.

PubMed

Yalcin, Gorkem; Sogut, Ozlem

2014-01-01

Oxygen radical absorbance capacity (ORAC) is a widely used hydrogen atom transfer-based method which measures the antioxidant capacity of natural products. ORAC values of oleaster (Elaeagnus angustifolia L.), which was extracted with ethanol/acetone (7:3, v/v), ethanol/water (1:1, v/v) and methanol/water (1:1, v/v) in order to evaluate the effects of solvent type on antioxidant capacity, were examined. In general, results revealed that ethanol/water extracts exhibited better antioxidant capacity values. Furthermore, results obtained by using ORAC-eosin y (ORAC-EY), one of the widely used derivative of fluorescein (FL), as a fluorescent probe were compared with those obtained by using ORAC-FL. According to the results, ORAC-EY values were found to be compatible with ORAC-FL values.

Evaluation of DNA extraction methods for the analysis of microbial community in biological activated carbon.

PubMed

Zheng, Lu; Gao, Naiyun; Deng, Yang

2012-01-01

It is difficult to isolate DNA from biological activated carbon (BAC) samples used in water treatment plants, owing to the scarcity of microorganisms in BAC samples. The aim of this study was to identify DNA extraction methods suitable for a long-term, comprehensive ecological analysis of BAC microbial communities. To identify a procedure that can produce high molecular weight DNA, maximizes detectable diversity and is relatively free from contaminants, the microwave extraction method, the cetyltrimethylammonium bromide (CTAB) extraction method, a commercial DNA extraction kit, and the ultrasonic extraction method were used for the extraction of DNA from BAC samples. Spectrophotometry, agarose gel electrophoresis and polymerase chain reaction (PCR)-restriction fragment length polymorphisms (RFLP) analysis were conducted to compare the yield and quality of DNA obtained using these methods. The results showed that the CTAB method produce the highest yield and genetic diversity of DNA from BAC samples, but DNA purity was slightly less than that obtained with the DNA extraction-kit method. This study provides a theoretical basis for establishing and selecting DNA extraction methods for BAC samples.

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

EPA Science Inventory

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

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

EPA Science Inventory

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

Method Development for the Analysis of 1,4-Dioxane in Drinking Water Using Solid Phase Extraction and Gas Chromatography/Mass Spectrometry

EPA Science Inventory

1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of...

Method and apparatus for extracting water from air

DOEpatents

Spletzer, Barry L.; Callow, Diane Schafer; Marron, Lisa C.; Salton, Jonathan R.

2002-01-01

The present invention provides a method and apparatus for extracting liquid water from moist air using minimal energy input. The method comprises compressing moist air under conditions that foster the condensation of liquid water. The air can be decompressed under conditions that do not foster the vaporization of the condensate. The decompressed, dried air can be exchanged for a fresh charge of moist air and the process repeated. The liquid condensate can be removed for use. The apparatus can comprise a compression chamber having a variable internal volume. An intake port allows moist air into the compression chamber. An exhaust port allows dried air out of the compression chamber. A condensation device fosters condensation at the desired conditions. A condensate removal port allows liquid water to be removed.

Determination of Ultra-trace Rhodium in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction Using 2-(5-Iodo-2-Pyridylazo)-5-Dimethylaminoaniline as a Chelating Agent.

PubMed

Han, Quan; Huo, Yanyan; Wu, Jiangyan; He, Yaping; Yang, Xiaohui; Yang, Longhu

2017-03-24

A highly sensitive method based on cloud point extraction (CPE) separation/preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection has been developed for the determination of ultra-trace amounts of rhodium in water samples. A new reagent, 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA), was used as the chelating agent and the nonionic surfactant TritonX-114 was chosen as extractant. In a HAc-NaAc buffer solution at pH 5.5, Rh(III) reacts with 5-I-PADMA to form a stable chelate by heating in a boiling water bath for 10 min. Subsequently, the chelate is extracted into the surfactant phase and separated from bulk water. The factors affecting CPE were investigated. Under the optimized conditions, the calibration graph was linear in the range of 0.1-6.0 ng/mL, the detection limit was 0.023 ng/mL for rhodium and relative standard deviation was 3.67% ( c = 1.0 ng/mL, n = 11)．The method has been applied to the determination of trace rhodium in water samples with satisfactory results.

Apparatus and method for extraction of chemicals from aquifer remediation effluent water

DOEpatents

McMurtrey, Ryan D.; Ginosar, Daniel M.; Moor, Kenneth S.; Shook, G. Michael; Moses, John M.; Barker, Donna L.

2002-01-01

An apparatus and method for extraction of chemicals from an aquifer remediation aqueous effluent are provided. The extraction method utilizes a critical fluid for separation and recovery of chemicals employed in remediating aquifers contaminated with hazardous organic substances, and is particularly suited for separation and recovery of organic contaminants and process chemicals used in surfactant-based remediation technologies. The extraction method separates and recovers high-value chemicals from the remediation effluent and minimizes the volume of generated hazardous waste. The recovered chemicals can be recycled to the remediation process or stored for later use.

Method and system for extraction of chemicals from aquifer remediation effluent water

DOEpatents

McMurtrey, Ryan D.; Ginosar, Daniel M.; Moor, Kenneth S.; Shook, G. Michael; Barker, Donna L.

2003-01-01

A method and system for extraction of chemicals from an groundwater remediation aqueous effluent are provided. The extraction method utilizes a critical fluid for separation and recovery of chemicals employed in remediating groundwater contaminated with hazardous organic substances, and is particularly suited for separation and recovery of organic contaminants and process chemicals used in surfactant-based remediation technologies. The extraction method separates and recovers high-value chemicals from the remediation effluent and minimizes the volume of generated hazardous waste. The recovered chemicals can be recycled to the remediation process or stored for later use.

Simultaneous analysis of multiple classes of antimicrobials in environmental water samples using SPE coupled with UHPLC-ESI-MS/MS and isotope dilution.

PubMed

Tran, Ngoc Han; Chen, Hongjie; Do, Thanh Van; Reinhard, Martin; Ngo, Huu Hao; He, Yiliang; Gin, Karina Yew-Hoong

2016-10-01

A robust and sensitive analytical method was developed for the simultaneous analysis of 21 target antimicrobials in different environmental water samples. Both single SPE and tandem SPE cartridge systems were investigated to simultaneously extract multiple classes of antimicrobials. Experimental results showed that good extraction efficiencies (84.5-105.6%) were observed for the vast majority of the target analytes when extraction was performed using the tandem SPE cartridge (SB+HR-X) system under an extraction pH of 3.0. HPLC-MS/MS parameters were optimized for simultaneous analysis of all the target analytes in a single injection. Quantification of target antimicrobials in water samples was accomplished using 15 isotopically labeled internal standards (ILISs), which allowed the efficient compensation of the losses of target analytes during sample preparation and correction of matrix effects during UHPLC-MS/MS as well as instrument fluctuations in MS/MS signal intensity. Method quantification limit (MQL) for most target analytes based on SPE was below 5ng/L for surface waters, 10ng/L for treated wastewater effluents, and 15ng/L for raw wastewater. The method was successfully applied to detect and quantify the occurrence of the target analytes in raw influent, treated effluent and surface water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

PubMed

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2018-01-01

The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

Method of extracting iodine from liquid mixtures of iodine, water and hydrogen iodide

DOEpatents

Mysels, Karol J.

1979-01-01

The components of a liquid mixture consisting essentially of HI, water and at least about 50 w/o iodine are separated in a countercurrent extraction zone by treating with phosphoric acid containing at least about 90 w/o H.sub.3 PO.sub.4. The bottom stream from the extraction zone is substantially completely molten iodine, and the overhead stream contains water, HI, H.sub.3 PO.sub.4 and a small fraction of the amount of original iodine. When the water and HI are present in near-azeotropic proportions, there is particular advantage in feeding the overhead stream to an extractive distillation zone wherein it is treated with additional concentrated phosphoric acid to create an anhydrous HI vapor stream and bottoms which contain at least about 85 w/o H.sub.3 PO.sub.4. Concentration of these bottoms provides phosphoric acid infeed for both the countercurrent extraction zone and for the extractive distillation zone.

Single-step microwave-assisted hot water extraction of hemicelluloses from selected lignocellulosic materials - A biorefinery approach.

PubMed

Mihiretu, Gezahegn T; Brodin, Malin; Chimphango, Annie F; Øyaas, Karin; Hoff, Bård H; Görgens, Johann F

2017-10-01

The viability of single-step microwave-induced pressurized hot water conditions for co-production of xylan-based biopolymers and bioethanol from aspenwood sawdust and sugarcane trash was investigated. Extraction of hemicelluloses was conducted using microwave-assisted pressurized hot water system. The effects of temperature and time on extraction yield and enzymatic digestibility of resulting solids were determined. Temperatures between 170-200°C for aspenwood and 165-195°C for sugarcane trash; retention times between 8-22min for both feedstocks, were selected for optimization purpose. Maximum xylan extraction yields of 66 and 50%, and highest cellulose digestibilities of 78 and 74%, were attained for aspenwood and sugarcane trash respectively. Monomeric xylose yields for both feedstocks were below 7%, showing that the xylan extracts were predominantly in non-monomeric form. Thus, single-step microwave-assisted hot water method is viable biorefinery approach to extract xylan from lignocelluloses while rendering the solid residues sufficiently digestible for ethanol production. Copyright © 2017 Elsevier Ltd. All rights reserved.

[The isolation of organic compounds from hydrosulfuric mineral waters with the use of the extractive freezing-out technique with centrifugation].

PubMed

Bekhterev, V N; Kabina, E A

The mineral waters, enriched with organic substances find extensive application in balneotherapy. The fast and efficient methods for the identification and quantitative measurement of organic compounds (in the first place, organic acids) in such waters need to be developed for the estimation of their quality and biological activity. The objective of the present study was to elaborate a gas chromatographic method for the determination of monobasic carbonic acids in sulfide-containing mineral waters by means of extractive freezing-out in combination with the application of the centrifugal forces for the elucidation of the metrological characteristics of the compounds of interest. The secondary objective was to estimate the prospects for the application of the method of interest for determining the dissolved organic compounds in mineral waters. The following carbonic acids were used for the purposes of the study: acetic acid (analytical grade), Russia; propionic grade (extra pure), Ferak, Germany; butyric acid (pure), Russia; valeric acid (pure), Russia; caproic acid (pure), Russia; oenanthic acid (pure), Russia; and caprylic acid (pure), Russia). Acetonitrile («O» grade), Russia, was used as the extracting agent. The LV-210 analytical balance (Russia) was used to prepare the model and standard solutions of the organic compounds and to determine their mass. The extracts and standard mixture were investigated by the gas chromatographic technique with the use of the Kristallyuks apparatus («Meta-Khrom», Russia) equipped with the flame ionization detector and the capillary column. Extractive freezing-out in the combination with centrifugation was performed with the laboratory installation for this purpose. Under the model conditions, a single extractive freezing-out procedure with the centrifugation of the sample made it possible to reach the 22-37-fold concentration of C2-C8 monobasic carbonic acids during their transfer from water into acetonitrile. The metrological parameters of the proposed procedure for gas-chromatographic determination of the aforementioned acids in hydrosulfuric mineral waters were estimated. The limit of detection of acetic and propionic acids has been 0,2 mg/l, that for butyric acid 0,1 mg/l, for valeric, caproic, oenanthic and caprylic acids 0,05 mg/l. We failed to identify C2-C8 carbonic acids in hydrosulfuric water from the 6T well of the field Matsesta fields. The investigation of the extracts obtained by the proposed extraction procedure with the use of the newly developed variant of high performance liquid chromatography (HPLC) with diode-matrix detection revealed the presence of various amounts of unknown organic substances. The UV-spectrum of one of those components was obtained which made it possible to conjecture its molecular structure. The procedure for the sample preparation and the following determination of organic acids in water is simple, carried out in a single stage, and does not impose special requirements to the qualification of the researcher. It allows to describe the newly developed technique as a rapid test method. Along with it, realization of extraction in the negative temperature mode reduces the risk of decomposition of the thermally unstable chemical compounds being extracted and reduces volatility of the organic solvents being used. The technology of the method does not demand a special laboratory glassware and expendables.

Radical scavenging activities of Rio Red grapefruits and Sour orange fruit extracts in different in vitro model systems.

PubMed

Jayaprakasha, G K; Girennavar, Basavaraj; Patil, Bhimanagouda S

2008-07-01

Antioxidant fractions from two different citrus species such as Rio Red (Citrus paradise Macf.) and Sour orange (Citrus aurantium L.) were extracted with five different polar solvents using Soxhlet type extractor. The total phenolic content of the extracts was determined by Folin-Ciocalteu method. Ethyl acetate extract of Rio Red and Sour orange was found to contain maximum phenolics. The dried fractions were screened for their antioxidant activity potential using in vitro model systems such as 1,1-diphenyl-2-picryl hydrazyl (DPPH), phosphomolybdenum method and nitroblue tetrazolium (NBT) reduction at different concentrations. The methanol:water (80:20) fraction of Rio Red showed the highest radical scavenging activity 42.5%, 77.8% and 92.1% at 250, 500 and 1000 ppm, respectively, while methanol:water (80:20) fraction of Sour orange showed the lowest radical scavenging activity at all the tested concentrations. All citrus fractions showed good antioxidant capacity by the formation of phosphomolybdenum complex at 200 ppm. In addition, superoxide radical scavenging activity was assayed using non-enzymatic (NADH/phenaxine methosulfate) superoxide generating system. All the extracts showed variable superoxide radical scavenging activity. Moreover, methanol:water (80:20) extract of Rio Red and methanol extract of Sour orange exhibited marked reducing power in potassium ferricyanide reduction method. The data obtained using above in vitro models clearly establish the antioxidant potential of citrus fruit extracts. However, comprehensive studies need to be conducted to ascertain the in vivo bioavailability, safety and efficacy of such extracts in experimental animals. To the best of our knowledge, this is the first report on antioxidant activity of different polar extracts from Rio Red and Sour oranges.

Two-step microextraction combined with high performance liquid chromatographic analysis of pyrethroids in water and vegetable samples.

PubMed

Mukdasai, Siriboon; Thomas, Chunpen; Srijaranai, Supalax

2014-03-01

Dispersive liquid microextraction (DLME) combined with dispersive µ-solid phase extraction (D-µ-SPE) has been developed as a new approach for the extraction of four pyrethroids (tetramethrin, fenpropathrin, deltamethrin and permethrin) prior to the analysis by high performance liquid chromatography (HPLC) with UV detection. 1-Octanol was used as the extraction solvent in DLME. Magnetic nanoparticles (Fe3O4) functionalized with 3-aminopropyl triethoxysilane (APTS) were used as the dispersive in DLME and as the adsorbent in D-µ-SPE. The extracted pyrethroids were separated within 30 min using isocratic elution with acetonitrile:water (72:28). The factors affecting the extraction efficiency were investigated. Under the optimum conditions, the enrichment factors were in the range of 51-108. Linearity was obtained in the range 0.5-400 ng mL(-1) (tetramethrin) and 5-400 ng mL(-1) (fenpropathrin, deltamethrin and permethrin) with the correlation coefficients (R(2)) greater than 0.995. Detection limits were 0.05-2 ng mL(-1) (water samples) and 0.02-2.0 ng g(-1) (vegetable samples). The relative standard deviations of peak area varied from 1.8 to 2.5% (n=10). The extraction recoveries of the four pyrethroids in field water and vegetable samples were 91.7-104.5%. The proposed method has high potential for use as a sensitive method for determination of pyrethroid residues in water and vegetable samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Multi-residue determination of 47 organic compounds in water, soil, sediment and fish-Turia River as case study.

PubMed

Carmona, Eric; Andreu, Vicente; Picó, Yolanda

2017-11-30

A sensitive and reliable method based on solid-liquid extraction (SLE) using McIlvaine-Na 2 EDTA buffer (pH=4.5)-methanol and solid-phase extraction (SPE) clean up prior to ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was applied to determine 47 organic contaminants in fish, soil and sediments. The SPE procedure to clean-up the extracts was also used as extraction method to determine these compounds in water. Recoveries ranged from 38 to 104% for all matrices with RSDs<30%. Limits of Quantification for the target compounds were in the range of 10-50ng/g for soil, 2-40ng/g for sediment, 5-30ng/g for fish and 0.3-26ng/L for water. Furthermore, the proposed method was compared to QuEChERS (widely used for environmental matrices) that involves extraction with buffered acetonitrile (pH 5.5) and dispersive SPE clean-up. The results obtained (recoveries>50% for 36 compounds in front of 9, matrix effect<20% for 31 compounds against 21, and LOQs <25ngg -1 for 38 compounds against 22) indicates that the proposed method is more efficient than QuEChERS, The method was applied to monitoring these compounds along the Turia River. In river waters, Paracetamol (175ngL -1 ), ibuprofen (153ngL -1 ) and bisphenol A (41ngL -1 ) were the compounds most frequently detected while in sediments were vildagliptin (7ngg -1 ) and metoprolol (31ngg -1 ) and in fish, bisphenol A (33ngg -1 ) or sulfamethoxazole (13ngg -1 ). Copyright © 2017 Elsevier B.V. All rights reserved.

An analytical method for 14C in environmental water based on a wet-oxidation process.

PubMed

Huang, Yan-Jun; Guo, Gui-Yin; Wu, Lian-Sheng; Zhang, Bing; Chen, Chao-Feng; Zhang, Hai-Ying; Qin, Hong-Juan; Shang-Guan, Zhi-Hong

2015-04-01

An analytical method for (14)C in environmental water based on a wet-oxidation process was developed. The method can be used to determine the activity concentrations of organic and inorganic (14)C in environmental water, or total (14)C, including in drinking water, surface water, rainwater and seawater. The wet-oxidation of the organic component allows the conversion of organic carbon to an inorganic form, and the extraction of the inorganic (14)C can be achieved by acidification and nitrogen purging. Environmental water with a volume of 20 L can be used for the wet-oxidation and extraction, and a detection limit of about 0.02 Bq/g(C) can be achieved for water with carbon content above 15 mg(C)/L, obviously lower than the natural level of (14)C in the environment. The collected carbon is sufficient for measurement with a low level liquid scintillation counter (LSC) for typical samples. Extraction or recovery experiments for inorganic carbon and organic carbon from typical materials, including analytical reagents of organic benzoquinone, sucrose, glutamic acid, nicotinic acid, humic acid, ethane diol, et cetera., were conducted with excellent results based on measurement on a total organic carbon analyzer and LSC. The recovery rate for inorganic carbon ranged tween 98.7%-99.0% with a mean of 98.9(± 0.1)%, for organic carbon recovery ranged between 93.8% and 100.0% with a mean of 97.1(± 2.6)%. Verification and an uncertainty budget of the method are also presented for a representative environmental water. The method is appropriate for (14)C analysis in environmental water, and can be applied also to the analysis of liquid effluent from nuclear facilities. Copyright © 2015 Elsevier Ltd. All rights reserved.

Antimicrobial Activities of Silver Nanoparticles Synthesized by Using Water Extract of Arnicae anthodium.

PubMed

Dobrucka, Renata; Długaszewska, Jolanta

2015-06-01

Green synthesis of nanoparticles has gained significant importance in recent years and has become the one of the most preferred methods. Also, green synthesis of nanoparticles is valuable branch of nanotechnology. Plant extracts are eco-friendly and can be an economic option for synthesis of nanoparticles. This study presents method the synthesis of silver nanoparticles using water extract of Arnicae anthodium. Formation of silver nanoparticles was confirmed by UV-visble spectroscopy, Fourier transform infrared spectroscopy and total reflection X-ray fluorescence analysis. The morphology of the synthesized silver nanoparticles was verified by SEM-EDS. The obtained silver nanoparticles were used to study their antimicrobial activity.

The effect of filler addition and oven temperature to the antioxidant quality in the drying of Physalis angulata fruit extract obtained by subcritical water extraction

NASA Astrophysics Data System (ADS)

Susanti, R. F.; Christianto, G.

2016-01-01

Physalis angulata or ceplukan is medicinal herb, which grows naturally in Indonesia. It has been used in traditional medicine to treat several diseases. It is also reported to have antimycobacterial, antileukemic, antipyretic. In this research, Pysalis angulata fruit was investigated for its antioxidant capacity. In order to avoid the toxic organic solvent commonly used in conventional extraction, subcritical water extraction method was used. During drying, filler which is inert was added to the extract. It can absorb water and change the oily and sticky form of extract to powder form. The effects of filler types, concentrations and drying temperatures were investigated to the antioxidant quality covering total phenol, flavonoid and antioxidant activity. The results showed that total phenol, flavonoid and antioxidant activity were improved by addition of filler because the drying time was shorter compared to extract without filler. Filler absorbs water and protects extract from exposure to heat during drying. The combination between high temperature and shorter drying time are beneficial to protect the antioxidant in extract. The type of fillers investigation showed that aerosil gave better performance compared to Microcrystalline Celullose (MCC).

Improved tandem mass spectrometry (MS/MS) derivatized method for the detection of tyrosinemia type I, amino acids and acylcarnitine disorders using a single extraction process.

PubMed

Dhillon, Kuldeep S; Bhandal, Ajit S; Aznar, Constantino P; Lorey, Fred W; Neogi, Partha

2011-05-12

Succinylacetone (SUAC), a specific marker for tyrosinemia type I (Tyr I) cannot be detected by the routine LC-MS/MS screening of amino acids (AA) and acylcarnitines (AC) in newborns. The current derivatized methods require double extraction of newborn dried blood spots (DBS); one for AA and AC and the second for SUAC from the blood spot left after the first extraction. We have developed a method in which AA, AC and SUAC are extracted in a single extraction resulting in significant reduction in labor and assay time. The 3.2 mm DBS were extracted by incubating at 45 °C for 45 min with 100 μl of acetonitrile (ACN)-water-formic acid mixture containing hydrazine and stable-isotope labeled internal standards of AA, AC and SUAC. The extract was derivatized with n-butanolic-HCl and analyzed by LC-MS/MS. The average inter-assay CVs for, AA, AC and SUAC were 10.1, 10.8 and 7.1% respectively. The extraction of analytes with ACN-water mixture showed no significant difference in their recovery compared to commonly used solvent MeOH. The concentration of hydrazine had considerable impact on SUAC extraction. We developed a new MS/MS derivatized method to detect AA/AC/SUAC in a single extraction process for screening Tyr I along with disorders of AA and AC. Published by Elsevier B.V.

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

PubMed

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

2016-01-01

A rapid and efficient sample pretreatment using solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was studied for the extraction of 58 pharmaceuticals and personal care products (PPCPs) and pesticides from water samples. Type and volume of extraction and disperser solvents, pH, salt addition, amount of salt and type of demulsification solvent were evaluated. Limits of quantification (LOQ) in the range from 0.0125 to 1.25 µg L(-1) were reached, and linearity was in the range from the LOQ of each compound to 25 μg L(-1). Recoveries ranged from 60% to 120% for 84% of the compounds, with relative standard deviations lower than 29%. The proposed method demonstrated, for the first time, that sample preparation by SD-DLLME with determination by LC-MS/MS can be successfully used for the simultaneous extraction of 32 pesticides and 26 PPCPs from water samples. The entire procedure, including the extraction of 58 organic compounds from the aqueous sample solution and the breaking up of the emulsion after extraction with water, rather than with an organic solvent, was environmentally friendly. In addition, this technique was less expensive and faster than traditional techniques. Finally, the analytical method under study was successfully applied to the analysis of all 58 pesticides and PPCPs in surface water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive.

PubMed

Gandolfi, F; Malleret, L; Sergent, M; Doumenq, P

2015-08-07

The water framework directives (WFD 2000/60/EC and 2013/39/EU) force European countries to monitor the quality of their aquatic environment. Among the priority hazardous substances targeted by the WFD, short chain chlorinated paraffins C10-C13 (SCCPs), still represent an analytical challenge, because few laboratories are nowadays able to analyze them. Moreover, an annual average quality standards as low as 0.4μgL(-1) was set for SCCPs in surface water. Therefore, to test for compliance, the implementation of sensitive and reliable analysis method of SCCPs in water are required. The aim of this work was to address this issue by evaluating automated solid phase micro-extraction (SPME) combined on line with gas chromatography-electron capture negative ionization mass spectrometry (GC/ECNI-MS). Fiber polymer, extraction mode, ionic strength, extraction temperature and time were the most significant thermodynamic and kinetic parameters studied. To determine the suitable factors working ranges, the study of the extraction conditions was first carried out by using a classical one factor-at-a-time approach. Then a mixed level factorial 3×2(3) design was performed, in order to give rise to the most influent parameters and to estimate potential interactions effects between them. The most influent factors, i.e. extraction temperature and duration, were optimized by using a second experimental design, in order to maximize the chromatographic response. At the close of the study, a method involving headspace SPME (HS-SPME) coupled to GC/ECNI-MS is proposed. The optimum extraction conditions were sample temperature 90°C, extraction time 80min, with the PDMS 100μm fiber and desorption at 250°C during 2min. Linear response from 0.2ngmL(-1) to 10ngmL(-1) with r(2)=0.99 and limits of detection and quantification, respectively of 4pgmL(-1) and 120pgmL(-1) in MilliQ water, were achieved. The method proved to be applicable in different types of waters and show key advantages, such as simplicity, automation and sensitivity, required for the monitoring programs linked to the WFD. Copyright © 2015 Elsevier B.V. All rights reserved.

Microextraction of non-steroidal anti-inflammatory drugs from waste water samples by rotating-disk sorptive extraction.

PubMed

Manzo, Valentina; Honda, Luis; Navarro, Orielle; Ascar, Loreto; Richter, Pablo

2014-10-01

In this study, six non-steroidal anti-inflammatory drugs (NSAIDs) were extracted from water samples using the rotating-disk sorptive extraction (RDSE) technique. The extraction disk device contains a central cavity that allows for the incorporation of a powdered sorbent phase (Oasis™ HLB). The analytes were extracted from water and pre-concentrated on the sorbent to reach the extraction equilibrium, and then they were desorbed with solvent, derivatized and determined by gas chromatography-mass spectrometry (GC-MS). The variables for the extraction were studied using high performance liquid chromatography with a diode array detector (HPLC-DAD) to avoid the derivatization step, and the optimum values were as follows: 60 mg of Oasis™ HLB, a rotation velocity of 3,000 rpm, a pH of 2, a sample volume of 50 mL, and an extraction time of approximately 90-100 min. The recoveries ranged from 71 to 104%, with relative standard deviations (RSD) between 2 and 8%. The detection limits ranged from 0.001 to 0.033 µg L(-1). The described method was applied to the analysis of influents and effluents from wastewater treatment plants (WWTP) in Santiago, Chile. The concentrations of the detected drugs ranged from 1.5 to 13.4 µg L(-1) and from 1.0 to 3.2 µg L(-1) in the influents and effluents, respectively. The samples were extracted by solid phase extraction (SPE). No significant differences were observed in the determined concentrations for most of the NSAIDs, indicating that RDSE is an alternative method for the preparation of water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

METHOD 530 DETERMINATION OF SELECT SEMIVOLATILE ORGANIC CHEMICALS IN DRINKING WATER BY SOLID PHASE EXTRACTION AND GAS CHROMATOGRAPHY/ MASS SPECTROMETRY (GC/MS)

EPA Science Inventory

1.1. This is a gas chromatography/mass spectrometry (GC/MS) method for the determination of selected semivolatile organic compounds in drinking waters. Accuracy and precision data have been generated in reagent water, and in finished ground and surface waters for the compounds li...

Nanofluid of zinc oxide nanoparticles in ionic liquid for single drop liquid microextraction of fungicides in environmental waters prior to high performance liquid chromatographic analysis.

PubMed

Amde, Meseret; Tan, Zhi-Qiang; Liu, Rui; Liu, Jing-Fu

2015-05-22

Using a nanofluid obtained by dispersing ZnO nanoparticles (ZnO NPs) in 1-hexyl-3-methylimidazolium hexafluorophosphate, new single drop microextraction method was developed for simultaneous extraction of three fungicides (chlorothalonil, kresoxim-methyl and famoxadone) in water samples prior to their analysis by high performance liquid chromatography (HPLC-VWD). The parameters affecting the extraction efficiency such as amount of ZnO NPs in the nanofluid, solvent volume, extraction time, stirring rate, pH and ionic strength of the sample solution were optimized. Under the optimized conditions, the limits of detection were in the range of 0.13-0.19ng/mL, the precision of the method assessed with intra-day and inter-day relative standard deviations were <4.82% and <7.04%, respectively. The proposed method was successfully applied to determine the three fungicides in real water samples including lake water, river water, as well as effluent and influent of wastewater treatment plant, with recoveries in the range of 74.94-96.11% at 5ng/mL spiking level. Besides to being environmental friendly, the high enrichment factor and the data quality obtained with the proposed method demonstrated its potential for application in multi residue analysis of fungicides in actual water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

PubMed

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of isothiazolinones in environmental waters by gas chromatography-mass spectrometry.

PubMed

Rafoth, Astrid; Gabriel, Sabine; Sacher, Frank; Brauch, Heinz-Jürgen

2007-09-14

This paper describes an analytical method for the determination of five biocides of isothiazolinone type (2-methyl-3-isothiazolinone (MI), 5-chloro-2-methyl-3-isothiazolinone (CMI), 1,2-benzisothiazolinone (BIT), 2-octyl-3-isothiazolinone (OI), 4,5-dichloro-2-octyl-3-isothiazolinone (DCOI)) in environmental waters. The method is based on pre-concentration of the analytes by solid-phase extraction onto a mixture of a polymeric material and RP-C18 material and subsequent determination by gas chromatography-mass spectrometry (GC-MS). One of the target compounds (BIT) is derivatised with diazomethane after pre-concentration to improve its chromatographic performance. The method was optimised with respect to pre-concentration conditions (liquid-liquid extraction versus solid-phase extraction, solid-phase material, elution solvent and volume) and extensively validated. Applying the method to surface waters, groundwaters, and drinking waters, limits of detection between 0.01 and 0.1 microg/l could be achieved and the repeatability was below 10% for all compounds except for MI. Additional investigations showed that the stability of the isothiazolinones in environmental waters is limited and sample storage at 4 degrees C is mandatory to preserve the target biocides. First investigations of influents and effluents of a wastewater treatment plant showed that conventional wastewater treatment exhibits a high efficiency for removal of the isothiazolinones. In river waters, the target isothiazolinones could not be detected.

Changes in total phenol, flavonoid contents and anti-Lactobacillus activity of Callisia fragrans due to extraction solvent

NASA Astrophysics Data System (ADS)

Le, Thom; Cao, Diem Kieu; Pham, Thanh Vy; Huynh, Tan Dat; Ta, Nhat Thuy Anh; Nguyen, Ngoc Thao Linh; Nguyen, Huu Thanh; Le, Hue Huong; Bui, Anh Vo; Truong, Dieu-Hien

2018-04-01

Callisia fragrans is a wonder herb with many medicinal properties such as burn, dental diseases, cancer diseases and arthritis in folk medicine. It is noted that the phytochemical constituents and antimicrobial activity of traditional plants depend on not only the extracting method but also the solvent used for extraction. In this study, the effect of five extraction solvents (i.e., distilled water, 80% methanol, 80% ethanol, 80% ethyl acetate, and 80% chloroform) on yield, total phenolic content (TPC) and total flavonoid content (TFC) of Callisia leaves was determined. Besides, changes in anti-Lactobacillus fermentum activity of C. fragrans freeze-dried extract was also evaluated using disk-diffusion method. The recovery percentage of extractable yield of fresh leaves are ranged from 11.93% w/w for distilled water extract to 16.60% w/w for aqueous ethanol extracts. The yield of 80% aqueous methanol extract (16.27% w/w) is only slightly less than that of the ethanol extract. Significant differences were observed among TPC and TFC obtaining by 80% methanol (0.0522% and 0.0335% w/w, respectively) compared to other solvents (p < 0.05). TPC and TFC of C. fragrans extracts increase in the following order: distilled water < 80% chloroform < 80% ethyl acetate < 80% ethanol < 80% methanol. The results revealed that 80% aqueous methanol Calissia extracts has moderate inhibition (9.0 mm of inhibition zone for 1.5 mg/mL of extracts) of L. fermentum compared to standard antibacterial agent. Based on the study results, it can be concluded that the yield, TPC and TFC of C. frgrans extract varied with the extracting solvent. It also showed that Callisia extracts can prevent dental caries by inhibiting the growth of L. fermentum, towards new insights for treatment of dental caries.

Optimization of a sensitive method for the determination of nitro musk fragrances in waters by solid-phase microextraction and gas chromatography with micro electron capture detection using factorial experimental design.

PubMed

Polo, Maria; Garcia-Jares, Carmen; Llompart, Maria; Cela, Rafael

2007-08-01

A solid-phase microextraction method (SPME) followed by gas chromatography with micro electron capture detection for determining trace levels of nitro musk fragrances in residual waters was optimized. Four nitro musks, musk xylene, musk moskene, musk tibetene and musk ketone, were selected for the optimization of the method. Factors affecting the extraction process were studied using a multivariate approach. Two extraction modes (direct SPME and headspace SPME) were tried at different extraction temperatures using two fiber coatings [Carboxen-polydimethylsiloxane (CAR/PDMS) and polydimethylsiloxane-divinylbenzene (PDMS/DVB)] selected among five commercial tested fibers. Sample agitation and the salting-out effect were also factors studied. The main effects and interactions between the factors were studied for all the target compounds. An extraction temperature of 100 degrees C and sampling the headspace over the sample, using either CAR/PDMS or PDMS/DVB as fiber coatings, were found to be the experimental conditions that led to a more effective extraction. High sensitivity, with detection limits in the low nanogram per liter range, and good linearity and repeatability were achieved for all nitro musks. Since the method proposed performed well for real samples, it was applied to different water samples, including wastewater and sewage, in which some of the target compounds (musk xylene and musk ketone) were detected and quantified.

Simultaneous determination of 12 pharmaceuticals in water samples by ultrasound-assisted dispersive liquid-liquid microextraction coupled with ultra-high performance liquid chromatography with tandem mass spectrometry.

PubMed

Guan, Jin; Zhang, Chi; Wang, Yang; Guo, Yiguang; Huang, Peiting; Zhao, Longshan

2016-11-01

A new analytical method was developed for simultaneous determination of 12 pharmaceuticals using ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) followed by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). Six nonsteroidal anti-inflammatory drugs (NSAIDs, ketoprofen, mefenamic acid, tolfenamic acid, naproxen, sulindac, and piroxicam) and six antibiotics (tinidazole, cefuroxime axetil, ciprofloxacin, sulfamethoxazole, sulfadiazine, and chloramphenicol) were extracted by ultrasound-assisted DLLME using dichloromethane (800 μL) and methanol/acetonitrile (1:1, v/v, 1200 μL) as the extraction and dispersive solvents, respectively. The factors affecting the extraction efficiency, such as the type and volume of extraction and dispersive solvent, vortex and ultrasonic time, sample pH, and ionic strength, were optimized. The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution by using a small volume of dispersive solvent, which increased the extraction efficiency and reduced the equilibrium time. Under the optimal conditions, the calibration curves showed good linearity in the range of 0.04-20 ng mL -1 (ciprofloxacin and sulfadiazine), 0.2-100 ng mL -1 (ketoprofen, tinidazole, cefuroxime axetil, naproxen, sulfamethoxazole, and sulindac), and 1-200 ng mL -1 (mefenamic acid, tolfenamic acid, piroxicam, and chloramphenicol). The LODs and LOQs of the method were in the range of 0.006-0.091 and 0.018-0.281 ng mL -1 , respectively. The relative recoveries of the target analytes were in the range from 76.77 to 99.97 % with RSDs between 1.6 and 8.8 %. The developed method was successfully applied to the extraction and analysis of 12 pharmaceuticals in five kinds of water samples (drinking water, running water, river water, influent and effluent wastewater) with satisfactory results. Graphical Abstract Twelve pharmaceuticals in water samples analyted by UHPLC-MS/MS using ultrasound-assisted DLLME.

Novel chromatographic separation and carbon solid-phase extraction of acetanilide herbicide degradation products.

PubMed

Shoemaker, Jody A

2002-01-01

One acetamide and 5 acetanilide herbicides are currently registered for use in the United States. Over the past several years, ethanesulfonic acid (ESA) and oxanilic acid (OA) degradation products of these acetanilide/acetamide herbicides have been found in U.S. ground waters and surface waters. Alachlor ESA and other acetanilide degradation products are listed on the U.S. Environmental Protection Agency's (EPA) 1998 Drinking Water Contaminant Candidate List. Consequently, EPA is interested in obtaining national occurrence data for these contaminants in drinking water. EPA currently does not have a method for determining these acetanilide degradation products in drinking water; therefore, a research method is being developed using liquid chromatography/negative ion electrospray/mass spectrometry with solid-phase extraction (SPE). A novel chromatographic separation of the acetochlor/alachlor ESA and OA structural isomers was developed which uses an ammonium acetate-methanol gradient combined with heating the analytical column to 70 degrees C. Twelve acetanilide degradates were extracted by SPE from 100 mL water samples using carbon cartridges with mean recoveries >90% and relative standard deviations < or =16%.

Determination of Prometryne in water and soil by HPLC-UV using cloud-point extraction.

PubMed

Zhou, Jihai; Chen, Jiandong; Cheng, Yanhong; Li, Daming; Hu, Feng; Li, Huixin

2009-07-15

A CPE-HPLC (UV) method has been developed for the determination of Prometryne. In this method, non-ionic surfactant Triton X-114 was first used to extract and pre-concentrate Prometryne from water and soil samples. The separation and determination of Prometryne were then carried out in an HPLC-UV system with isocratic elution using a detector set at 254 nm wavelength. The parameters and variables that affected the extraction were also investigated and the optimal conditions were found to be 0.5% of Triton X-114 (w/v), 3% of NaCl (w/v) and heat-assisted at 50 degrees C for 30 min. Using these conditions, the recovery rates of Prometryne ranged from 92.84% to 99.23% in water and 85.48% to 93.67% in soil, respectively, with all the relative standard deviations less than 3.05%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.5 microg L(-1) and 11.0 microg L(-1) in water and 4.0 microg kg(-1) and 13.0 microg kg(-1) in soil, respectively. Thus, we developed a method that has proven to be an efficient, green, rapid and inexpensive approach for extraction and determination of Prometryne from soil samples.

Application of cation-exchange solid-phase extraction for the analysis of amino alcohols from water and human plasma for verification of Chemical Weapons Convention.

PubMed

Kanaujia, Pankaj K; Tak, Vijay; Pardasani, Deepak; Gupta, A K; Dubey, D K

2008-03-28

The analysis of nitrogen containing amino alcohols, which are the precursors and degradation products of nitrogen mustards and nerve agent VX, constitutes an important aspect for verifying the compliance to the CWC (Chemical Weapons Convention). This work devotes on the development of solid-phase extraction method using silica- and polymer-based SCX (strong cation-exchange) and MCX (mixed-mode strong cation-exchange) cartridges for N,N-dialkylaminoethane-2-ols and alkyl N,N-diethanolamines, from water. The extracted analytes were analyzed by GC-MS (gas chromatography-mass spectrometry) in the full scan and selected ion monitoring modes. The extraction efficiencies of SCX and MCX cartridges were compared, and results revealed that SCX performed better. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 2 mL methanol containing 10% NH(4)OH and limits of detection could be achieved up to 5 x 10(-3) microg mL(-1) in the selected ion monitoring mode and 0.01 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of amino alcohol present in water sample sent by Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests. The method was also applied to extract the analytes from human plasma. The SCX cartridge showed good recoveries of amino alcohols from human plasma after protein precipitation.

Rapid determination of eight bioactive alkaloids in Portulaca oleracea L. by the optimal microwave extraction combined with positive-negative conversion multiple reaction monitor (+/-MRM) technology.

PubMed

Liang, Xiao; Tian, Jinlong; Li, Lingzhi; Gao, Jun; Zhang, Qingyi; Gao, Pinyi; Song, Shaojiang

2014-03-01

A rapid and reliable microwave extraction and the triple quadrupole-linear ion trap mass spectrometry method was developed and validated for the determination of eight alkaloids in Portulaca oleracea L. The optimal microwave extraction (MWE) condition was performed at 60 °C for 12 min with ethanol-water (70:30, v/v) as the extracting solvent, and the solvent to solid ratio was 30:1. The alkaloids were first detected simultaneously by electrospray ionization tandem mass spectrometry under positive-negative conversion multiple reaction monitor ((+/-)MRM) technique. With investigating three different columns, samples were separated in only 8 min on a Waters ACQUITY UPLC HSS T3 (50 × 2.1 mm(2), 1.8 μm) column using acetonitrile and formic acid-water solution as a mobile phase with a flow rate at 0.2 mL/min. All calibration curves showed good linearity (r>0.999) within the test ranges. The method developed was validated with acceptable sensitivity, intra- and inter-day precision, reproducibility, and extraction recoveries. It was successfully applied to the determination of eight alkaloids in Portulaca oleracea L. from different sources and different harvest periods. The method also provide a reference for extraction and determination of alkaloids in other complex systems. © 2013 Elsevier B.V. All rights reserved.

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination.

PubMed

Mogolodi Dimpe, K; Mpupa, Anele; Nomngongo, Philiswa N

2018-01-05

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5μgL -1 and 1.7μgL -1 , respectively, and intraday and interday precision expressed in terms of relative standard deviation were >6%.The maximum adsorption capacity was 138mgg -1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of 70 Environmental Protection Agency priority pharmaceuticals in water by EPA Method 1694.

PubMed

Ferrer, Imma; Zweigenbaum, Jerry A; Thurman, E Michael

2010-09-03

The U.S. Environmental Protection Agency (EPA) Method 1694 for the determination of pharmaceuticals in water recently brought a new challenge for treatment utilities, where pharmaceuticals have been reported in the drinking water of 41-million Americans. This proposed methodology, designed to address this important issue, consists of solid-phase extraction (SPE) followed by liquid chromatography-mass spectrometry (LC/MS-MS) using triple quadrupole. Under the guidelines of Method 1694, a multi-residue method was developed, validated, and applied to wastewater, surface water and drinking water samples for the analysis of 70 pharmaceuticals. Four distinct chromatographic gradients and LC conditions were used according to the polarity and extraction of the different pharmaceuticals. Positive and negative ion electrospray were used with two MRM transitions (a quantifier and a qualifier ion for each compound), which adds extra confirmation not included in the original Method 1694. Finally, we verify, for the first time, EPA Method 1694 on water samples collected in several locations in Colorado, where positive identifications for several pharmaceuticals were found. This study is a valuable indicator of the potential of LC/MS-MS for routine quantitative multi-residue analysis of pharmaceuticals in drinking water and wastewater samples and will make monitoring studies much easier to develop for water utilities across the US, who are currently seeking guidance on analytical methods for pharmaceuticals in their water supplies. 2010 Elsevier B.V. All rights reserved.

A selective electromembrane extraction of uranium (VI) prior to its fluorometric determination in water.

PubMed

Davarani, Saied Saeed Hosseiny; Moazami, Hamid Reza; Keshtkar, Ali Reza; Banitaba, Mohammad Hossein; Nojavan, Saeed

2013-06-14

A novel method for the selective electromembrane extraction (EME) of U(6+) prior to fluorometric determination has been proposed. The effect of extraction conditions including supported liquid membrane (SLM) composition, extraction time and extraction voltage were investigated. An SLM composition of 1% di-2-ethyl hexyl phosphonic acid in nitrophenyl octyl ether (NPOE) showed good selectivity, recovery and enrichment factor. The best performance was achieved at an extraction potential of 80 volts and an extraction time of 14 minutes Under the optimized conditions, a linear range from 1 to 1000 ng mL(-1) and LOD of 0.1 ng mL(-1) were obtained for the determination of U(6+). The EME method showed good performance in sample cleanup and the reduction of the interfering effects of Mn(2+), Zn(2+), Cd(2+), Ni(2+), Fe(3+), Co(2+), Cu(2+), Cl(-) and PO4(3-) ions during fluorometric determination of uranium in real water samples. The recoveries above 54% and enrichment factors above 64.7 were obtained by the proposed method for real sample analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

Oil extraction from algae: A comparative approach.

PubMed

Valizadeh Derakhshan, Mehrab; Nasernejad, Bahram; Abbaspour-Aghdam, Farzin; Hamidi, Mohammad

2015-01-01

In this article, various methods including soxhlet, Bligh & Dyer (B&D), and ultrasonic-assisted B&D were investigated for the extraction of lipid from algal species Chlorella vulgaris. Relative polarity/water content and impolar per polar ratios of solvents were considered to optimize the relative proportions of each triplicate agent by applying the response surface method (RSM). It was found that for soxhlet, hexane-methanol (54-46%, respectively) with total lipid extraction of 14.65% and chloroform-methanol (54-46%, respectively) with the extraction of 19.87% lipid were the best set of triplicate where further addition of acetone to the first group and ethanol to the second group did not contributed to further extraction. In B&D, however, chloroform-methanol-water (50%-35%-15%, respectively) reached the all-time maximum of 24%. Osmotic shock as well as ultrasonication contributed to 3.52% of further extraction, which is considered to promote the total yield up to almost 15%. From the growth data and fatty acid analysis, the applied method was assessed to be appropriate for biodiesel production with regard to selectivity and extraction yield. © 2014 International Union of Biochemistry and Molecular Biology, Inc.

Analysis of Free Amino Acids in Different Extracts of Orthosiphon stamineus Leaves by High-Performance Liquid Chromatography Combined with Solid-Phase Extraction.

PubMed

Shafaei, Armaghan; Halim, Nor Hidayah Ab; Zakaria, Norhidayah; Ismail, Zhari

2017-10-01

Orthosiphon stamineus (OS) Benth is a medicinal plant and native in Southeast Asia. Previous studies have shown that OS leaves possess antioxidant, cytotoxic, diuretic, antihypertensive, and uricosuric effects. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids, and flavonoids. To develop and validate an high-performance liquid chromatography (HPLC)-diode array detector (DAD) method combined with solid-phase extraction that involves precolumn derivatization with O -phthaladehyde for simultaneous analysis of free amino acids in OS leaves extracts. OS leaves were extracted with water (OS-W), ethanol (OS-E), methanol (OS-M), 50% ethanol (OS-EW), and 50% methanol (OS-MW). The extracts were treated by C18 cartridge before derivatization, resulting in great improvement of separation by Zorbox Eclipse XDB-C 18 column. The HPLC-DAD method was successfully developed and validated for analyzing the contents of free amino acids in OS extracts. The results showed that l-aspartic acid with 0.93 ± 0.01 nmol/mg was the major free amino acid in OS-W extract. However, in OS-E, OS-M, OS-EW, and OS-MW, l-glutamic acid with 3.53 ± 0.16, 2.17 ± 0.10, 4.01 ± 0.12, and 2.49 ± 0.12 nmol/mg, respectively, was the major free amino acid. Subsequently, l-serine, which was detected in OS-W, OS-E, and OS-M, was the minor free amino acid with 0.33 ± 0.02, 0.12 ± 0.01, and 0.06 ± 0.01 nmol/mg, respectively. However, l-threonine with 0.26 ± 0.02 and 0.19 ± 0.08 nmol/mL in OS-EW and OS-MW, respectively, had the lowest concentration compared with other amino acid components. All validation parameters of the developed method indicate that the method is reliable and efficient to simultaneously determine the free amino acids content for routine analysis of OS extracts. The HPLC-DAD method combined with solid phase extraction was successfully developed and validated for simultaneous determination and quantification of 17 free amino acids in Orthosiphon stamineus (OS) Benth extractsOS extracts were found to be rich in free amino acid contentL-aspartic acid was the major free amino acid in OS water extract while, in OS ethanol, methanol, 50% ethanol and 50% methanol extracts, L-glutamic acid was the major free amino acidL-serine was the minor free amino acid in OS water, ethanol and methanol extracts while, in OS 50% ethanol and 50% methanol extracts, L-threonine had the lowest concentration compared to other amino acid components. Abbreviations used: HPLC-DAD: High-Performance Liquid Chromatography with Diode-Array Detection, OS: Orthosiphon stamineus , OS-W: Orthosiphon stamineus water extract, OS-E: Orthosiphon stamineus ethanol extract, OS-M: Orthosiphon stamineus methanol extract, OS-EW: Orthosiphon stamineus 50% ethanol extract, OS-MW: Orthosiphon stamineus 50% methanol extract, OPA: O-phthaladehyde , SPE: Solid Phase Extraction, UV: Ultraviolet, LOD: Limit of Detection, LOQ: Limit of Quantification, RSD: Relative Standard Deviation.

Collagen proteins exchange O with demineralisation and gelatinisation reagents and also with atmospheric moisture.

PubMed

von Holstein, Isabella; von Tersch, Matthew; Coutu, Ashley N; Penkman, Kirsty E H; Makarewicz, Cheryl A; Collins, Matthew J

2018-01-23

The oxygen isotope composition of collagen proteins is a potential indicator of adult residential location, useful for provenancing in ecology, archaeology and forensics. In acidic solution, proteins can exchange O from carboxylic acid moieties with reagent O. This study investigated whether this exchange occurs during demineralisation and gelatinisation preparation of bone/ivory collagen. EDTA and HCl demineralisation or gelatinisation reagents were made up in waters with different δ 18 O values, and were used to extract collagen from four skeletal tissue samples. Aliquots of extracted collagen were exposed to two different atmospheric waters, at 120°C and ambient temperature, and subsequently dried in a vacuum oven at 40°C or by freeze drying. Sample δ 18 O values were measured by HT/EA pyrolysis-IRMS using a zero-blank autosampler. Collagen samples exchanged O with both reagent waters and atmospheric water, which altered sample δ 18 O values. Exchange with reagent waters occurred in all extraction methods, but was greater at lower pH. Damage to the collagen samples during extraction increased O exchange. The nature of exchange of O with atmospheric water depended on the temperature of exposure: kinetic fractionation of O was identified at 120°C but not at ambient temperature. Exchange was difficult to quantify due to high variability of δ 18 O value between experimental replicates. Studies of δ 18 O values in collagen proteins should avoid extraction methods using acid solutions. This article is protected by copyright. All rights reserved.

Analysis of Free Amino Acids in Different Extracts of Orthosiphon stamineus Leaves by High-Performance Liquid Chromatography Combined with Solid-Phase Extraction

PubMed Central

Shafaei, Armaghan; Halim, Nor Hidayah Ab; Zakaria, Norhidayah; Ismail, Zhari

2017-01-01

Background: Orthosiphon stamineus (OS) Benth is a medicinal plant and native in Southeast Asia. Previous studies have shown that OS leaves possess antioxidant, cytotoxic, diuretic, antihypertensive, and uricosuric effects. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids, and flavonoids. Objective: To develop and validate an high-performance liquid chromatography (HPLC)-diode array detector (DAD) method combined with solid-phase extraction that involves precolumn derivatization with O-phthaladehyde for simultaneous analysis of free amino acids in OS leaves extracts. Materials and Methods: OS leaves were extracted with water (OS-W), ethanol (OS-E), methanol (OS-M), 50% ethanol (OS-EW), and 50% methanol (OS-MW). The extracts were treated by C18 cartridge before derivatization, resulting in great improvement of separation by Zorbox Eclipse XDB-C18 column. Results: The HPLC–DAD method was successfully developed and validated for analyzing the contents of free amino acids in OS extracts. The results showed that l-aspartic acid with 0.93 ± 0.01 nmol/mg was the major free amino acid in OS-W extract. However, in OS-E, OS-M, OS-EW, and OS-MW, l-glutamic acid with 3.53 ± 0.16, 2.17 ± 0.10, 4.01 ± 0.12, and 2.49 ± 0.12 nmol/mg, respectively, was the major free amino acid. Subsequently, l-serine, which was detected in OS-W, OS-E, and OS-M, was the minor free amino acid with 0.33 ± 0.02, 0.12 ± 0.01, and 0.06 ± 0.01 nmol/mg, respectively. However, l-threonine with 0.26 ± 0.02 and 0.19 ± 0.08 nmol/mL in OS-EW and OS-MW, respectively, had the lowest concentration compared with other amino acid components. Conclusion: All validation parameters of the developed method indicate that the method is reliable and efficient to simultaneously determine the free amino acids content for routine analysis of OS extracts. SUMMARY The HPLC-DAD method combined with solid phase extraction was successfully developed and validated for simultaneous determination and quantification of 17 free amino acids in Orthosiphon stamineus (OS) Benth extractsOS extracts were found to be rich in free amino acid contentL-aspartic acid was the major free amino acid in OS water extract while, in OS ethanol, methanol, 50% ethanol and 50% methanol extracts, L-glutamic acid was the major free amino acidL-serine was the minor free amino acid in OS water, ethanol and methanol extracts while, in OS 50% ethanol and 50% methanol extracts, L-threonine had the lowest concentration compared to other amino acid components. Abbreviations used: HPLC-DAD: High-Performance Liquid Chromatography with Diode-Array Detection, OS: Orthosiphon stamineus, OS-W: Orthosiphon stamineus water extract, OS-E: Orthosiphon stamineus ethanol extract, OS-M: Orthosiphon stamineus methanol extract, OS-EW: Orthosiphon stamineus 50% ethanol extract, OS-MW: Orthosiphon stamineus 50% methanol extract, OPA: O-phthaladehyde, SPE: Solid Phase Extraction, UV: Ultraviolet, LOD: Limit of Detection, LOQ: Limit of Quantification, RSD: Relative Standard Deviation. PMID:29142388

Method 1664, Revision A: n-hexane extractable material (HEM; oil and grease) and silica gel treated n-hexane extractable material (SGT-HEM; non-polar material) by extraction and gravimetry

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

Not Available

This method is for determination of n-hexane extractable material (HEM; oil and grease) and n-hexane extractable material that is not adsorbed by silica gel (SGT-HEM; non-polar material) in surface and saline waters and industrial and domestic aqueous wastes. Extractable materials that may be determined are relatively non-volatile hydrocarbons, vegetable oils, animal fats, waxes, soaps, greases, and related materials. This method is capable of measuring HEM and SGT-HEM in the range of 5 to 1000 mg/L, and may be extended to higher levels by analysis of a smaller sample volume collected separately.

Comparison of the Composition and Antioxidant Activities of Phenolics from the Fruiting Bodies of Cultivated Asian Culinary-Medicinal Mushrooms.

PubMed

Lin, Shaoling; Ching, Lai Tsz; Ke, Xinxin; Cheung, Peter Chi Keung

2016-01-01

The composition profile and the antioxidant properties of phenolics in water extracts obtained from the fresh fruiting bodies of 4 common cultivated Asian edible mushrooms-Agrocybe aegerita, Pleurotus ostreatus, P. eryngii, and Pholiota nameko were compared. The water extract from A. aegerita (AaE) had the highest total phenolic content (TPC) at 54.18 ± 0.27 gallic acid equivalents (μmol/L)/mg extract (P < 0.05), as measured by the Folin-Ciocalteu method, and consisted of the largest number (including gallic acid, protocatechuic acid, chlorogenic acid, ferulic acid, and sinapic acid) and total amounts of phenolic acids identified by Fourier transform-ion cyclotron resonance mass spectrometry. The water extract of Ph. nameko was found to have the second-highest TPC (43.55 ± 0.10 gallic acid equivalents [μmol/L]/mg extract), followed by the water extract of P. eryngii and the water extract of P. ostreatus (39.55 ± 0.25 and 39.02 ± 0.30 gallic acid equivalents/mg extract, respectively). The scavenging activities of the water extracts from these mushrooms were evaluated against 2,2-diphenyl-l-(2,4,6-trinitrophenyl) hydrazyl diphenylpicrylhydrazyl (DPPH), superoxide anion radicals, hydroxyl radicals, and hydrogen peroxide. Based on halfmaximal effective concentrations, AaE was more effective in scavenging hydrogen peroxide (<0.05), followed by DPPH (0.51 mg/mL), superoxide anion radicals (0.85 mg/mL) and hydroxyl radicals (5.94 mg/mL), then the other mushroom water extracts. The differences in the half-maximal effective concentrations of individual mushroom water extracts were probably the result of the different numbers and amounts of individual phenolic acids in the extracts. The antioxidant activities of the mushroom water extracts were correlated with their TPC. The strongest antioxidant properties of AaE were consistent with its highest TPC and with the largest number and amount of phenolics identified in the extract. These results indicated that cultivated edible mushrooms could be a potential source of natural antioxidants with free radical scavenging properties for application as a functional food ingredient.

Physicochemical properties and antimicrobial activity of Roselle (Hibiscus sabdariffa L.).

PubMed

Jung, EunKyung; Kim, YoungJun; Joo, Nami

2013-12-01

The therapeutic action of a plant depends on its chemical constituents. In this study, experiments were carried out in order to evaluate the effect of extraction conditions on the antioxidative and antimicrobial activities of Roselle (Hibiscus sabdariffa L.). Roselle was found to be rich in malic acid, anthocyanins, ascorbic acid and minerals, especially Ca and Fe, but low in glucose. More than 18 volatile compounds were identified by gas chromatography and gas chromatography-mass spectrometry. This herb, which is rich in phenolic compounds and displays DPPH radical scavenging activity, could be a good source of natural antioxidants. The antimicrobial activity of the Roselle water and ethanol extracts was tested with Bacillus subtilis (ATCC6633), Staphylococcus aureus (ATCC6538) and Escherichia coli (ATCC 8739). The inhibition of the Roselle ethanol extract against B. subtilis and S. aureus was slightly higher than that of water extract but this difference was not significant. However, E. coli was strongly inhibited by the Roselle water extract at concentrations of 25 and 50 mg mL(-1) as determined by a paper disc method. The obtained results indicated that antioxidant and antimicrobial activity was related to different methods of extraction and Roselle extracts could be a source of therapeutically useful products. © 2013 Society of Chemical Industry.

Fabrication of a novel hydrophobic/ion-exchange mixed-mode adsorbent for the dispersive solid-phase extraction of chlorophenols from environmental water samples.

PubMed

Gao, Li; Wei, Yinmao

2016-08-01

A novel mixed-mode adsorbent was prepared by functionalizing silica with tris(2-aminoethyl)amine and 3-phenoxybenzaldehyde as the main mixed-mode scaffold due to the presence of the plentiful amino groups and benzene rings in their molecules. The adsorption mechanism was probed with acidic, natural and basic compounds, and the mixed hydrophobic and ion-exchange interactions were found to be responsible for the adsorption of analytes. The suitability of dispersive solid-phase extraction was demonstrated in the determination of chlorophenols in environmental water. Several parameters, including sample pH, desorption solvent, ionic strength, adsorbent dose, and extraction time were optimized. Under the optimal extraction conditions, the proposed dispersive solid-phase extraction coupled with high-performance liquid chromatography showed good linearity range and acceptable limits of detection (0.22∽0.54 ng/mL) for five chlorophenols. Notably, the higher extraction recoveries (88.7∽109.7%) for five chlorophenols were obtained with smaller adsorbent dose (10 mg) and shorter extraction time (15 min) compared with the reported methods. The proposed method might be potentially applied in the determination of trace chlorophenols in real water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

New sorbent in the dispersive solid phase extraction step of quick, easy, cheap, effective, rugged, and safe for the extraction of organic contaminants in drinking water treatment sludge.

PubMed

Cerqueira, Maristela B R; Caldas, Sergiane S; Primel, Ednei G

2014-04-04

Recent studies have shown a decrease in the concentration of pesticides, pharmaceuticals and personal care products (PCPs) in water after treatment. A possible explanation for this phenomenon is that these compounds may adhere to the sludge; however, investigation of these compounds in drinking water treatment sludge has been scarce. The sludge generated by drinking water treatment plants during flocculation and decantation steps should get some special attention not only because it has been classified as non-inert waste but also because it is a very complex matrix, consisting essentially of inorganic (sand, argil and silt) and organic (humic substances) compounds. In the first step of this study, three QuEChERS methods were used, and then compared, for the extraction of pesticides (atrazine, simazine, clomazone and tebuconazole), pharmaceuticals (amitriptyline, caffeine, diclofenac and ibuprofen) and PCPs (methylparaben, propylparaben, triclocarban and bisphenol A) from drinking water treatment sludge. Afterwards, the study of different sorbents in the dispersive solid phase extraction (d-SPE) step was evaluated. Finally, a new QuEChERS method employing chitin, obtained from shrimp shell waste, was performed in the d-SPE step. After having been optimized, the method showed limits of quantification (LOQ) between 1 and 50 μg kg(-1) and the analytical curves showed r values higher than 0.98, when liquid chromatography tandem mass spectrometry was employed. Recoveries ranged between 50 and 120% with RSD≤15%. The matrix effect was evaluated and compensated with matrix-matched calibration. The method was applied to drinking water treatment sludge samples and methylparaben and tebuconazole were found in concentration

Noncontact methods for measuring water-surface elevations and velocities in rivers: Implications for depth and discharge extraction

USGS Publications Warehouse

Nelson, Jonathan M.; Kinzel, Paul J.; McDonald, Richard R.; Schmeeckle, Mark

2016-01-01

Recently developed optical and videographic methods for measuring water-surface properties in a noninvasive manner hold great promise for extracting river hydraulic and bathymetric information. This paper describes such a technique, concentrating on the method of infrared videog- raphy for measuring surface velocities and both acoustic (laboratory-based) and laser-scanning (field-based) techniques for measuring water-surface elevations. In ideal laboratory situations with simple flows, appropriate spatial and temporal averaging results in accurate water-surface elevations and water-surface velocities. In test cases, this accuracy is sufficient to allow direct inversion of the governing equations of motion to produce estimates of depth and discharge. Unlike other optical techniques for determining local depth that rely on transmissivity of the water column (bathymetric lidar, multi/hyperspectral correlation), this method uses only water-surface information, so even deep and/or turbid flows can be investigated. However, significant errors arise in areas of nonhydrostatic spatial accelerations, such as those associated with flow over bedforms or other relatively steep obstacles. Using laboratory measurements for test cases, the cause of these errors is examined and both a simple semi-empirical method and computational results are presented that can potentially reduce bathymetric inversion errors.

Characterization of halogenated DBPs and identification of new DBPs trihalomethanols in chlorine dioxide treated drinking water with multiple extractions.

PubMed

Han, Jiarui; Zhang, Xiangru; Liu, Jiaqi; Zhu, Xiaohu; Gong, Tingting

2017-08-01

Chlorine dioxide (ClO 2 ) is a widely used alternative disinfectant due to its high biocidal efficiency and low-level formation of trihalomethanes and haloacetic acids. A major portion of total organic halogen (TOX), a collective parameter for all halogenated DBPs, formed in ClO 2 -treated drinking water is still unknown. A commonly used pretreatment method for analyzing halogenated DBPs in drinking water is one-time liquid-liquid extraction (LLE), which may lead to a substantial loss of DBPs prior to analysis. In this study, characterization and identification of polar halogenated DBPs in a ClO 2 -treated drinking water sample were conducted by pretreating the sample with multiple extractions. Compared to one-time LLE, the combined four-time LLEs improved the recovery of TOX by 2.3 times. The developmental toxicity of the drinking water sample pretreated with the combined four-time LLEs was 1.67 times higher than that pretreated with one-time LLE. With the aid of ultra-performance liquid chromatography/electrospray ionization-triple quadrupole mass spectrometry, a new group of polar halogenated DBPs, trihalomethanols, were detected in the drinking water sample pretreated with multiple extractions; two of them, trichloromethanol and bromodichloromethanol, were identified with synthesized standard compounds. Moreover, these trihalomethanols were found to be the transformation products of trihalomethanes formed during ClO 2 disinfection. The results indicate that multiple LLEs can significantly improve extraction efficiencies of polar halogenated DBPs and is a better pretreatment method for characterizing and identifying new polar halogenated DBPs in drinking water. Copyright © 2017. Published by Elsevier B.V.

Extraction and identification of flavonoids from parsley extracts by HPLC analysis

NASA Astrophysics Data System (ADS)

Stan, M.; Soran, M. L.; Varodi, C.; Lung, I.

2012-02-01

Flavonoids are phenolic compounds isolated from a wide variety of plants, and are valuable for their multiple properties, including antioxidant and antimicrobial activities. In the present work, parsley (Petroselinum crispum L.) extracts were obtained by three different extraction techniques: maceration, ultrasonic-assisted and microwave-assisted solvent extractions. The extractions were performed with ethanol-water mixtures in various ratios. From these extracts, flavonoids like the flavones apigenin and luteolin, and the flavonols quercetin and kaempferol were identified using an HPLC Shimadzu apparatus equipped with PDA and MS detectors. The separation method involved a gradient step. The mobile phase consisted of two solvents: acetonitrile and distilled water with 0.1% formic acid. The separation was performed on a RP-C18 column.

A New Method of Obtaining High-Resolution Paleoclimate Records from Speleothem Fluid Inclusions

NASA Astrophysics Data System (ADS)

Logan, A. J.; Horton, T. W.

2010-12-01

We present a new method for stable hydrogen and oxygen isotope analysis of ancient drip water trapped within cave speleothems. Our method improves on existing fluid inclusion isotopic analytical techniques in that it decreases the sample size by a factor of ten or more, dramatically improving the spatial and temporal precision of fluid inclusion-based paleoclimatology. Published thermal extraction methods require large samples (c. 150 mg) and temperatures high enough (c. 500-900°C) to cause calcite decomposition, which is also associated with isotopic fractionation of the trapped fluids. Extraction by crushing faces similar challenges, where the failure to extract all the trapped fluid can result in isotopic fractionation, and samples in excess of 500 mg are required. Our new method combines the strengths of these published thermal and crushing methods using continuous-flow isotope ratio analytical techniques. Our method combines relatively low-temperature (~250°C) thermal decrepitation with cryogenic trapping across a switching valve sample loop. In brief, ~20 mg carbonate samples are dried (75°C for >1 hour) and heated (250°C for >1 hour) in a quartz sample chamber under a continuously flowing stream of ultra-high purity helium. Heating of the sample chamber is achieved by use of a tube furnace. Fluids released during the heating step are trapped in a coiled stainless steel cold trap (~ -98°C) serving as the sample loop in a 6-way switching valve. Trapped fluids are subsequently injected into a high-temperature conversion elemental analyzer by switching the valve and rapidly thawing the trap. This approach yielded accurate and precise measurements of injected liquid water IAEA reference materials (GISP; SMOW2; SLAP2) for both hydrogen and oxygen isotopic compositions. Blanking tests performed on the extraction line demonstrate extremely low line-blank peak heights (<50mv). Our tests also demonstrate that complete recovery of liquid water is possible and that a minimum quantity of ~100nL water was required. In contrast to liquid water analyses, carbonate inclusion waters gave highly variable results. As plenty of signal was produced from relatively small sample sizes (~20 mg), the observed isotopic variation most likely reflects fractionation during fluid extraction, or natural isotopic variability. Additional tests and modifications to the extraction procedure are in progress, using a recently collected New Zealand stalagmite from a West Coast cave (DOC collection permit WC-27462-GEO). U-Th age data will accompany a paleoclimate record from this stalagmite obtained using standard carbonate analytical techniques, and compared to the results from our new fluid inclusion analyses.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory : determination of organophosphate pesticides in whole water by continuous liquid-liquid extraction and capillary-column gas chromatography with flame photometric detection

USGS Publications Warehouse

Jha, Virendra K.; Wydoski, Duane S.

2003-01-01

A method for the isolation of 20 parent organophosphate pesticides and 5 organophosphate pesticide degradates from natural-water samples is described. Compounds are extracted from water samples with methylene chloride using a continuous liquid-liquid extractor for 6 hours. The solvent is evaporated using heat and a flow of nitrogen to a volume of 1 milliliter and solvent exchanged to ethyl acetate. Extracted compounds are determined by capillary-column gas chromatography with flame photometric detection. Single-operator derived method detection limits in three water-matrix samples ranged from 0.003 to 0.009 microgram per liter. Method performance was validated by spiking all compounds in three different matrices at three different concentrations. Eight replicates were analyzed at each concentration in each matrix. Mean recoveries of most method compounds spiked in surface-water samples ranged from 54 to 137 percent and those in ground-water samples ranged from 40 to 109 percent for all pesticides. Recoveries in reagent-water samples ranged from 42 to 104 percent for all pesticides. The only exception was O-ethyl-O-methyl-S-propylphosphorothioate, which had variable recovery in all three matrices ranging from 27 to 79 percent. As a result, the detected concentration of O-ethyl-O-methyl-S-propylphosphorothioate in samples is reported in this method with an estimated remark code. Based on the performance issue, two more compounds, disulfoton and ethion monoxon, also will be reported in this method with an estimated remark code. Estimated-value compounds, which are ?E-coded? in the data base, do not meet the performance criteria for unqualified quantification, but are retained in the method because the compounds are important owing to high use or potential environmental effects and because analytical performance has been consistent and reproducible.

Evaluation of the anticancer potential of six herbs against a hepatoma cell line

PubMed Central

2012-01-01

Background Six herbs in the Plant Genetics Conservation Project that have been used as complementary medicines were chosen on the basis of their medicinal value, namely Terminalia mucronata, Diospyros winitii, Bridelia insulana, Artabotrys harmandii, Terminallia triptera, and Croton oblongifolius. This study aims to evaluate the potential anticancer activity of 50% ethanol-water extracts of these six herbs. Methods Fifty percent ethanol-water crude extracts of the six herbs were prepared. The cytotoxicity of the herbal extracts relative to that of melphalan was evaluated using a hepatoma cell line (HepG2), and examined by neutral red assays and apoptosis induction by gel electrophoresis and flow cytometry after 24 h. Results A significant difference was found between the cytotoxicity of the 50% ethanol-water crude extracts and melphalan (P = 0.000). The 50% ethanol-water crude extracts of all six herbs exhibited cytotoxicity against HepG2 cells, with IC50 values ranging from 100 to 500 μg/mL. The extract of T. triptera showed the highest cytotoxicity with an IC50 of 148.7 ± 12.3 μg/mL, while melphalan had an IC50 of 39.79 ± 7.62 μg/mL. The 50% ethanol-water crude extracts of D. winitii and T. triptera, but not A. harmandii, produced a DNA ladder. The 50% ethanol-water crude extracts of D. winitii, T. triptera, and A. harmandii induced apoptosis detected by flow cytometry. Conclusion The 50% ethanol-water crude extracts of D. winitii, T. triptera, and A. harmandii showed anticancer activity in vitro. PMID:22682026

Extraction of solubles from plant biomass for use as microbial growth stimulant and methods related thereto

DOEpatents

Lau, Ming Woei

2015-12-08

A method for producing a microbial growth stimulant (MGS) from a plant biomass is described. In one embodiment, an ammonium hydroxide solution is used to extract a solution of proteins and ammonia from the biomass. Some of the proteins and ammonia are separated from the extracted solution to provide the MGS solution. The removed ammonia can be recycled and the proteins are useful as animal feeds. In one embodiment, the method comprises extracting solubles from pretreated lignocellulosic biomass with a cellulase enzyme-producing growth medium (such T. reesei) in the presence of water and an aqueous extract.

Antibacterial efficacy and effect of Morinda citrifolia L. mixed with irreversible hydrocolloid for dental impressions: A randomized controlled trial

PubMed Central

Ahmed, A. Shafath; Charles, P. David; Cholan, R.; Russia, M.; Surya, R.; Jailance, L.

2015-01-01

Aim: This study aimed to evaluate whether the extract of Morinda citrifolia L. mixed with irreversible hydrocolloid powder decreases microbial contamination during impression making without affecting the resulting casts. Materials and Methods: Twenty volunteers were randomly divided into two groups (n = 10). Group A 30 ml extract of M. citrifolia L diluted in 30 ml of water was mixed to make the impression with irreversible hydrocolloid material. Group B 30 ml deionized water was mixed with irreversible hydrocolloid material to make the impressions following which the surface roughness and dimensional stability of casts were evaluated. Results: Extract of M. citrifolia L. mixed with irreversible hydrocolloid decreased the percentage of microorganisms when compared with water (P < 0.001) but did not affect the surface quality or dimensional stability of the casts. Conclusion: Mixing the extract of M. citrifolia L. with irreversible hydrocolloid powder is an alternative method to prevent contamination without sacrificing impression quality. PMID:26538926

Double-disk solid-phase extraction--Simultaneous cleanup and trace enrichment of herbicides and metabolites from environmental samples

USGS Publications Warehouse

Ferrar, Imma; Barceló, Damià; Thurman, E.M.

1999-01-01

Phenylurea and triazine herbicides, including some metabolites, were isolated from water and soil extracts by solid-phase extraction using a layered system of two extraction disks, a method called double-disk solid-phase extraction. The first disk consisted of strong anion exchange (SAX) of 10-μm styrene divinylbenzene (SDB) particles embedded in Teflon, and the second disk was a C18 disk of 10-μm particles also embedded in Teflon. A volume of 500 mL of water or aqueous soil extract is passed through the layered system with the SAX disk first. The purpose of the SAX disk is to remove the humic and fulvic acids from the water or aqueous soil extract by ion exchange through their carboxyl groups. Even during methanol elution of herbicides, the humic substances remain bound to the SAX disk with >85% retention. Elution with methanol results in more than 90% recovery of the herbicides from the layered extraction disks. Removal of the humic and fulvic acids results in greater sensitivity for diode array detection quantitation (0.05 μg/L for herbicides) by substantially reducing the absorbance of the humic peak on the LC chromatogram. The herbicides adsorb to the SAX disk either through hydrogen bonding to the anion-exchange sites or by hydrophobic interaction with the SDB surface of the anion-exchange disk. The method was tested for the analysis of natural water samples from the Mississippi Embayment, a cotton-growing area of the southeastern United States.

Comparison of accelerated solvent extraction and quick, easy, cheap, effective, rugged and safe method for extraction and determination of pharmaceuticals in vegetables.

PubMed

Chuang, Ya-Hui; Zhang, Yingjie; Zhang, Wei; Boyd, Stephen A; Li, Hui

2015-07-24

Land application of biosolids and irrigation with reclaimed water in agricultural production could result in accumulation of pharmaceuticals in vegetable produce. To better assess the potential human health impact from long-term consumption of pharmaceutical-contaminated vegetables, it is important to accurately quantify the amount of pharmaceuticals accumulated in vegetables. In this study, a quick, easy, cheap, effective, rugged and safe (QuEChERS) method was developed and optimized to extract multiple classes of pharmaceuticals from vegetables, which were subsequently quantified by liquid chromatography coupled to tandem mass spectrometry. For the eleven target pharmaceuticals in celery and lettuce, the extraction recovery of the QuEChERS method ranged from 70.1 to 118.6% with relative standard deviation <20%, and the method detection limit was achieved at the levels of nanograms of pharmaceuticals per gram of vegetables. The results revealed that the performance of the QuEChERS method was comparable to, or better than that of accelerated solvent extraction (ASE) method for extraction of pharmaceuticals from plants. The two optimized extraction methods were applied to quantify the uptake of pharmaceuticals by celery and lettuce growing hydroponically. The results showed that all the eleven target pharmaceuticals could be absorbed by the vegetables from water. Compared to the ASE method, the QuEChERS method offers the advantages of short time and reduced costs of sample preparation, and less amount of organic solvents used. The established QuEChERS method could be used to determine the accumulation of multiple classes of pharmaceutical residues in vegetables and other plants, which is needed to evaluate the quality and safety of agricultural produce consumed by humans. Copyright © 2015 Elsevier B.V. All rights reserved.

Green extraction of grape skin phenolics by using deep eutectic solvents.

PubMed

Cvjetko Bubalo, Marina; Ćurko, Natka; Tomašević, Marina; Kovačević Ganić, Karin; Radojčić Redovniković, Ivana

2016-06-01

Conventional extraction techniques for plant phenolics are usually associated with high organic solvent consumption and long extraction times. In order to establish an environmentally friendly extraction method for grape skin phenolics, deep eutectic solvents (DES) as a green alternative to conventional solvents coupled with highly efficient microwave-assisted and ultrasound-assisted extraction methods (MAE and UAE, respectively) have been considered. Initially, screening of five different DES for proposed extraction was performed and choline chloride-based DES containing oxalic acid as a hydrogen bond donor with 25% of water was selected as the most promising one, resulting in more effective extraction of grape skin phenolic compounds compared to conventional solvents. Additionally, in our study, UAE proved to be the best extraction method with extraction efficiency superior to both MAE and conventional extraction method. The knowledge acquired in this study will contribute to further DES implementation in extraction of biologically active compounds from various plant sources. Copyright © 2016 Elsevier Ltd. All rights reserved.

A novel strategy for isolation and determination of sugars and sugar alcohols from conifers.

PubMed

Sarvin, B A; Seregin, A P; Shpigun, O A; Rodin, I A; Stavrianidi, A N

2018-06-02

The ultrasound-assisted extraction method for isolation of 17 sugars and sugar alcohols from conifers with a subsequent hydrophilic interaction liquid chromatography-tandem mass spectrometry method for their determination is proposed. The optimization of extraction parameters was carried out using Taguchi - L 9 (3 4 ) orthogonal array experimental design for the following parameters-a methanol concentration in the extraction solution, an extraction time, a type of plant sample and an extraction temperature. The optimal ultrasound-assisted extraction conditions were-MeOH concentration - 30% (water - 70%), extraction time - 30 min, type of plant sample - II (grinded leaves 2-4 mm long), extraction temperature - 60 °C. Pure water and acetonitrile were used as eluents in gradient elution mode to separate the analytes. Direct determination of multiple sugars and sugar alcohols was carried out using a mass spectrometric detector operated in a multiple reaction monitoring mode, providing detection limits in the range between 0.1 and 20 ng/mL and good analytical characteristics of the method without derivatization. The developed approach was validated by multiple successive extraction method applied to test its performance on a series of 10 samples, i.e. 2 samples per each of 5 genera: Abies, Larix, Picea, Pinus (Pinaceae) and Juniperus (Cupressaceae), widely distributed in the boreal conifer forests of Eurasia. The novel strategy can be used for profiling of sugars and sugar alcohols in a wide range of plant species. Copyright © 2018. Published by Elsevier B.V.

Development of the extraction method for the simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge.

PubMed

Zuliani, Tea; Lespes, Gaetane; Milacic, Radmila; Scancar, Janez

2010-03-15

The toxicity and bioaccumulation of organotin compounds (OTCs) led to the development of sensitive and selective analytical methods for their determination. In the past much attention was assigned to the study of OTCs in biological samples, water and sediments, coming mostly from marine environment. Little information about OTCs pollution of terrestrial ecosystems is available. In order to optimise the extraction method for simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge five different extractants (tetramethylammonium hydroxide, HCl in methanol, glacial acetic acid, mixture of acetic acid and methanol (3:1), and mixture of acetic acid, methanol and water (1:1:1)), the presence or not of a complexing agent (tropolone), and the use of different modes of extraction (mechanical stirring, microwave and ultrasonic assisted extraction) were tested. Extracted OTCs were derivatised with sodium tetraethylborate and determined by gas chromatography coupled with mass spectrometer. Quantitative extraction of butyl-, phenyl- and octyltin compounds was obtained by the use of glacial acetic acid as extractant and mechanical stirring for 16h or sonication for 30 min. The limits of detection and quantification for OTCs investigated in sewage sludge were in the ng S ng(-1) range. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Development of water-phase derivatization followed by solid-phase microextraction and gas chromatography/mass spectrometry for fast determination of valproic acid in human plasma.

PubMed

Deng, Chunhui; Li, Ning; Ji, Jie; Yang, Bei; Duan, Gengli; Zhang, Xiangmin

2006-01-01

In this study, a simple, rapid, and sensitive method was developed and validated for the quantification of valproic acid (VPA), an antiepileptic drug, in human plasma, which was based on water-phase derivatization followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS). In the proposed method, VPA in plasma was rapidly derivatized with a mixture of isobutyl chloroformate, ethanol and pyridine under mild conditions (room temperature, aqueous medium), and the VPA ethyl ester formed was headspace-extracted and simultaneously concentrated using the SPME technique. Finally, the analyte extracted on SPME fiber was analyzed by GC/MS. The experimental parameters and method validations were studied. The optimal conditions were obtained: PDMS fiber, stirring rate of 1100 rpm, sample temperature of 80 degrees C, extraction time of 20 min, NaCl concentration of 30%. The proposed method had a limit of quantification (0.3 microg/mL), good recovery (89-97%) and precision (RSD value less than 10%). Because the proposed method combined a rapid water-phase derivatization with a fast, simple and solvent-free sample extraction and concentration technique of SPME, the sample preparation time was less than 25 min. This much shortens the whole analysis time of VPA in plasma. The validated method has been successfully used to analyze VPA in human plasma samples for application in pharmacokinetic studies. All these results show that water-phase derivatization followed by HS-SPME and GC/MS is an alternative and powerful method for fast determination of VPA in biological fluids. Copyright 2006 John Wiley & Sons, Ltd.

Method and apparatus for extracting water from air

DOEpatents

Spletzer, Barry L.

2001-01-01

The present invention provides a method and apparatus for extracting liquid water from moist air using minimal energy input. The method comprises compressing moist air under conditions that foster the condensation of liquid water (ideally isothermal to a humidity of 1.0, then adiabatic thereafter). The air can be decompressed under conditions that do not foster the vaporization of the condensate. The decompressed, dried air can be exchanged for a fresh charge of moist air and the process repeated. The liquid condensate can be removed for use. The apparatus can comprise a compression chamber having a variable internal volume. An intake port allows moist air into the compression chamber. An exhaust port allows dried air out of the compression chamber. A condensation device fosters condensation at the desired conditions. A condensate removal port allows liquid water to be removed.

Quantification of polyphenols and evaluation of antimicrobial, analgesic and anti-inflammatory activities of aqueous and acetone-water extracts of Libidibia ferrea, Parapiptadenia rigida and Psidium guajava.

PubMed

de Araújo, Aurigena Antunes; Soares, Luiz Alberto Lira; Assunção Ferreira, Magda Rhayanny; de Souza Neto, Manoel André; da Silva, Giselle Ribeiro; de Araújo, Raimundo Fernandes; Guerra, Gerlane Coelho Bernardo; de Melo, Maria Celeste Nunes

2014-10-28

Vast numbers of plant species from northeastern Brazil have not yet been phytochemically or biologically evaluated. The goal of this work was to obtain, characterize and show the antimicrobial, analgesic and anti-inflammatory activities of aqueous and acetone-water extracts of Libidibia ferrea, Parapiptadenia rigida and Psidium guajava. The plant material (100g) was dried, and the crude extracts were obtained by using turbo-extraction (10%; w/v) with water or acetone:water (7:3, v/v) as the extraction solvent. High-performance liquid chromatography (HPLC) methods were used to screen the crude extracts for hydrolysable tannins (gallic acid) and condensed tannins (catechins). The antibacterial activity was evaluated by agar-diffusion and microdilution methods against Gram-positive strains (Staphylococcus aureus ATCC 25923, Staphylococcus epidermidis INCQS 00016, Enterococcus faecalis ATCC 29212 and a clinical isolate of methicillin-resistant Staphylococcus aureus) as well as Gram-negative strains (Escherichia coli ATCC 25922, Salmonella enteritidis INCQS 00258, Shigella flexneri and Klebsiella pneumoniae). To evaluate the anti-inflammatory activity, a leukocyte migration model was used. Analgesic activity was determined by the hot plate test and the acetic acid-induced abdominal writhing test. Data were analyzed by analysis of variance (ANOVA) at a significance level of 5%. Parapiptadenia rigida presented the highest amount of total polyphenols (35.82 ± 0.20%), while the greatest catechin content was found in the acetone-water extract of Psidium guajava (EAWPg; 1.04 μg/g). The largest amounts of catechins were found in the aqueous extract of Libidibia ferrea (EALf; 1.07 μg/g) and the acetone-water extract of Parapiptadenia rigida (EAWPr; 1.0 μg/g). All extracts showed activity against Gram-positive bacteria. The aqueous and acetone-water extracts of Psidium guajava showed the greatest inhibition zones in the agar diffusion tests. In the evaluation of the minimum inhibitory concentration (MIC), the most susceptible Gram-positive bacterium was Staphylococcus epidermidis and the most susceptible Gram-negative bacterium was Shigella flexneri. EAPg and EAWPg showed the greatest MIC values. All extracts were significant inhibitors of leukocyte migration (p<0.05). Using the writhing test, significant analgesic activity was found for EAPr (50 mg/kg), EAWPr (100 mg/kg and 200 mg/kg) and EAWPg (50 mg/kg) (p<0.05). Thus, the appropriate extraction procedure preserves the chemical components such as gallic acid and catechin, and showed antimicrobial, anti-inflammatory and analgesic properties. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Detection of Giardia in environmental waters by immuno-PCR amplification methods.

PubMed

Mahbubani, M H; Schaefer, F W; Jones, D D; Bej, A K

1998-02-01

Genomic DNA was extracted either directly from Giardia muris cysts seeded into environmental surface waters or from cysts isolated by immunomagnetic beads (IMB). A 0.171-kbp segment of the giardin gene was PCR-amplified following "direct extraction" of Giardia DNA from seeded Cahaba river water concentrate with moderate turbidity (780 JTU's), but DNA purified from seeded Colorado river water concentrates with high turbidity (2 x 10(5) JTUs) failed to amplify. However, if the cysts were first separated by the IMB approach from seeded Cahaba or Colorado river waters, and the DNA released by a freeze-boil Chelex(R)100 treatment, detection of G. muris by PCR amplification could be achieved at a sensitivity of 3 x 10(0) or 3 x 10(1) cysts/ml, respectively. If, however, the G. muris cysts used to seed even moderately turbid river waters (780 JTUs) were formalin treated (which is conventionally used for microscopic examination), neither direct extraction nor IMB purification methods yielded amplifiable DNA. Use of immunomagnetic beads to separate Giardia cysts from complex matrices of environmental surface waters followed by DNA release and PCR amplification of the target giardin gene improved the reliability of detection of this pathogen with the required sensitivity.

Determination of chlorinated polycyclic aromatic hydrocarbons in water by solid-phase extraction coupled with gas chromatography and mass spectrometry.

PubMed

Wang, Xianli; Kang, Haiyan; Wu, Junfeng

2016-05-01

Given the potential risks of chlorinated polycyclic aromatic hydrocarbons, the analysis of their presence in water is very urgent. We have developed a novel procedure for determining chlorinated polycyclic aromatic hydrocarbons in water based on solid-phase extraction coupled with gas chromatography and mass spectrometry. The extraction parameters of solid-phase extraction were optimized in detail. Under the optimal conditions, the proposed method showed wide linear ranges (1.0-1000 ng/L) with correlation coefficients ranging from 0.9952 to 0.9998. The limits of detection and the limits of quantification were in the range of 0.015-0.591 and 0.045-1.502 ng/L, respectively. Recoveries ranged from 82.5 to 102.6% with relative standard deviations below 9.2%. The obtained method was applied successfully to the determination of chlorinated polycyclic aromatic hydrocarbons in real water samples. Most of the chlorinated polycyclic aromatic hydrocarbons were detected and 1-monochloropyrene was predominant in the studied water samples. This is the first report of chlorinated polycyclic aromatic hydrocarbons in water samples in China. The toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in the studied tap water were 9.95 ng the toxic equivalency quotient m(-3) . 9,10-Dichloroanthracene and 1-monochloropyrene accounted for the majority of the total toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in tap water. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ionic Liquid Dispersive Liquid-Liquid Microextraction Method for the Determination of Irinotecan, an Anticancer Drug, in Water and Urine Samples Using UV-Vis Spectrophotometry.

PubMed

Uysal, Deniz; Karadaş, Cennet; Kara, Derya

2017-05-01

A new, simple, efficient, and environmentally friendly ionic liquid dispersive liquid-liquid microextraction method was developed for the determination of irinotecan, an anticancer drug, in water and urine samples using UV-Vis spectrophotometry. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the extraction solvent, and ethanol was used as the disperser solvent. The main parameters affecting the extraction efficiency, including sample pH, volume of the ionic liquid, choice of the dispersive solvent and its volume, concentration of NaCl, and extraction and centrifugation times, were investigated and optimized. The effect of interfering species on the recovery of irinotecan was also examined. Under optimal conditions, the LOD (3σ) was 48.7 μg/L without any preconcentration. Because the urine sample was diluted 10-fold, the LOD for urine would be 487 μg/L. However, this could be improved 16-fold if preconcentration using a 40 mL aliquot of the sample is used. The proposed method was successfully applied to the determination of irinotecan in tap water, river water, and urine samples spiked with 10.20 mg/L for the water samples and 8.32 mg/L for the urine sample. The average recovery values of irinotecan determined were 99.1% for tap water, 109.4% for river water, and 96.1% for urine.

Pretreatment Solution for Water Recovery Systems

NASA Technical Reports Server (NTRS)

Muirhead, Dean (Inventor)

2018-01-01

Chemical pretreatments are used to produce usable water by treating a water source with a chemical pretreatment that contains a hexavalent chromium and an acid to generate a treated water source, wherein the concentration of sulfate compounds in the acid is negligible, and wherein the treated water source remains substantially free of precipitates after the addition of the chemical pretreatment. Other methods include reducing the pH in urine to be distilled for potable water extraction by pretreating the urine before distillation with a pretreatment solution comprising one or more acid sources selected from a group consisting of phosphoric acid, hydrochloric acid, and nitric acid, wherein the urine remains substantially precipitate free after the addition of the pretreatment solution. Another method described comprises a process for reducing precipitation in urine to be processed for water extraction by mixing the urine with a pretreatment solution comprising hexavalent chromium compound and phosphoric acid.

LC-MS determination of steroidal glycosides from Dioscorea deltoidea Wall cell suspension culture: Optimization of pre-LC-MS procedure parameters by Latin Square design.

PubMed

Sarvin, Boris; Fedorova, Elizaveta; Shpigun, Oleg; Titova, Maria; Nikitin, Mikhail; Kochkin, Dmitry; Rodin, Igor; Stavrianidi, Andrey

2018-03-30

In this paper, the ultrasound assisted extraction method for isolation of steroidal glycosides from D. deltoidea plant cell suspension culture with a subsequent HPLC-MS determination was developed. After the organic solvent was selected via a two-factor experiment the optimization via Latin Square 4 × 4 experimental design was carried out for the following parameters: extraction time, organic solvent concentration in extraction solution and the ratio of solvent to sample. It was also shown that the ultrasound assisted extraction method is not suitable for isolation of steroidal glycosides from the D. deltoidea plant material. The results were double-checked using the multiple successive extraction method and refluxing extraction. Optimal conditions for the extraction of steroidal glycosides by the ultrasound assisted extraction method were: extraction time, 60 min; acetonitrile (water) concentration in extraction solution, 50%; the ratio of solvent to sample, 400 mL/g. Also, the developed method was tested on D. deltoidea cell suspension cultures of different terms and conditions of cultivation. The completeness of the extraction was confirmed using the multiple successive extraction method. Copyright © 2018 Elsevier B.V. All rights reserved.

A sensitive analytical procedure for monitoring acrylamide in environmental water samples by offline SPE-UPLC/MS/MS.

PubMed

Togola, Anne; Coureau, Charlotte; Guezennec, Anne-Gwenaëlle; Touzé, Solène

2015-05-01

The presence of acrylamide in natural systems is of concern from both environmental and health points of view. We developed an accurate and robust analytical procedure (offline solid phase extraction combined with UPLC/MS/MS) with a limit of quantification (20 ng L(-1)) compatible with toxicity threshold values. The optimized (considering the nature of extraction phases, sampling volumes, and solvent of elution) solid phase extraction (SPE) was validated according to ISO Standard ISO/IEC 17025 on groundwater, surface water, and industrial process water samples. Acrylamide is highly polar, which induces a high variability during the SPE step, therefore requiring the use of C(13)-labeled acrylamide as an internal standard to guarantee the accuracy and robustness of the method (uncertainty about 25 % (k = 2) at limit of quantification level). The specificity of the method and the stability of acrylamide were studied for these environmental media, and it was shown that the method is suitable for measuring acrylamide in environmental studies.

Ultrasonic Removal of Mucilage for Pressurized Liquid Extraction of Omega-3 Rich Oil from Chia Seeds (Salvia hispanica L.).

PubMed

Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

2017-03-29

Chia (Salvia hispanica L.) seeds contain an important amount of edible oil rich in omega-3 fatty acids. Fast and alternative extraction techniques based on polar solvents, such as ethanol or water, have become relevant for oil extraction in recent years. However, chia seeds also contain a large amount of soluble fiber or mucilage, which makes difficult an oil extraction process with polar solvents. For that reason, the aim of this study was to develop a gentle extraction method for mucilage in order to extract chia oil with polar solvents using pressurized liquids and compare with organic solvent extraction. The proposed mucilage extraction method, using an ultrasonic probe and only water, was optimized at mild conditions (50 °C and sonication 3 min) to guarantee the omega-3 oil quality. Chia oil extraction was performed using pressurized liquid extraction (PLE) with different solvents and their mixtures at five different extraction temperatures (60, 90, 120, 150, and 200 °C). Optimal PLE conditions were achieved with ethyl acetate or hexane at 90 °C in only 10 min of static extraction time (chia oil yield up to 30.93%). In addition, chia oils extracted with nonpolar and polar solvents by PLE were analyzed by gas chromatography-mass spectrometry (GC-MS) to evaluate fatty acid composition at different extraction conditions. Chia oil contained ∼65% of α-linolenic acid regardless of mucilage extraction method, solvent, or temperature used. Furthermore, tocopherols and tocotrienols were also analyzed by HPLC in the extracted chia oils. The mucilage removal allowed the subsequent extraction of the chia oil with polar or nonpolar solvents by PLE producing chia oil with the same fatty acid and tocopherol composition as traditional extraction.

Automated solid-phase extraction of herbicides from water for gas chromatographic-mass spectrometric analysis

USGS Publications Warehouse

Meyer, M.T.; Mills, M.S.; Thurman, E.M.

1993-01-01

An automated solid-phase extraction (SPE) method was developed for the pre-concentration of chloroacetanilide and triazine herbicides, and two triazine metabolites from 100-ml water samples. Breakthrough experiments for the C18 SPE cartridge show that the two triazine metabolites are not fully retained and that increasing flow-rate decreases their retention. Standard curve r2 values of 0.998-1.000 for each compound were consistently obtained and a quantitation level of 0.05 ??g/l was achieved for each compound tested. More than 10,000 surface and ground water samples have been analyzed by this method.

Revealing the properties of oils from their dissolved hydrocarbon compounds in water with an integrated sensor array system.

PubMed

Qi, Xiubin; Crooke, Emma; Ross, Andrew; Bastow, Trevor P; Stalvies, Charlotte

2011-09-21

This paper presents a system and method developed to identify a source oil's characteristic properties by testing the oil's dissolved components in water. Through close examination of the oil dissolution process in water, we hypothesise that when oil is in contact with water, the resulting oil-water extract, a complex hydrocarbon mixture, carries the signature property information of the parent oil. If the dominating differences in compositions between such extracts of different oils can be identified, this information could guide the selection of various sensors, capable of capturing such chemical variations. When used as an array, such a sensor system can be used to determine parent oil information from the oil-water extract. To test this hypothesis, 22 oils' water extracts were prepared and selected dominant hydrocarbons analyzed with Gas Chromatography-Mass Spectrometry (GC-MS); the subsequent Principal Component Analysis (PCA) indicates that the major difference between the extract solutions is the relative concentration between the volatile mono-aromatics and fluorescent polyaromatics. An integrated sensor array system that is composed of 3 volatile hydrocarbon sensors and 2 polyaromatic hydrocarbon sensors was built accordingly to capture the major and subtle differences of these extracts. It was tested by exposure to a total of 110 water extract solutions diluted from the 22 extracts. The sensor response data collected from the testing were processed with two multivariate analysis tools to reveal information retained in the response patterns of the arrayed sensors: by conducting PCA, we were able to demonstrate the ability to qualitatively identify and distinguish different oil samples from their sensor array response patterns. When a supervised PCA, Linear Discriminate Analysis (LDA), was applied, even quantitative classification can be achieved: the multivariate model generated from the LDA achieved 89.7% of successful classification of the type of the oil samples. By grouping the samples based on the level of viscosity and density we were able to reveal the correlation between the oil extracts' sensor array responses and their original oils' feature properties. The equipment and method developed in this study have promising potential to be readily applied in field studies and marine surveys for oil exploration or oil spill monitoring.

Polydimethylsiloxane rod extraction, a novel technique for the determination of organic micropollutants in water samples by thermal desorption-capillary gas chromatography-mass spectrometry.

PubMed

Montero, L; Popp, P; Paschke, A; Pawliszyn, J

2004-01-30

A novel, simple and inexpensive approach to absorptive extraction of organic compounds from environmental samples is presented. It consists of a polydimethylsiloxane rod used as an extraction media, enriched with analytes during shaking, then thermally desorbed and analyzed by GC-MS. Its performance was illustrated and evaluated for the enrichment of sub- to ng/l of selected chlorinated compounds (chlorobenzenes and polychlorinated biphenyls) in water samples. The new approach was compared to the stir bar sorptive extraction performance. A natural ground water sample from Bitterfeld, Germany, was also extracted using both methods, showing good agreement. The proposed approach presented good linearity, high sensitivity, good blank levels and recoveries comparable to stir bars, together with advantages such as simplicity, lower cost and higher feasibility.

Comparison of different methods for isolation of bacterial DNA from retail oyster tissues

USDA-ARS?s Scientific Manuscript database

Oysters are filter-feeders that bio-accumulate bacteria in water while feeding. To evaluate the bacterial genomic DNA extracted from retail oyster tissues, including the gills and digestive glands, four isolation methods were used. Genomic DNA extraction was performed using the Allmag™ Blood Genomic...

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.

Magnetic sporopollenin-cyanopropyltriethoxysilane-dispersive micro-solid phase extraction coupled with high performance liquid chromatography for the determination of selected non-steroidal anti-inflammatory drugs in water samples.

PubMed

Abd Wahib, Siti Munirah; Wan Ibrahim, Wan Aini; Sanagi, Mohd Marsin; Kamboh, Muhammad Afzal; Abdul Keyon, Aemi S

2018-01-12

A facile dispersive-micro-solid phase extraction (D-μ-SPE) method coupled with HPLC for the analysis of selected non-steroidal anti-inflammatory drugs (NSAIDs) in water samples was developed using a newly prepared magnetic sporopollenin-cyanopropyltriethoxysilane (MS-CNPrTEOS) sorbent. Sporopollenin homogenous microparticles of Lycopodium clavatum spores possessed accessible functional groups that facilitated surface modification. Simple modification was performed by functionalization with 3-cyanopropyltriethoxysilane (CNPrTEOS) and magnetite was introduced onto the biopolymer to simplify the extraction process. MS-CNPrTEOS was identified by infrared spectrometrywhile the morphology and the magnetic property were confirmed by scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM), respectively. To maximize the extraction performance of ketoprofen, ibuprofen, diclofenac and mefenamic acid using the proposed MS-CNPrTEOS, important D-μ-SPE parameters were comprehensively optimized. The optimum extraction conditions were sorbent amount, 40 mg; extraction time, 5 min; desorption time; 5 min; sample volume, 15 mL; sample pH 2.0; and salt addition, 2.5% (w/v). The feasibility of the developed method was evaluated using spiked tap water, lake water, river water and waste water samples. Results showed that ketoprofen and ibuprofen were linear in the range of 1.0-1000 μg L -1 whilst diclofenac and mefenamic acid were linear in the range 0.8-500 μg L -1 . The results also showed good detection limits for the studied NSAIDs in the range of 0.21-0.51 μg L -1 and good recoveries for spiked water samples in the range of 85.1-106.4%. The MS-CNPrTEOS proved a promising dispersive sorbent and applicable to facile and rapid assay of NSAIDs in water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Acidified pressurized hot water for the continuous extraction of cadmium and lead from plant materials prior to ETAAS

NASA Astrophysics Data System (ADS)

Morales-Muñoz, S.; Luque-García, J. L.; Luque de Castro, M. D.

2003-01-01

Acidified and pressurized hot water is proposed for the continuous leaching of Cd and Pb from plants prior to determination by electrothermal atomic absorption spectrometry. Beech leaves (a certified reference material—CRM 100—where the analytes were not certified) were used for optimizing the method by a multivariate approach. The samples (0.5 g) were subjected to dynamic extraction with water modified with 1% v/v HNO 3 at 250 °C as leachant. A kinetics study was performed in order to know the pattern of the extraction process. The method was validated with a CRM (olive leaves, 062 from the BCR) where the analytes had been certified. The agreement between the certified values and those found using the proposed method demonstrates its usefulness. The repeatability and within-laboratory reproducibility were 3.7 and 2.3% for Cd and 1.04% and 6.3% for Pb, respectively. The precision of the method, together with its efficiency, rapidity, and environmental acceptability, makes it a good alternative for the determination of trace metals in plant material.

Determination of phthalate esters from environmental water samples by micro-solid-phase extraction using TiO2 nanotube arrays before high-performance liquid chromatography.

PubMed

Zhou, Qingxiang; Fang, Zhi; Liao, Xiangkun

2015-07-01

We describe a highly sensitive micro-solid-phase extraction method for the pre-concentration of six phthalate esters utilizing a TiO2 nanotube array coupled to high-performance liquid chromatography with a variable-wavelength ultraviolet visible detector. The selected phthalate esters included dimethyl phthalate, diethyl phthalate, dibutyl phthalate, butyl benzyl phthalate, bis(2-ethylhexyl)phthalate and dioctyl phthalate. The factors that would affect the enrichment, such as desorption solvent, sample pH, salting-out effect, extraction time and desorption time, were optimized. Under the optimum conditions, the linear range of the proposed method was 0.3-200 μg/L. The limits of detection were 0.04-0.2 μg/L (S/N = 3). The proposed method was successfully applied to the determination of six phthalate esters in water samples and satisfied spiked recoveries were achieved. These results indicated that the proposed method was appropriate for the determination of trace phthalate esters in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction process of palm kernel cake as a source of mannan for feed additive on poultry diet

NASA Astrophysics Data System (ADS)

Tafsin, M.; Hanafi, N. D.; Yusraini, E.

2017-05-01

Palm Kernel Cake (PKC) is a by-product of palm kernel oil extraction and found in large quantity in Indonesia. The inclusion of PKC on poultry diet are limited due to some nutritional problems such as anti-nutritional properties (mannan). On the other hand, mannan containing polysaccharides play in various biological functions particularly in enhancing the immune response and to control pathogen in poultry. The research objective to find out the extraction process of PKC and conducted at animal nutrition and Feed Science Laboratory, Agricultural Faculty, University of Sumatera Utara. Various extraction methode were used in this experiment, including fraction analysis used 7 number sieves, and followed by water and acetic acid extraction. The result indicated that PKC had different particle size according to sieve size and dominated by particle size 850 um. The analysis of sugar content indicated that each particle size had different characteristic on treatment by hot water extraction. The particle size 180—850 um had higher sugar content than coarse PKC (2000—3000 um). The total sugar content were recovered vary between 0.9—3,2% from PKC were extracted. Treatment grinding method followed by hot water extraction (100—120 °C, 1 h) increased total sugar content than previous treatments and reach 8% from PKC were extracted. Utilisation acetic acid decreased the total amount of total sugar from PKC were extracted. It is concluded that treatment by hot temperature (110—120 °C) for 1 h show highest yield to extract sugar from PKC.

ANALYSIS OF SWINE LAGOONS AND GROUND WATER FOR ENVIRONMENTAL ESTROGENS

EPA Science Inventory

A method was developed for analysis of low levels of natural (estradiol, estrone, estriol) and synthetic (ethynylestradiol) estrogens in ground water and swine waste lagoon effluent. The method includes solid phase extraction of the estrogens, preparation of pentafluorobenzyl der...

Technical aspects on production of fluid extract from Brosimum gaudichaudii Trécul roots

PubMed Central

Martins, Frederico Severino; Pascoa, Henrique; de Paula, José Realino; da Conceição, Edemilson Cardoso

2015-01-01

Instruction: Despite the increased use of Brosimum gaudichaudii roots as raw material on medicine to treatment of vitiligo, there are not studies that showing the impact of unit operations on the quality and standardized of the extract of B. gaudichaudii. The quality of the herbal extract is essential to ensure the safety and efficacy of pharmaceutical product. Due the medical and commercial importance, this study aimed to evaluate the impact of the extraction method (ultrasound or percolation) on the quality of herbal extract and optimize the extraction of psoralen and 8-methoxypsoralen (8-MOP) from B. gaudichaudii. Materials and Methods: The extraction recovery was evaluate by high-performance liquid chromatography (C8 reverse phase column and acetonitrile: Water 45:55 and flow rate 0.6 mL/min). The extraction was performed by ultrasound-assisted extraction (UEA) or percolation using a Box-Behnken design. Results: From both chemical markers (psoralen and bergapten), the optimal conditions for the UEA were an extraction time of 25 min, the mean particle size of 100 μm, and an ethanol: Water ratio of 55:45 (v/v). Conclusion: The extraction by percolation revealed that ethanol 55% was more efficient than ethanol 80% to extract psoralen and bergapten. PMID:25709236

Pseudophasic extraction method for the separation of ultra-fine minerals

DOEpatents

Chaiko, David J.

2002-01-01

An improved aqueous-based extraction method for the separation and recovery of ultra-fine mineral particles. The process operates within the pseudophase region of the conventional aqueous biphasic extraction system where a low-molecular-weight, water soluble polymer alone is used in combination with a salt and operates within the pseudo-biphase regime of the conventional aqueous biphasic extraction system. A combination of low molecular weight, mutually immiscible polymers are used with or without a salt. This method is especially suited for the purification of clays that are useful as rheological control agents and for the preparation of nanocomposites.

Extraction tools for identification of chemical contaminants in estuarine and coastal waters to determine toxic pressure on primary producers.

PubMed

Booij, Petra; Sjollema, Sascha B; Leonards, Pim E G; de Voogt, Pim; Stroomberg, Gerard J; Vethaak, A Dick; Lamoree, Marja H

2013-09-01

The extent to which chemical stressors affect primary producers in estuarine and coastal waters is largely unknown. However, given the large number of legacy pollutants and chemicals of emerging concern present in the environment, this is an important and relevant issue that requires further study. The purpose of our study was to extract and identify compounds which are inhibitors of photosystem II activity in microalgae from estuarine and coastal waters. Field sampling was conducted in the Western Scheldt estuary (Hansweert, The Netherlands). We compared four different commonly used extraction methods: passive sampling with silicone rubber sheets, polar organic integrative samplers (POCIS) and spot water sampling using two different solid phase extraction (SPE) cartridges. Toxic effects of extracts prepared from spot water samples and passive samplers were determined in the Pulse Amplitude Modulation (PAM) fluorometry bioassay. With target chemical analysis using LC-MS and GC-MS, a set of PAHs, PCBs and pesticides was determined in field samples. These compound classes are listed as priority substances for the marine environment by the OSPAR convention. In addition, recovery experiments with both SPE cartridges were performed to evaluate the extraction suitability of these methods. Passive sampling using silicone rubber sheets and POCIS can be applied to determine compounds with different structures and polarities for further identification and determination of toxic pressure on primary producers. The added value of SPE lies in its suitability for quantitative analysis; calibration of passive samplers still needs further investigation for quantification of field concentrations of contaminants. Copyright © 2013 Elsevier Ltd. All rights reserved.

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.

Model-Based Extracted Water Desalination System for Carbon Sequestration

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

Dees, Elizabeth M.; Moore, David Roger; Li, Li

Over the last 1.5 years, GE Global Research and Pennsylvania State University defined a model-based, scalable, and multi-stage extracted water desalination system that yields clean water, concentrated brine, and, optionally, salt. The team explored saline brines that ranged across the expected range for extracted water for carbon sequestration reservoirs (40,000 up to 220,000 ppm total dissolved solids, TDS). In addition, the validated the system performance at pilot scale with field-sourced water using GE’s pre-pilot and lab facilities. This project encompassed four principal tasks, in addition to Project Management and Planning: 1) identify a deep saline formation carbon sequestration site andmore » a partner that are suitable for supplying extracted water; 2) conduct a techno-economic assessment and down-selection of pre-treatment and desalination technologies to identify a cost-effective system for extracted water recovery; 3) validate the downselected processes at the lab/pre-pilot scale; and 4) define the scope of the pilot desalination project. Highlights from each task are described below: Deep saline formation characterization The deep saline formations associated with the five DOE NETL 1260 Phase 1 projects were characterized with respect to their mineralogy and formation water composition. Sources of high TDS feed water other than extracted water were explored for high TDS desalination applications, including unconventional oil and gas and seawater reverse osmosis concentrate. Technoeconomic analysis of desalination technologies Techno-economic evaluations of alternate brine concentration technologies, including humidification-dehumidification (HDH), membrane distillation (MD), forward osmosis (FO), turboexpander-freeze, solvent extraction and high pressure reverse osmosis (HPRO), were conducted. These technologies were evaluated against conventional falling film-mechanical vapor recompression (FF-MVR) as a baseline desalination process. Furthermore, a quality function deployment (QFD) method was used to compare alternate high TDS desalination technologies to FF-MVR. High pressure reverse osmosis was found to a be a promising alternative desalination technology. A deep-dive technoeconomic analysis of HPRO was performed, including Capex and Opex estimates, for seawater RO (SWRO). Additionally, two additional cases were explored: 1) a comparison of a SWRO plus HPRO system to the option of doubling the size of a standard seawater RO system to achieve the same total pure water recovery rate; and 2) a flue gas desulfurization wastewater treatment zero-liquid discharge (ZLD) application, where preconcentration with RO (SWRO or SWRO + HPRO) before evaporation and crystallization was compared to FF-MVR and crystallization technologies without RO preconcentration. Pre-pilot process validation Pre-pilot-scale tests were conducted using field production water to validate key process steps for extracted water pretreatment. Approximately 5,000 gallons of field produced water was processed through, microfiltration, ultrafiltration, and steam regenerable sorbent operations. Smaller quantities were processed through microclarification. In addition, analytical methods (purge-and-trap gas chromatography and Hach TOC analytical methods) were validated. Lab-scale HPRO elements were constructed and tested at high pressures, to identify and mitigate technical risks of the technology. Lastly, improvements in RO membrane materials were identified as the necessary next step to achieve further improvement in element performance at high pressure. Scope of Field Pilot A field pilot for extracted water pretreatment was designed.« less

Composite Magnetic Nanoparticles (CuFe₂O₄) as a New Microsorbent for Extraction of Rhodamine B from Water Samples.

PubMed

Roostaie, Ali; Allahnoori, Farzad; Ehteshami, Shokooh

2017-09-01

In this work, novel composite magnetic nanoparticles (CuFe2O4) were synthesized based on sol-gel combustion in the laboratory. Next, a simple production method was optimized for the preparation of the copper nanoferrites (CuFe2O4), which are stable in water, magnetically active, and have a high specific area used as sorbent material for organic dye extraction in water solution. CuFe2O4 nanopowders were characterized by field-emission scanning electron microscopy (SEM), FTIR spectroscopy, and energy dispersive X-ray spectroscopy. The size range of the nanoparticles obtained in such conditions was estimated by SEM images to be 35-45 nm. The parameters influencing the extraction of CuFe2O4 nanoparticles, such as desorption solvent, amount of sorbent, desorption time, sample pH, ionic strength, and extraction time, were investigated and optimized. Under the optimum conditions, a linear calibration curve in the range of 0.75-5.00 μg/L with R2 = 0.9996 was obtained. The LOQ (10Sb) and LOD (3Sb) of the method were 0.75 and 0.25 μg/L (n = 3), respectively. The RSD for a water sample spiked with 1 μg/L rhodamine B was 3% (n = 5). The method was applied for the determination of rhodamine B in tap water, dishwashing foam, dishwashing liquid, and shampoo samples. The relative recovery percentages for these samples were in the range of 95-99%.

A robust Multi-Band Water Index (MBWI) for automated extraction of surface water from Landsat 8 OLI imagery

NASA Astrophysics Data System (ADS)

Wang, Xiaobiao; Xie, Shunping; Zhang, Xueliang; Chen, Cheng; Guo, Hao; Du, Jinkang; Duan, Zheng

2018-06-01

Surface water is vital resources for terrestrial life, while the rapid development of urbanization results in diverse changes in sizes, amounts, and quality of surface water. To accurately extract surface water from remote sensing imagery is very important for water environment conservations and water resource management. In this study, a new Multi-Band Water Index (MBWI) for Landsat 8 Operational Land Imager (OLI) images is proposed by maximizing the spectral difference between water and non-water surfaces using pure pixels. Based on the MBWI map, the K-means cluster method is applied to automatically extract surface water. The performance of MBWI is validated and compared with six widely used water indices in 29 sites of China. Results show that our proposed MBWI performs best with the highest accuracy in 26 out of the 29 test sites. Compared with other water indices, the MBWI results in lower mean water total errors by a range of 9.31%-25.99%, and higher mean overall accuracies and kappa coefficients by 0.87%-3.73% and 0.06-0.18, respectively. It is also demonstrated for MBWI in terms of robustly discriminating surface water from confused backgrounds that are usually sources of surface water extraction errors, e.g., mountainous shadows and dark built-up areas. In addition, the new index is validated to be able to mitigate the seasonal and daily influences resulting from the variations of the solar condition. MBWI holds the potential to be a useful surface water extraction technology for water resource studies and applications.

Water quality real-time monitoring system via biological detection based on video analysis

NASA Astrophysics Data System (ADS)

Xin, Chen; Fei, Yuan

2017-11-01

With the development of society, water pollution has become the most serious problem in China. Therefore, real-time water quality monitoring is an important part of human activities and water pollution prevention. In this paper, the behavior of zebrafish was monitored by computer vision. Firstly, the moving target was extracted by the method of saliency detection, and tracked by fitting the ellipse model. Then the motion parameters were extracted by optical flow method, and the data were monitored in real time by means of Hinkley warning and threshold warning. We achieved classification warning through a number of dimensions by comprehensive toxicity index. The experimental results show that the system can achieve more accurate real-time monitoring.

Graphene oxide/Fe3O4 as sorbent for magnetic solid-phase extraction coupled with liquid chromatography to determine 2,4,6-trinitrotoluene in water samples.

PubMed

Costa Dos Reis, Luciana; Vidal, Lorena; Canals, Antonio

2017-04-01

A fast, simple, economical, and environmentally friendly magnetic solid-phase extraction (MSPE) procedure has been developed to preconcentrate 2,4,6-trinitrotoluene (TNT) from water samples prior to determination by liquid chromatography-UV-Vis employing graphene oxide/Fe 3 O 4 nanocomposite as sorbent. The nanocomposite synthesis was investigated, and the MSPE was optimized by a multivariate approach. The optimum MSPE conditions were 40 mg of nanocomposite, 10 min of vortex extraction, 1 mL of acetonitrile as eluent, and 6 min of desorption in an ultrasonic bath. Under the optimized experimental conditions, the method was evaluated to obtain a preconcentration factor of 153. The linearity of the method was studied from 1 to 100 μg L -1 (N = 5), obtaining a correlation coefficient of 0.994. The relative standard deviation and limit of detection were found to be 12% (n = 6, 10 μg L -1 ) and 0.3 μg L -1 , respectively. The applicability of the method was investigated, analyzing three types of water samples (i.e., reservoir and drinking water and effluent wastewater) and recovery values ranged between 87 and 120% (50 μg L -1 spiking level), showing that the matrix had a negligible effect upon extraction. Finally, the semiquantitative Eco-Scale metrics confirmed the greenness of the developed method.

Evaluation of δ2H and δ18O of water in pores extracted by compression method-effects of closed pores and comparison to direct vapor equilibration and laser spectrometry method

NASA Astrophysics Data System (ADS)

Nakata, Kotaro; Hasegawa, Takuma; Oyama, Takahiro; Miyakawa, Kazuya

2018-06-01

Stable isotopes (δ2H and δ18O) of water can help our understanding of origin, mixing and migration of groundwater. In the formation with low permeability, it provides information about migration mechanism of ion such as diffusion and/or advection. Thus it has been realized as very important information to understand the migration of water and ions in it. However, in formation with low permeability it is difficult to obtain the ground water sample as liquid and water in pores needs to be extracted to estimate it. Compressing rock is the most common and widely used method of extracting water in pores. However, changes in δ2H and δ18O may take place during compression because changes in ion concentration have been reported in previous studies. In this study, two natural rocks were compressed, and the changes in the δ2H and δ18O with compression pressure were investigated. Mechanisms for the changes in water isotopes observed during the compression were then discussed. In addition, δ2H and δ18O of water in pores were also evaluated by direct vapor equilibration and laser spectrometry (DVE-LS) and δ2H and δ18O were compared with those obtained by compression. δ2H was found to change during the compression and a part of this change was found to be explained by the effect of water from closed pores extracted by compression. In addition, water isotopes in both open and closed pores were estimated by combining the results of 2 kinds of compression experiments. Water isotopes evaluated by compression that not be affected by water from closed pores showed good agreements with those obtained by DVE-LS indicating compression could show the mixed information of water from open and closed pores, while DVE-LS could show the information only for open pores. Thus, the comparison of water isotopes obtained by compression and DVE-LS could provide the information about water isotopes in closed and open pores.

Determination of trace mercury in water based on N-octylpyridinium ionic liquids preconcentration and stripping voltammetry.

PubMed

Li, Zhenhan; Xia, Shanhong; Wang, Jinfen; Bian, Chao; Tong, Jianhua

2016-01-15

A novel method for determination of trace mercury in water is developed. The method is performed by extracting mercury firstly with ionic liquids (ILs) and then detecting the concentration of mercury in organic media with anodic stripping voltammetry. Liquid-liquid extraction of mercury(II) ions by four ionic liquids with N-octylpyridinium cations ([OPy](+)) was studied. N-octylpyridinium tetrafluoroborate and N-octylpyridinium trifluoromethylsulfonate were found to be efficient and selective extractant for mercury. Temperature controlled dispersive liquid phase microextraction (TC-DLPME) technique was utilized to improve the performance of preconcentration. After extraction, precipitated IL was diluted by acetonitrile buffer and mercury was detected by differential pulse stripping voltammetry (DPSV) with gold disc electrode. Mercury was enriched by 17 times while interfering ions were reduced by two orders of magnitude in the organic media under optimum condition. Sensitivity and selectivity for electrochemical determination of mercury were improved by using the proposed method. Tap, pond and waste water samples were analyzed with recoveries ranging from 81% to 107% and detection limit of 0.05 μg/L. Copyright © 2015 Elsevier B.V. All rights reserved.

Evaluation of graphene-based sorbent in the determination of polar environmental contaminants in water by micro-solid phase extraction-high performance liquid chromatography.

PubMed

Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

2016-01-04

A facile method of extraction using porous membrane protected micro-solid phase extraction (μ-SPE) with a graphene-based sorbent followed by high performance liquid chromatography-ultraviolet detector was developed. The reduced graphene oxide (r-GO) (1mg), synthesized from graphite oxide, was enclosed in a polypropylene bag representing the μ-SPE device, which was used for the extraction of estrogens such as estrone, 17β-estradiol, 17α-ethynylestradiol and diethylstilbestrol in water. The r-GO obtained was identified and characterized by Fourier transform infrared, transmission electron microscopy, scanning electron microscopy and thermogravimetric analysis. The sorbent was loaded with sodium dodecyl sulfate by sonication to prevent agglomeration in aqueous solution. With this method, low limits of detection of between 0.24 and 0.52 ng L(-1) were achieved. For estrogen analysis a linear calibration range of 0.01-100 μg L(-1) was obtained, with the coefficients of determination (r(2)) higher than 0.992. This proposed method was successfully applied to determine estrogens in water. Copyright © 2015 Elsevier B.V. All rights reserved.

Cytotoxicity of different extracts of arial parts of Ziziphus spina-christi on Hela and MDA-MB-468 tumor cells

PubMed Central

Jafarian, Abbas; Zolfaghari, Behzad; Shirani, Kobra

2014-01-01

Background: It has been shown that plants from the family Rhamnaceae possess anticancer activity. In this study, we sought to determine if Ziziphus spina-christi, a species from this family, has cytotoxic effect on cancer cell lines. Materials and Methods: Using maceration method, different extracts of leaves of Z. spina-christi were prepared. Hexane, chloroform, chloroform-methanol (9:1), methanol-water (7:1) methanol, butanol and water were used for extraction, after preliminary phytochemical analyses were done. The cytotoxic activity of the extracts against Hela and MDA-MB-468 tumor cells was evaluated by MTT assay. Briefly, cells were seeded in microplates and different concentrations of extracts were added. After incubation of cells for 72 h, their viability was evaluated by addition of tetrazolium salt solution. After 3 h medium was aspirated, dimethyl sulfoxide was added and absorbance was determined at 540 nm with an ELISA plate reader. Extracts were considered cytotoxic when more than 50% reduction on cell survival was observed. Results: Hexane, chloroform, chloroform-methanol, butanol, methanol-water and aqueous extracts of Z. spina-christi significantly and concentration-dependently reduced viability of Hela and MAD-MB-468 cells. In the both cell lines, chloroform-methanol extract of Z. spina-christi was more potent than the other extracts. Results: From the finding of this study it can be concluded that Z. spina-christi is a good candidate for further study for new cytotoxic agents. PMID:24627846

Comparison of salting-out and sugaring-out liquid-liquid extraction methods for the partition of 10-hydroxy-2-decenoic acid in royal jelly and their co-extracted protein content.

PubMed

Tu, Xijuan; Sun, Fanyi; Wu, Siyuan; Liu, Weiyi; Gao, Zhaosheng; Huang, Shaokang; Chen, Wenbin

2018-01-15

Homogeneous liquid-liquid extraction (h-LLE) has been receiving considerable attention as a sample preparation method due to its simple and fast partition of compounds with a wide range of polarities. To better understand the differences between the two h-LLE extraction approaches, salting-out assisted liquid-liquid extraction (SALLE) and sugaring-out assisted liquid-liquid extraction (SULLE), have been compared for the partition of 10-hydroxy-2-decenoic acid (10-HDA) from royal jelly, and for the co-extraction of proteins. Effects of the amount of phase partition agents and the concentration of acetonitrile (ACN) on the h-LLE were discussed. Results showed that partition efficiency of 10-HDA depends on the phase ratio in both SALLE and SULLE. Though the partition triggered by NaCl and glucose is less efficient than MgSO 4 in the 50% (v/v) ACN-water mixture, their extraction yields can be improved to be similar with that in MgSO 4 SALLE by increasing the initial concentration of ACN in the ACN-water mixture. The content of co-extracted protein was correlated with water concentration in the obtained upper phase. MgSO 4 showed the largest protein co-extraction at the low concentration of salt. Glucose exhibited a large protein co-extraction in the high phase ratio condition. Furthermore, NaCl with high initial ACN concentration is recommended because it produced high extraction yield for 10-HDA and the lowest amount of co-extracted protein. These observations would be valuable for the sample preparation of royal jelly. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of perfluorinated chemicals in food and drinking water using high-flow solid-phase extraction and ultra-high performance liquid chromatography/tandem mass spectrometry.

PubMed

Chang, Ying-Chia; Chen, Wen-Ling; Bai, Fang-Yu; Chen, Pau-Chung; Wang, Gen-Shuh; Chen, Chia-Yang

2012-01-01

For this study, we developed methods of determining ten perfluorinated chemicals in drinking water, milk, fish, beef, and pig liver using high-flow automated solid-phase extraction (SPE) and ultra-high performance liquid chromatography/tandem mass spectrometry. The analytes were separated on a core-shell Kinetex C18 column. The mobile phase was composed of methanol and 10-mM N-methylmorpholine. Milk was digested with 0.5 N potassium hydroxide in Milli-Q water, and was extracted with an Atlantic HLB disk to perform automated SPE at a flow rate ranged from 70 to 86 mL/min. Drinking water was directly extracted by the SPE. Solid food samples were digested in alkaline methanol and their supernatants were diluted and also processed by SPE. The disks were washed with 40% methanol/60% water and then eluted with 0.1% ammonium hydroxide in methanol. Suppression of signal intensity of most analytes by matrixes was lower than 50%; it was generally lower in fish and drinking water but higher in liver. Most quantitative biases and relative standard deviations were lower than 15%. The limits of detection for most analytes were sub-nanograms per liter for drinking water and sub-nanograms per gram for solid food samples. This method greatly shortened the time and labor needed for digestion, SPE, and liquid chromatography. This method has been applied to analyze 14 types of food samples. Perfluorooctanoic acid was found to be the highest among the analytes (median at 3.2-64 ng/g wet weight), followed by perfluorodecanoic acid (0.7-25 ng/g) and perfluorododecanoic acid (0.6-15 ng/g).

Zeolite/iron oxide composite as sorbent for magnetic solid-phase extraction of benzene, toluene, ethylbenzene and xylenes from water samples prior to gas chromatography⬜mass spectrometry.

PubMed

Fernández, Elena; Vidal, Lorena; Canals, Antonio

2016-08-05

This study reports a new composite based on ZSM-5 zeolite decorated with iron oxide magnetic nanoparticles as a valuable sorbent for magnetic solid-phase extraction (MSPE). A proposal is made to determine benzene, toluene, ethylbenzene and xylenes (BTEX) as model analytes in water samples using gas chromatography-mass spectrometry. A two-step multivariate optimization strategy, using Plackett⬜Burman and circumscribed central composite designs, was employed to optimize experimental parameters affecting MSPE. The method was evaluated under optimized extraction conditions (i.e., amount of sorbent, 138mg; extraction time, 11min; sample pH, pH of water (i.e., 5.5⬜6.5); eluent solvent volume, 0.5mL; and elution time, 5min), obtaining a linear response from 1 to 100μgL(↙1) for benzene; from 10 to 100μgL(↙1) for toluene, ethylbenzene and o-xylene; and from 10 to 75μgL(↙1) for m,p-xylene. The repeatability of the proposed method was evaluated at a 40μgL(↙1) spiking level and coefficients of variation ranged between 8 and 11% (n=5). Limits of detection were found to be 0.3μgL(↙1) for benzene and 3μgL(↙1) for the other analytes. These values satisfy the current normative of the Environmental Protection Agency and European Union for BTEX content in waters for human consumption. Finally, drinking water, wastewater and river water were selected as real water samples to assess the applicability of the method. Relative recoveries varied between 85% and 114% showing negligible matrix effects. Copyright © 2016 Elsevier B.V. All rights reserved.

Method 522 - Determination of 1,4-Dioxane in Drinking Water by Solid Phase Extraction (SPE) and Gas Chromatography Mass Spectrometry (GC/MS) with Selected Ion Monitoring (SIM)

EPA Science Inventory

1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of...

Use of magnetic effervescent tablet-assisted ionic liquid dispersive liquid-liquid microextraction to extract fungicides from environmental waters with the aid of experimental design methodology.

PubMed

Yang, Miyi; Wu, Xiaoling; Jia, Yuhan; Xi, Xuefei; Yang, Xiaoling; Lu, Runhua; Zhang, Sanbing; Gao, Haixiang; Zhou, Wenfeng

2016-02-04

In this work, a novel effervescence-assisted microextraction technique was proposed for the detection of four fungicides. This method combines ionic liquid-based dispersive liquid-liquid microextraction with the magnetic retrieval of the extractant. A magnetic effervescent tablet composed of Fe3O4 magnetic nanoparticles, sodium carbonate, sodium dihydrogen phosphate and 1-hexyl-3-methylimidazolium bis(trifluoromethanesulfonimide) was used for extractant dispersion and retrieval. The main factors affecting the extraction efficiency were screened by a Plackett-Burman design and optimized by a central composite design. Under the optimum conditions, good linearity was obtained for all analytes in pure water model and real water samples. Just for the pure water, the recoveries were between 84.6% and 112.8%, the limits of detection were between 0.02 and 0.10 μg L(-1) and the intra-day precision and inter-day precision both are lower than 4.9%. This optimized method was successfully applied in the analysis of four fungicides (azoxystrobin, triazolone, cyprodinil, trifloxystrobin) in environmental water samples and the recoveries ranged between 70.7% and 105%. The procedure promising to be a time-saving, environmentally friendly, and efficient field sampling technique. Copyright © 2015 Elsevier B.V. All rights reserved.

Chapter 3. Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spectrometry

USGS Publications Warehouse

Zaugg, Steven D.; Burkhardt, Mark R.; Burbank, Teresa L.; Olson, Mary C.; Iverson, Jana L.; Schroeder, Michael P.

2006-01-01

A method for the determination of 38 polycyclic aromatic hydrocarbons (PAHs) and semivolatile organic compounds in solid samples is described. Samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from the solid sample twice at 13,800 kilopascals; first at 120 degrees Celsius using a water/isopropyl alcohol mixture (50:50, volume-to-volume ratio), and then the sample is extracted at 200 degrees Celsius using a water/isopropyl alcohol mixture (80:20, volume-to-volume ratio). The compounds are isolated using disposable solid-phase extraction (SPE) cartridges containing divinylbenzene-vinylpyrrolidone copolymer resin. The cartridges are dried with nitrogen gas, and then sorbed compounds are eluted from the SPE material using a dichloromethane/diethyl ether mixture (80:20, volume-to-volume ratio) and passed through a sodium sulfate/Florisil SPE cartridge to remove residual water and to further clean up the extract. The concentrated extract is solvent exchanged into ethyl acetate and the solvent volume reduced to 0.5 milliliter. Internal standard compounds are added prior to analysis by capillary-column gas chromatography/mass spectrometry. Comparisons of PAH data for 28 sediment samples extracted by Soxhlet and the accelerated solvent extraction (ASE) method described in this report produced similar results. Extraction of PAH compounds from standard reference material using this method also compared favorably with Soxhlet extraction. The recoveries of PAHs less than molecular weight 202 (pyrene or fluoranthene) are higher by up to 20 percent using this ASE method, whereas the recoveries of PAHs greater than or equal to molecular weight 202 are equivalent. This ASE method of sample extraction of solids has advantages over conventional Soxhlet extraction by increasing automation of the extraction process, reducing extraction time, and using less solvent. Extract cleanup also is greatly simplified because SPE replaces commonly used gel permeation chromatography. The performance of the method (as expressed by mean recoveries and mean precision) was determined using Ottawa sand, a commercially available topsoil, and an environmental stream sediment, fortified at 1.5 and 15 micrograms per compound. Recoveries of PAH and semivolatile compounds in Ottawa sand samples fortified at 1.5 micrograms averaged 88 percent ? 9.4 percent relative standard deviation, and calculated initial method detection limits per compound averaged 14 micrograms per kilogram, assuming a 25-gram sample size. The recovery for 1,2,4-trichlorobenzene is less than 60 percent; thus, the concentration of this compound will always be reported as estimated with the E remark code. The analysis of 25 alkylated PAH homolog groups also can be determined with this method with extra data analysis and review, but because of the lack of authentic reference standard compounds, these results are considered to be semiquantitative. The PAH homolog groups are quantitated using the response factor of a parent PAH method compound, if available. Precision data for the alkylated PAH homologs detected in a marine sediment standard reference material (SRM 1944) also are presented to document and demonstrate method capability.

Comparison of Enzymatic and Ultrasonic Extraction of Albumin from Defatted Pumpkin (Cucurbita pepo)
Seed Powder

PubMed Central

Tu, Gia Loi; Bui, Thi Hoang Nga; Tran, Thi Thu Tra; Ton, Nu Minh Nguyet

2015-01-01

Summary In this study, ultrasound- and enzyme-assisted extractions of albumin (water-soluble protein group) from defatted pumpkin (Cucurbita pepo) seed powder were compared. Both advanced extraction techniques strongly increased the albumin yield in comparison with conventional extraction. The extraction rate was two times faster in the ultrasonic extraction than in the enzymatic extraction. However, the maximum albumin yield was 16% higher when using enzymatic extraction. Functional properties of the pumpkin seed albumin concentrates obtained using the enzymatic, ultrasonic and conventional methods were then evaluated. Use of hydrolase for degradation of cell wall of the plant material did not change the functional properties of the albumin concentrate in comparison with the conventional extraction. The ultrasonic extraction enhanced water-holding, oil-holding and emulsifying capacities of the pumpkin seed albumin concentrate, but slightly reduced the foaming capacity, and emulsion and foam stability. PMID:27904383

Comparison of Enzymatic and Ultrasonic Extraction of Albumin from Defatted Pumpkin (Cucurbita pepo)
Seed Powder.

PubMed

Tu, Gia Loi; Bui, Thi Hoang Nga; Tran, Thi Thu Tra; Ton, Nu Minh Nguyet; Man Le, Van Viet

2015-12-01

In this study, ultrasound- and enzyme-assisted extractions of albumin (water-soluble protein group) from defatted pumpkin ( Cucurbita pepo ) seed powder were compared. Both advanced extraction techniques strongly increased the albumin yield in comparison with conventional extraction. The extraction rate was two times faster in the ultrasonic extraction than in the enzymatic extraction. However, the maximum albumin yield was 16% higher when using enzymatic extraction. Functional properties of the pumpkin seed albumin concentrates obtained using the enzymatic, ultrasonic and conventional methods were then evaluated. Use of hydrolase for degradation of cell wall of the plant material did not change the functional properties of the albumin concentrate in comparison with the conventional extraction. The ultrasonic extraction enhanced water-holding, oil-holding and emulsifying capacities of the pumpkin seed albumin concentrate, but slightly reduced the foaming capacity, and emulsion and foam stability.

Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

PubMed

Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

2016-02-01

A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

Antioxidant Effect of Extracts from the Coffee Residue in Raw and Cooked Meat

PubMed Central

Kim, Ji-Hee; Ahn, Dong Uk; Eun, Jong Bang; Moon, Sun Hee

2016-01-01

The residue of ground coffee obtained after the brewing process (spent coffee) still contains various functional components with high antioxidant capacity and health benefits, but no attempts have been made to use it as a resource to produce value-added food ingredients. This study evaluates the antioxidant activity of ethanol or hot water extracts from the residues of coffee after brewing. An extraction experiment was carried out using the conventional solid–liquid methods, including ethanol and water as the extraction media at different temperatures and liquid/solid ratios. The antioxidant activity of extracts was tested for total phenolic compound (TPC), 2,2-diphenyl-1-picrylhydrazyl (DPPH), and 2-thiobarbituric acid reactive substances (TBARS) using oil emulsion and raw/cooked meat systems. The DPPH radical scavenging activity of the ethanol extracts with heating (HEE) and without heating (CEE) were higher than that of the hot water extracts (WE). The highest DPPH value of HEE and CEE at 1000 ppm was 91.22% and 90.21%, respectively. In oil emulsion and raw/cooked systems, both the water and ethanol extracts had similar antioxidant effects to the positive control (BHA), but HEE and CEE extracts showed stronger antioxidant activities than WE extract. These results indicated that the ethanol extracts of coffee residue have a strong antioxidant activity and have the potential to be used as a natural antioxidant in meat. PMID:27384587

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.

Plant Growth Biostimulants Based on Different Methods of Seaweed Extraction with Water.

PubMed

Godlewska, Katarzyna; Michalak, Izabela; Tuhy, Łukasz; Chojnacka, Katarzyna

2016-01-01

We explored two methods for obtaining aqueous extracts: boiling and soaking of Baltic seaweeds (EB and ES, resp.). Algal extracts were characterized in terms of polyphenols, micro- and macroelements, lipids content, and antibacterial properties. The utilitarian properties were examined in the germination tests on Lepidium sativum for three extract dilutions (0.5, 2.5, and 10%). It was found that the extracts were similar in micro- and macroelement concentrations. Water was proved to be a good solvent to extract phenolic compounds. The algal extract produced by soaking biomass did not show inhibitory effect on Escherichia coli and Staphylococcus aureus. Only the boiled extract had an inhibitory activity against E. coli. Germination tests revealed a positive influence of the bioproducts on the cultivated plants. In the group treated with 10% EB, plants were 13% longer than in the control group; the content of elements B, Mo, Zn, and Na in the group treated with 10% ES was higher by 76%, 48%, 31%, and 59% than in the control group, respectively; the content of chlorophyll was 2.5 times higher in 0.5% ES than in the control group. Extracts showed the slight impact on the morphology of plants.

Plant Growth Biostimulants Based on Different Methods of Seaweed Extraction with Water

PubMed Central

Godlewska, Katarzyna; Tuhy, Łukasz; Chojnacka, Katarzyna

2016-01-01

We explored two methods for obtaining aqueous extracts: boiling and soaking of Baltic seaweeds (EB and ES, resp.). Algal extracts were characterized in terms of polyphenols, micro- and macroelements, lipids content, and antibacterial properties. The utilitarian properties were examined in the germination tests on Lepidium sativum for three extract dilutions (0.5, 2.5, and 10%). It was found that the extracts were similar in micro- and macroelement concentrations. Water was proved to be a good solvent to extract phenolic compounds. The algal extract produced by soaking biomass did not show inhibitory effect on Escherichia coli and Staphylococcus aureus. Only the boiled extract had an inhibitory activity against E. coli. Germination tests revealed a positive influence of the bioproducts on the cultivated plants. In the group treated with 10% EB, plants were 13% longer than in the control group; the content of elements B, Mo, Zn, and Na in the group treated with 10% ES was higher by 76%, 48%, 31%, and 59% than in the control group, respectively; the content of chlorophyll was 2.5 times higher in 0.5% ES than in the control group. Extracts showed the slight impact on the morphology of plants. PMID:27366749

Hollow fiber supported ionic liquid membrane microextraction for determination of sulfonamides in environmental water samples by high-performance liquid chromatography.

PubMed

Tao, Yong; Liu, Jing-Fu; Hu, Xia-Lin; Li, Hong-Cheng; Wang, Thanh; Jiang, Gui-Bin

2009-08-28

By using ionic liquid as membrane liquid and tri-n-octylphosphine oxide (TOPO) as additive, hollow fiber supported liquid phase microextraction (HF-LPME) was developed for the determination of five sulfonamides in environmental water samples by high-performance liquid chromatography with ultraviolet detection The extraction solvent and the parameters affecting the extraction enrichment factor such as the type and amount of carrier, pH and volume ratio of donor phase and acceptor phase, extraction time, salt-out effect and matrix effect were optimized. Under the optimal extraction conditions (organic liquid membrane phase: [C(8)MIM][PF(6)] with 14% TOPO (w/v); donor phase: 4mL, pH 4.5 KH(2)PO(4) with 2M Na(2)SO(4); acceptor phase: 25microL, pH 13 NaOH; extraction time: 8 h), low detection limits (0.1-0.4microg/L, RSDor=0.999) were obtained for all the analytes. The presence of humic acid (0-25mg/L dissolved organic carbon) and bovine serum albumin (0-100microg/mL) had no significant effect on the extraction efficiency. Good spike recoveries over the range of 82.2-103.2% were obtained when applying the proposed method on five real environmental water samples. These results indicated that this present method was very sensitive and reliable with good repeatabilities and excellent clean-up in water samples. The proposed method confirmed hollow fiber supported ionic liquid membrane based LPME to be robust to monitoring trace levels of sulfadiazine, sulfamerazine, sulfamethazine, sulfadimethoxine and sulfamethoxazole in aqueous samples.

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).

Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

PubMed

Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

2016-01-15

A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Recovery of Palm Oil and Valuable Material from Oil Palm Empty Fruit Bunch by Sub-critical Water.

PubMed

Ahmad Kurnin, Nor Azrin; Shah Ismail, Mohd Halim; Yoshida, Hiroyuki; Izhar, Shamsul

2016-01-01

Oil palm empty fruit bunch (EFB) is one of the solid wastes produced in huge volume by palm oil mill. Whilst it still contains valuable oil, approximately 22.6 million tons is generated annually and treated as solid waste. In this work, sub-critical water (sub-cw) was used to extract oil, sugar and tar from spikelet of EFB. The spikelet was treated with sub-cw between 180-280°C and a reaction time of 2 and 5 minutes. The highest yield of oil was 0.075 g-oil/g-dry EFB, obtained at 240°C and reaction time of 5 minutes. Astonishingly, oil that was extracted through this method was 84.5% of that obtained through Soxhlet method using hexane. Yield of oil extracted was strongly affected by the reaction temperature and time. Higher reaction temperature induces the dielectric constant of water towards the non-polar properties of solvent; thus increases the oil extraction capability. Meanwhile, the highest yield of sugar was 0.20 g-sugar/g-dry EFB obtained at 220°C. At this temperature, the ion product of water is high enough to enable maximum sub-critical water hydrolysis reaction. This study showed that oil and other valuable material can be recovered using water at sub-critical condition, and most attractive without the use of harmful organic solvent.

Ultrasound-assisted emulsification microextraction combined with injection-port derivatization for the determination of some chlorophenoxyacetic acids in water samples.

PubMed

Yamini, Yadollah; Saleh, Abolfazl

2013-07-01

An efficient method based on ultrasound-assisted emulsification microextraction followed by injection-port derivatization GC analysis was developed to determine 2,4-dichlorophenoxyacetic acid (2,4-D) and 4-chloro-2-methylphenoxyacetic acid (MCPA) in natural water samples. In this procedure, 12.5 μL of 1-undecanol was injected slowly into a 12 mL home-designed centrifuge glass vial containing an aqueous sample of the analytes located inside an ultrasonic water bath. The resulting emulsion was centrifuged, and 1 μL of the separated organic solvent together with 1 μL of the derivatization reagent were injected into a GC equipped with a flame ionization detector. Several factors that influence the derivatization and extraction were optimized. Under the optimal conditions, the LODs were 0.33 and 1.7 μg/L for MCPA and 2,4-D, respectively. Preconcentration factors of 670 and 836 were obtained for MCPA and 2,4-D, respectively. The precision of the proposed method was evaluated in terms of repeatability, which was <5.7% (n = 5). The applicability of the proposed method was evaluated by extraction and determination of chlorophenoxyacetic acids from some natural waters, which indicated that the matrices of natural waters have no significant effect on the extraction and derivatization efficiency of this method. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antioxidant Capacity, Phenolic Constituents and Toxicity of Hot Water Extract from Red Maple Buds.

PubMed

Meda, Naamwin R; Poubelle, Patrice E; Stevanovic, Tatjana

2017-06-01

The present study reports, for the first time, the results of the antioxidant capacity and the phenolic composition of a hot water extract from red maple buds (RMB), as well as its safety. In this regard and comparatively to antioxidant standards, this extract exhibits a significant antiradical capacity when tested by 2,2-diphenyl-1-picrylhydrazyl (DPPH · ) and anion superoxide trapping assays. High-resolution mass spectrometric and nuclear magnetic resonance analyses permitted to determine for the first time, in red maple species, cyanidin-3-O-glucoside, quercetin-3-O-galactoside, quercetin-3-O-arabinoside, and quercetin. Also, the quantification of individual phenolics by high-performance liquid chromatography method revealed that ginnalin A at 117.0 mg/g is the major compound of RMB hot water extract. Finally, using flow cytometry evaluation, the extract of RMB was determined to have no toxicity neither to cause significant modification of apoptosis process, up to concentration of 100 μg/ml, on human peripheral blood neutrophils. These results allow anticipating various fields of application of RMB water extract. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

Preparation of a polar monolithic stir bar based on methacrylic acid and divinylbenzene for the sorptive extraction of polar pharmaceuticals from complex water samples.

PubMed

Bratkowska, D; Fontanals, N; Cormack, P A G; Borrull, F; Marcé, R M

2012-02-17

A monolithic, hydrophilic stir bar coating based upon a copolymer of methacrylic acid and divinylbenzene [poly(MAA-co-DVB)] was synthesised and evaluated as a new polymeric phase for the stir bar sorptive extraction (SBSE) of polar compounds from complex environmental water samples. The experimental conditions for the extraction and liquid desorption in SBSE were optimised. Liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was used for the determination of a group of polar pharmaceuticals in environmental water matrices. The extraction performance of the poly(MAA-co-DVB) stir bar was compared to the extraction performance of a commercially available polydimethylsiloxane stir bar; it was found that the former gave rise to significantly higher extraction efficiency of polar analytes (% recovery values near to 100% for most of the studied analytes) than the commercial product. The developed method was applied to determine the studied analytes at low ng L⁻¹ in different complex environmental water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

A simple purification and activity assay of the coagulant protein from Moringa oleifera seed.

PubMed

Ghebremichael, Kebreab A; Gunaratna, K R; Henriksson, Hongbin; Brumer, Harry; Dalhammar, Gunnel

2005-06-01

Use of extracts from Moringa oleifera (MO) is of great interest for low-cost water treatment. This paper discusses water and salt extraction of a coagulant protein from the seed, purification using ion exchange, its chemical characteristics, coagulation and antimicrobial properties. The coagulant from both extracts is a cationic protein with pI greater than 9.6 and molecular mass less than 6.5 kDa. Mass spectrometric analysis of the purified water extract indicated that it contained at least four homologous proteins, based on MS/MS peptide sequence data. The protein is thermoresistant and remained active after 5h heat treatment at 95 degrees C. The coagulant protein showed both flocculating and antibacterial effects of 1.1--4 log reduction. With samples of high turbidity, the MO extract showed similar coagulation activity as alum. Cecropin A and MO extract were found to have similar flocculation effects for clay and microorganisms. Simple methods for both the purification and assay of MO coagulating proteins are presented, which are necessary for large-scale water treatment applications.

Suitability of TBA method for the evaluation of the oxidative effect of non-water-soluble and water-soluble rosemary extracts.

PubMed

Wada, Mitsuhiro; Nagano, Minori; Kido, Hirotsugu; Ikeda, Rie; Kuroda, Naotaka; Nakashima, Kenichiro

2011-01-01

The antioxidative effects of rosemary and grape-seed extracts spiked in human plasma were examined using the thiobarbituric acid (TBA) method. The TBA values of plasma spiked with reagents to generate reactive oxygen species, such as singlet oxygen ((1)O(2)), hydroxyl radicals ((·)OH), peroxynitrite (ONOO(-)), and superoxide anions (O(2)(·-)), were measured by a flow injection analysis method with fluorescence (FL) detection. TBA values obtained by the addition of 50 mg/mL of rosemary extracts for (1)O(2), (·)OH, ONOO(-), and O(2)(·-) increased to 964 ± 65%, 1063 ± 61%, 758 ± 78%, and 698 ± 41%, respectively (n = 3, P < 0.01), whereas the values with 1 mg/mL of grape-seed extracts or tocopherol decreased (40.2 - 66.3%). Furthermore, the antioxidative effects of rosemary extract in rat plasma, spiked with reagents to generate (·)OH, were examined by high-performance liquid chromatography with FL detection. No peak, other than TBA-malondialdehyde, could be detected using wavelengths of 532 (λ(ex)) and 553 nm (λ(em)).

Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry.

PubMed

Qiu, Huidong; Sun, Dongdi; Gunatilake, Sameera R; She, Jinyan; Mlsna, Todd E

2015-09-01

An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples. Copyright © 2015. Published by Elsevier B.V.

Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

PubMed

Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

2018-04-01

This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antioxidant Activity and Total Phenolic and Flavonoid Contents of Hieracium pilosella L. Extracts

PubMed Central

Stanojević, Ljiljana; Stanković, Mihajlo; Nikolić, Vesna; Nikolić, Ljubiša; Ristić, Dušica; Čanadanovic-Brunet, Jasna; Tumbas, Vesna

2009-01-01

The antioxidant activity of water, ethanol and methanol Hieracium pilosella L. extracts is reported. The antioxidative activity was tested by spectrophotometrically measuring their ability to scavenge a stable DPPH• free radical and a reactive hydroxyl radical trapped by DMPO during the Fenton reaction, using the ESR spectroscopy. Total phenolic content and total flavonoid content were evaluated according to the Folin-Ciocalteu procedure, and a colorimetric method, respectively. A HPLC method was used for identification of some phenolic compounds (chlorogenic acid, apigenin-7-O-glucoside and umbelliferone). The antioxidant activity of the investigated extracts slightly differs depending on the solvent used. The concentration of 0.30 mg/mL of water, ethanol and methanol extract is less effective in scavenging hydroxyl radicals (56.35, 58.73 and 54.35%, respectively) in comparison with the DPPH• radical scavenging activity (around 95% for all extracts). The high contents of total phenolic compounds (239.59–244.16 mg GAE/g of dry extract) and total flavonoids (79.13–82.18 mg RE/g of dry extract) indicated that these compounds contribute to the antioxidative activity. PMID:22346723

ANALYSIS OF SWINE LAGOONS AND GROUND WATER FOR ENVIRONMENTAL ESTROGENS

EPA Science Inventory

A method was developed for analysis of low levels of natural (estradiol, estrone, estriol) and synthetic (ethinyl estradiol) estrogens in ground water and swine waste lagoon effluent. The method includes solid phase extraction of the estrogens, preparation of pentafluorobenzyl de...

METAL SPECIATION IN SOIL, SEDIMENT, AND WATER SYSTEMS VIA SYNCHROTRON RADIATION RESEARCH

EPA Science Inventory

Metal contaminated environmental systems (soils, sediments, and water) have challenged researchers for many years. Traditional methods of analysis have employed extraction methods to determine total metal content and define risk based on the premise that as metal concentration in...

Heat reclaiming method and apparatus

DOEpatents

Jardine, Douglas M.

1984-01-01

Method and apparatus to extract heat by transferring heat from hot compressed refrigerant to a coolant, such as water, without exceeding preselected temperatures in the coolant and avoiding boiling in a water system by removing the coolant from direct or indirect contact with the hot refrigerant.

Selective extraction of bisphenol A from water by one-monomer molecularly imprinted magnetic nanoparticles.

PubMed

Lin, Zhenkun; Zhang, Yanfang; Su, Yu; Qi, Jinxia; Jia, Yinhang; Huang, Changjiang; Dong, Qiaoxiang

2018-01-15

One-monomer molecularly imprinted magnetic nanoparticles were prepared as adsorbents for selective extraction of bisphenol A from water in this study. A single bi-functional monomer was adopted for preparation of the molecularly imprinted polymer, avoiding the tedious trial-and-error optimizations as traditional strategy. Moreover, bisphenol F was used as the dummy template for bisphenol A to avoid the interference from residual template molecules. These nanoparticles showed not only large adsorption capacity and good selectivity to the bisphenol A but also outstanding magnetic response performance. Furthermore, they were successfully used as magnetic solid-phase extraction adsorbents of bisphenol A from various water samples, including tap water, river water, and seawater. The developed method was found to be much more efficient, convenient, and economical for selective extraction of bisphenol A compared with the traditional solid-phase extraction. Separation of these nanoparticles can be easily achieved with an external magnetic field, and the optimized adsorption time was only 15 min. The recoveries of bisphenol A in different water samples ranged from 85.38 to 93.75%, with relative standard deviation lower than 7.47%. These results showed that one-monomer molecularly imprinted magnetic nanoparticles had the potential to be popular adsorbents for selective extraction of pollutants from water. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical fluid extraction of fat from ground beef: effects of water on gravimetric and GC-FAME fat determinations.

PubMed

Eller, F J; King, J W

2001-10-01

This study investigated the supercritical carbon dioxide (SC-CO(2)) extraction of fat from ground beef and the effects of several factors on the gravimetric determination of fat. The use of ethanol modifier with the SC-CO(2) was not necessary for efficient fat extraction; however, the ethanol did increase the coextraction of water. This coextraction of water caused a significant overestimation of gravimetric fat. Oven-drying ground beef samples prior to extraction inhibited the subsequent extraction of fat, whereas oven-drying the extract after collection decreased the subsequent gas chromatographic fatty acid methyl ester (GC-FAME) fat determination. None of the drying agents tested were able to completely prevent the coextraction of water, and silica gel and molecular sieves inhibited the complete extraction of fat. Measurements of collection vial mass indicated that CO(2) extraction/collection causes an initial increase in mass due to the density of CO(2) (relative to displaced air) followed by a decrease in vial mass due to the removal of adsorbed water from the collection vial. Microwave-drying of the empty collection vials removes approximately 3 mg of adsorbed water, approximately 15-20 min is required for readsorption of the displaced water. For collection vials containing collected fat, microwave-drying effectively removed coextracted water, and the vials reached equilibration after approximately 10-15 min. Silanizing collection vials did not significantly affect weight loss during microwave-drying. SC-CO(2) can be used to accurately determine fat gravimetrically for ground beef, and the presented method can also be followed by GC-FAME analysis to provide specific fatty acid information as well.

Bioremediation of Turbid Surface Water Using Seed Extract from the Moringa oleifera Lam. (Drumstick) Tree.

PubMed

Lea, Michael

2014-05-01

An indigenous water treatment method uses Moringa oleifera seeds in the form of a crude water-soluble extract in suspension, resulting in an effective natural clarification agent for highly turbid and untreated pathogenic surface water. Efficient reduction (80.0% to 99.5%) of high turbidity produces an aesthetically clear supernatant, concurrently accompanied by 90.00% to 99.99% (1 to 4 log) bacterial reduction. Application of this low-cost Moringa oleifera protocol is recommended for water treatment where rural and peri-urban people living in extreme poverty are presently drinking highly turbid and microbiologically contaminated water. Copyright © 2014 John Wiley & Sons, Inc.

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.

An etched stainless steel wire/ionic liquid-solid phase microextraction technique for the determination of alkylphenols in river water.

PubMed

Cui, Meiyu; Qiu, Jinxue; Li, Zhenghua; He, Miao; Jin, Mingshi; Kim, Jiman; Quinto, Maurizio; Li, Donghao

2015-01-01

In this study, a stainless steel wire/ionic liquid-solid phase microextraction technique was developed for the direct extraction of APs from water samples. Some parameters were optimised, such as selection of the substrate and ILs, extraction time, extraction temperature, stirring rate and sample pH, etc. The experimental data demonstrated that the etched stainless steel wire was a suitable substrate for IL-coated SPME. The coating was prepared by directly depositing the ILs onto the surface of the etched stainless steel wire, which exhibited a porous structure and a high surface area. The [C8MIM][PF6] IL exhibited maximum efficiency with an extraction time of 30 min, and the aqueous sample was maintained at 40 °C and adjusted to pH 2 under stirring conditions. The enrichment factor of the IL coating for the four APs ranged from 1382 to 4779, the detection limits (LOD, S/N=3) of the four APs ranged from 0.01 to 0.04 ng mL(-1) and the RSD values for purified water spiked with APs ranged from 4.0 to 11.8% (n=3). The calibration graphs were linear in the concentration range from 0.5 to 200 ng mL(-1) (R(2)>0.9569). The optimised method was successfully applied for the analysis of real water samples, and the method was suitable for the extraction of APs from water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Copigmentation Of Anthocyanin Extract of Purple Sweet Potatoes (Ipomea Batatas L.) Using Ferulic Acid And Tannic Acid

NASA Astrophysics Data System (ADS)

Susanti, I.; Wijaya, H.; Hasanah, F.; Heryani, S.

2018-02-01

Copigmentation is one of the methods to improve the color stability and intensity of anthocyanin extract. This study aimed to do the copigmentation of the anthocyanin extract of purple sweet potato using ferulic acid and tannic acid. The anthocyanin extraction was conducted with distilled water at pH 7 and pH 2 while the copigmentation was conducted by varying the concentration of ferulic acid and tannic acid. The results showed that best anthocyanin extraction method of the purple sweet potato was using distilled water at pH 2. The yield of freeze dried anthocyanin on the extraction with distilled water at pH 2 was 1710 ppm, while the yield when using distilled water at pH 7 was 888 ppm. Ferulic acid and tannic acid can be used for the copigmentation of anthocyanin extract of purple sweet potato by observing the maximum wavelength shift (bathochromic effect, Δλmax) and increase of color intensity (hyperchromic effect, ΔAmax). The bathochromic effect of ferulic acid began to occur at a concentration of 0.01M, while the hypochromic effect on tannic acid occurred at a concentration of 0.005M and remained up to a concentration of 0.02M. The best copigmentation concentration of ferulic acid was 0.015M, while tannic acid was 0.02M. The use of tannic acid 0.02M is recommended compared to ferulic acid 0.015M because with the same bathocromic effect (Δλmaks = 3,9) results hyperchromic effect (ΔA = 0,258) higher by tannic acid.

Systematic screening of plant extracts from the Brazilian Pantanal with antimicrobial activity against bacteria with cariogenic relevance.

PubMed

Brighenti, F L; Salvador, M J; Delbem, Alberto Carlos Botazzo; Delbem, Ádina Cleia Bottazzo; Oliveira, M A C; Soares, C P; Freitas, L S F; Koga-Ito, C Y

2014-01-01

This study proposes a bioprospection methodology regarding the antimicrobial potential of plant extracts against bacteria with cariogenic relevance. Sixty extracts were obtained from ten plants--(1) Jatropha weddelliana, (2) Attalea phalerata, (3) Buchenavia tomentosa, (4) Croton doctoris, (5) Mouriri elliptica, (6) Mascagnia benthamiana, (7) Senna aculeata, (8) Unonopsis guatterioides, (9) Allagoptera leucocalyx and (10) Bactris glaucescens--using different extraction methods - (A) 70° ethanol 72 h/25°C, (B) water 5 min/100°C, (C) water 1 h/55°C, (D) water 72 h/25°C, (E) hexane 72 h/25°C and (F) 90° ethanol 72 h/25°C. The plants were screened for antibacterial activity at 50 mg/ml using the agar well diffusion test against Actinomyces naeslundii ATCC 19039, Lactobacillus acidophilus ATCC 4356, Streptococcus gordonii ATCC 10558, Streptococcus mutans ATCC 35688, Streptococcus sanguinis ATCC 10556, Streptococcus sobrinus ATCC 33478 and Streptococcus mitis ATCC 9811. The active extracts were tested to determine their minimum inhibitory concentration (MIC), minimum bactericidal concentration (MBC), cytotoxicity and chemical characterization. Forty-seven extracts (78%) were active against at least one microorganism. Extract 4A demonstrated the lowest MIC and MBC for all microorganisms except S. gordonii and the extract at MIC concentration was non-cytotoxic. The concentrated extracts were slightly cytotoxic. Electrospray ionization with tandem mass spectrometry analyses demonstrated that the extract constituents coincided with the mass of the terpenoids and phenolics. Overall, the best results were obtained for extraction methods A, B and C. The present work proved the antimicrobial activity of several plants. Particularly, extracts from C. doctoris were the most active against bacteria involved in dental caries disease. © 2014 S. Karger AG, Basel.

Solid-Phase Extraction Coupled to a Paper-Based Technique for Trace Copper Detection in Drinking Water.

PubMed

Quinn, Casey W; Cate, David M; Miller-Lionberg, Daniel D; Reilly, Thomas; Volckens, John; Henry, Charles S

2018-03-20

Metal contamination of natural and drinking water systems poses hazards to public and environmental health. Quantifying metal concentrations in water typically requires sample collection in the field followed by expensive laboratory analysis that can take days to weeks to obtain results. The objective of this work was to develop a low-cost, field-deployable method to quantify trace levels of copper in drinking water by coupling solid-phase extraction/preconcentration with a microfluidic paper-based analytical device. This method has the advantages of being hand-powered (instrument-free) and using a simple "read by eye" quantification motif (based on color distance). Tap water samples collected across Fort Collins, CO, were tested with this method and validated against ICP-MS. We demonstrate the ability to quantify the copper content of tap water within 30% of a reference technique at levels ranging from 20 to 500 000 ppb. The application of this technology, which should be sufficient as a rapid screening tool, can lead to faster, more cost-effective detection of soluble metals in water systems.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; extraction of nitroaromatic compounds from water by polystyrene divinylbenzene cartridge and determination by high-performance liquid chromatography

USGS Publications Warehouse

Lindley, C.E.; Burkhardt, M.R.; DeRusseau, S.N.

1994-01-01

Organic explosives are determined in samples of ground water and surface water with emphasis on identifying and quantifying trinitrotoluene (TNT) metabolites. Water samples are filtered to remove suspended particulate material and passed through a polystyrene divinylbenzene-packed cartridge by a vacuum-extraction system. The target analytes subsequently are eluted with acetonitrile. A high-performance liquid chromatograph (HPLC) equipped with a photodiode-array detector is used for sample analysis. Analytes are separated on an octadecylsilane column using a methanol, water, and acetonitrile gradient elution. The compounds 2,4- and 2,6-dinitrotoluene are separated through an independent, isocratic elution. Method detection limits, on the basis of a 1-liter sample size, range from 0.11 to 0.32 microgram per liter. Recoveries averaged from 71 to 101 percent for 13 analytes in one set of HPLC-grade water fortified at about 1 microgram per liter. The method is limited to use by analysts experienced in handling explosive materials. (USGS)

Determination of submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples by solid-phase extraction and liquid chromatography

USGS Publications Warehouse

Burkhardt, M.R.; Soliven, P.P.; Werner, S.L.; Vaught, D.G.

1999-01-01

A method for determining submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples has been developed. Caffeine is extracted from a 1 L water sample with a 0.5 g graphitized carbon-based solid-phase cartridge, eluted with methylene chloride-methanol (80 + 20, v/v), and analyzed by liquid chromatography with photodiode-array detection. The single-operator method detection limit for organic-free water samples was 0.02 ??g/L. Mean recoveries and relative standard deviations were 93 ?? 13% for organicfree water samples fortified at 0.04 ??g/L and 84 ?? 4% for laboratory reagent spikes fortified at 0.5 ??g/L. Environmental concentrations of caffeine ranged from 0.003 to 1.44 ??g/L in surface water samples and from 0.01 to 0.08 ??g/L in groundwater samples.

Comparison of ASE and SFE with Soxhlet, Sonication, and Methanolic Saponification Extractions for the Determination of Organic Micropollutants in Marine Particulate Matter.

PubMed

Heemken, O P; Theobald, N; Wenclawiak, B W

1997-06-01

The methods of accelerated solvent extraction (ASE) and supercritical fluid extraction (SFE) of polycyclic aromatic hydrocarbons (PAHs), aliphatic hydrocarbons, and chlorinated hydrocarbons from marine samples were investigated. The results of extractions of a certified sediment and four samples of suspended particulate matter (SPM) were compared to classical Soxhlet (SOX), ultrasonication (USE), and methanolic saponification extraction (MSE) methods. The recovery data, including precision and systematic deviations of each method, were evaluated statistically. It was found that recoveries and precision of ASE and SFE compared well with the other methods investigated. Using SFE, the average recoveries of PAHs in three different samples ranged from 96 to 105%, for ASE the recoveries were in the range of 97-108% compared to the reference methods. Compared to the certified values of sediment HS-6, the average recoveries of SFE and ASE were 87 and 88%, most compounds being within the limits of confidence. Also, for alkanes the average recoveries by SFE and ASE were equal to the results obtained by SOX, USE, and MSE. In the case of SFE, the recoveries were in the range 93-115%, and ASE achieved recoveries of 94-107% as compared to the other methods. For ASE and SFE, the influence of water on the extraction efficiency was examined. While the natural water content of the SPM sample (56 wt %) led to insufficient recoveries in ASE and SFE, quantitative extractions were achieved in SFE after addition of anhydrous sodium sulfate to the sample. Finally, ASE was applied to SPM-loaded filter candles whereby a mixture of n-hexane/acetone as extraction solvent allowed the simultaneous determination of PAHs, alkanes, and chlorinated hydrocarbons.

A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

PubMed

Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2017-07-01

Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

EPA Method 1615. Measurement of Enterovirus and Norovirus Occurrence in Water by Culture and RT-qPCR. Part III. Virus Detection by RT-qPCR

EPA Science Inventory

EPA Method 1615 measures enteroviruses and noroviruses present in environmental and drinking waters. The viral ribonucleic acid (RNA) from water sample concentrates is extracted and tested for enterovirus and norovirus RNA using reverse transcription-quantitative PCR (RT-qPCR). V...

Analysis of trace levels of sulfonamide and tetracycline antimicrobials in groundwater and surface water using solid-phase extraction and liquid chromatography/mass spectrometry

USGS Publications Warehouse

Lindsey, M.E.; Meyer, M.; Thurman, E.M.

2001-01-01

A method has been developed for the trace analysis of two classes of antimicrobials consisting of six sulfonamides (SAs) and five tetracyclines (TCs), which commonly are used for veterinary purposes and agricultural feed additives and are suspected to leach into ground and surface water. The method used solid-phase extraction and liquid chromatography/mass spectrometry (LC/MS) with positive ion electrospray. The unique combination of a metal chelation agent (Na2EDTA) with a macroporous copolymer resulted in quantitative recoveries by solid-phase extraction (mean recovery, 98 ?? 12%) at submicrogram-per-liter concentrations. An ammonium formate/formic acid buffer with a methanol/water gradient was used to separate the antimicrobials and to optimize the signal intensity. Mass spectral fragmentation and ionization characteristics were determined for each class of compounds for unequivocal identification. For all SAs, a characteristic m/z 156 ion representing the sulfanilyl fragment was identified. TCs exhibited neutral losses of 17 amu resulting from the loss of ammonia and 35 amu from the subsequent loss of water. Unusual matrix effects were seen only for TCs in this first survey of groundwater and surface water samples from sites around the United States, requiring that TCs be quantitated using the method of standard additions.

Molecularly imprinted solid-phase extraction combined with high performance liquid chromatography for analysis of phenolic compounds from environmental water samples.

PubMed

Feng, Qin-Zhong; Zhao, Li-Xia; Yan, Wei; Lin, Jin-Ming; Zheng, Zhi-Xia

2009-08-15

The molecularly imprinted bulk polymer with 2,4,6-trichlorophenol (2,4,6-TCP) as the template molecule and methylacrylic acid (MAA), ethylene glycol dimethacrylate (EGDMA) as functional monomer and the crosslinker, respectively, has been prepared and applied to the molecularly imprinted solid-phase extraction (MISPE) procedure for selective preconcentration of phenolic compounds from environmental water samples. Various parameters affecting the extraction efficiency of the polymer have been evaluated to optimize the selective preconcentration of the phenolic compounds from aqueous samples. The characteristics of the MISPE method were validated by HPLC. The recoveries ranged between 90% and 98% (RSD: 0.9-2.3%, n=3) for tap water, between 85% and 105% (RSD: 2.6-4.9%, n=3) for river water, between 78% and 98% (RSD: 2.6-5.4%, n=3) for sewage water fortified with 0.4 mg L(-1) of phenol, 4-chlorophenol (4-CP), 2,4-dichlorophenol (2,4-DCP), pentachlorophenol (PCP). It was demonstrated that this MISPE-HPLC method could be applied to direct preconcentration and determination of phenolic compounds in environmental water samples.

Speciation analysis of Mn(II)/Mn(VII) using Fe3O4@ionic liquids-β-cyclodextrin polymer magnetic solid phase extraction coupled with ICP-OES.

PubMed

Chen, Songqing; Qin, Xingxiu; Gu, Weixi; Zhu, Xiashi

2016-12-01

Ionic liquids-β-cyclodextrin polymer (ILs-β-CDCP) was attached on Fe 3 O 4 nanoparticles to prepare magnetic solid phase extraction agent (Fe 3 O 4 @ILs-β-CDCP). The properties and morphology of Fe 3 O 4 @ILs-β-CDCP were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction(XRD), size distribution and magnetic analysis. A new method of magnetic solid phase extraction (MSPE) coupled to ICP-OES for the speciation of Mn(II)/Mn(VII) in water samples was established. The results showed that Mn(VII) and total manganese [Mn(II)+Mn(VII)] were quantitatively extracted after adjusting aqueous sample solution to pH 6.0 and 10.0, respectively. Mn(II) was calculated by subtraction of Mn(VII) from total manganese. Fe 3 O 4 @ILs-β-CDCP showed a higher adsorption capacity toward Mn(II) and Mn(VII). Several factors, such as the pH value, extraction temperature and sample volume, were optimized to achieve the best extraction efficiency. Moreover, the adsorption ability of Fe 3 O 4 @ILs-β-CDCP would not be significantly lower after reusing of 10 times. The accuracy of the developed method was confirmed by analyzing certified reference materials (GSB 07-1189-2000), and by spiking spring water, city water and lake water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

[Effects of post-harvest processing and extraction methods on polysaccharides content of Dendrobium officinale].

PubMed

Li, Cong; Ning, Li-Dan; Si, Jin-Ping; Wu, Ling-Shang; Liu, Jing-Jing; Song, Xian-Shui; Yu, Qiao-Xian

2013-02-01

To reveal the quality variation of polysaccharide in Dendrobium officinale by post-harvest processing and extraction methods, and provide a basis for post-harvest processing and clinical and hygienical applications of Tiepifengdou (Dendrobii Officinalis Caulis). The content of polysaccharides were studied by 4 post-harvest processing methods, i. e. drying by drying closet, drying after scalding by boiling water, drying while twisting, and drying while twisting after scalding by boiling water. And a series of temperatures were set in each processing procedure. An orthogonal test L9 (3(4)) with crushed degrees, solid-liquid ratio, extraction time and extraction times as factors were designed to analyze the dissolution rate of polysaccharides in Tiepifengdou processed by drying while twisting at 80 degrees C. The content of polysaccharides was ranged from 26.59% to 32.70% in different samples processed by different processing methods, among which drying while twisting at 80 degrees C and 100 degrees C respectively were the best. Crushed degree was the most important influence on the dissolution rate of polysaccharides. The dissolution rate of polysaccharides was extremely low when the sample was boiled directly without crushing and sieving. Drying while twisting at 80 degrees C was the best post-harvest processing method, which can help to dry the fresh herbs and improve the accumulation of polysaccharides. Boiling the uncrushed Tiepifengdou for a long time as traditional method could not fully extract polysaccharides, while boiling the crushed Tiepifengdou can efficiently extract polysaccharides.

An on-line SPE-HPLC method for effective sample preconcentration and determination of fenoxycarb and cis, trans-permethrin in surface waters.

PubMed

Šatínský, Dalibor; Naibrtová, Linda; Fernández-Ramos, Carolina; Solich, Petr

2015-09-01

A new on-line SPE-HPLC method using fused-core columns for on-line solid phase extraction and large volume sample injection for increasing the sensitivity of detection was developed for the determination of insecticides fenoxycarb and cis-, trans-permethrin in surface waters. The separation was carried out on fused-core column Phenyl-Hexyl (100×4.6 mm), particle size 2.7 µm with mobile phase acetonitrile:water in gradient mode at flow rate 1.0 mL min(-1), column temperature 45°C. Large volume sample injection (1500 µL) to the extraction dimension using short precolumn Ascentis Express RP C-18 (5×4.6 mm); fused-core particle size 2.7 µm allowed effective sample preconcentration and efficient ballast sample matrix removal. The washing mobile phase consisting of a mixture of acetonitrile:water; 30:70, (v/v) was pumped at flow rate of 0.5 mL min(-1) through the extraction precolumn to the waste. Time of the valve switch for transferring the preconcentrated sample zone from the extraction to the separation column was set at 3rd min. Elution of preconcentrated insecticides from the extraction precolumn and separation on the analytical column was performed in gradient mode. Linear gradient elution started from 40% of acetonitrile at time of valve switch from SPE column (3rd min) to 95% of acetonitrile at 7th min. Synthetic dye sudan I was chosen as an internal standard. UV detection at wavelength 225 nm was used and the method reached the limits of detection (LOD) at ng mL(-1) levels for both insecticides. The method showing on-line sample pretreatment and preconcentration with highly sensitive determination of insecticides was applied for monitoring of fenoxycarb and both permethrin isomers in different surface water samples in Czech Republic. The time of whole analysis including on-line extraction, interferences removal, chromatography separation and system equilibration was less than 8 min. Copyright © 2015 Elsevier B.V. All rights reserved.

Dynamic fabric phase sorptive extraction for a group of pharmaceuticals and personal care products from environmental waters.

PubMed

Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Marcé, Rosa Maria; Fontanals, Núria

2016-07-22

This paper describes for the first time the use of a new extraction technique, based on fabric phase sorptive extraction (FPSE). This new mode proposes the extraction of the analytes in dynamic mode in order to reduce the extraction time. Dynamic fabric phase sorptive extraction (DFPSE) followed by liquid chromatography-tandem mass spectrometry was evaluated for the extraction of a group of pharmaceuticals and personal care products (PPCPs) from environmental water samples. Different parameters affecting the extraction were optimized and best conditions were achieved when 50mL of sample at pH 3 was passed through 3 disks and analytes retained were eluted with 10mL of ethyl acetate. The recoveries were higher than 60% for most of compounds with the exception of the most polar ones (between 8% and 38%). The analytical method was validated with environmental samples such as river water and effluent and influent wastewater, and good performance was obtained. The analysis of samples revealed the presence of some PPCPs at low ngL(-1) concentrations. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

[Polyphenolic compounds analysis and antioxidant activity in fruits of Prunus spinosa L.

PubMed

Varga, E; Domokos, E; Fogarasi, E; Steanesu, R; Fülöp, I; Croitoru, M D; Laczkó-Zöld, E

2017-01-01

Prunus spinosa L. (blackthorn, sloe) is a com- mon species in the wild flora of Europe. Marmalade, syrup, and alcoholic beverages have been prepared from fruits. In folk medicine they'are used due to the astringent effect. However there are few studies on these indigenous fruits. According to the literature they contain tannins, anthocyanins, sugars, vitamin C etc. Our objective is to determine the antioxidant activity as related to their phenolic composition. For this purpose we prepared extracts using methanol, methanol-water (1: 1) and water. The antioxidant activity was determined by DPPH method and by photochemiluminescens (PCL) method. The total polyphenols, total anthocyanins and flavonoids were determined by colorimetric methods. Individual polyphenols were identified by a RP-HPLC-UVIVIS method. The antioxidant activity decreased in the extracts as follows: methanol > methanol-water > water (IC₅₀= 1.33 mg/ml for DPPH; 11.94 μmol AAEIml for PCL > IC₅₀ = 1.87 mg/ml for DPPH; 10.35 μmol AAElml for PCL > IC₅₀ = 15.29 mg/ml for DPPH, 1.89 μmol AAElml for PCL) which is cor- related with the total polyphenol content (369 mg/100g > 244 mg1100g > 101 mg1100g) and total anthocyanin content (37.11 mg/100 g > 16.33 mg/100g > 7.76 mg/100g). The fla- vonoid content is similar in the three extracts (between 35.82 - 37.32 mg1100 g). The HPLC analysis shows high chloro- genic and neochlorogenic acid levels, followed by glycosides of quercetin. Our results demonstrated that blackthorn fruits are a rich source of phenolic compounds, with anti- oxidant activity, which are best extracted with methanol or methanol-water.

Supported liquid membrane-liquid chromatography-mass spectrometry analysis of cyanobacterial toxins in fresh water systems

NASA Astrophysics Data System (ADS)

Mbukwa, Elbert A.; Msagati, Titus A. M.; Mamba, Bhekie B.

Harmful algal blooms (HABs) are increasingly becoming of great concern to water resources worldwide due to indiscriminate waste disposal habits resulting in water pollution and eutrophication. When cyanobacterial cells lyse (burst) they release toxins called microcystins (MCs) that are well known for their hepatotoxicity (causing liver damage) and have been found in eutrophic lakes, rivers, wastewater ponds and other water reservoirs. Prolonged exposure to low concentrated MCs are equally of health importance as they are known to be bioaccumulative and even at such low concentration do exhibit toxic effects to aquatic animals, wildlife and human liver cells. The application of common treatment processes for drinking water sourced from HABs infested reservoirs have the potential to cause algal cell lyses releasing low to higher amounts of MCs in finished water. Trace microcystins in water/tissue can be analyzed and quantified using Liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) following solid-phase extraction (SPE) sample clean-up procedures. However, extracting MCs from algal samples which are rich in chlorophyll pigments and other organic matrices the SPE method suffers a number of drawbacks, including cartridge clogging, long procedural steps and use of larger volumes of extraction solvents. We applied a supported liquid membrane (SLM) based technique as an alternative sample clean-up method for LC-ESI-MS analysis of MCs from both water and algal cells. Four (4) MC variants (MC-RR, -YR, -LR and -WR) from lyophilized cells of Microcystis aeruginosa and water collected from a wastewater pond were identified) and quantified using LC-ESI-MS following a SLM extraction and liquid partitioning step, however, MC-WR was not detected from water extracts. Within 45 min of SLM extraction all studied MCs were extracted and pre-concentrated in approximately 15 μL of an acceptor phase at an optimal pH 2.02 of the donor phase (sample). The highest total quantifiable intracellular and extracellular MCs were 37.039 ± 0.087 μg/g DW and 5.123 ± 0.018 μg/L, respectively. The concentrations of MC-RR were the highest from all samples studied recording maximum values of 21.579 ± 0.066 μg/g DW and 3.199 ± 0.012 μg/L for intracellular and extracellular quantities, respectively.

Depuration Study of Heavy Metal Lead (Pb) and Copper (Cu) in Green Mussels Perna viridis through Continues-discontinues and Acid Extraction Methods

NASA Astrophysics Data System (ADS)

Budiawan; Bakri, Ridla; Cahaya Dani, Intan; Handayani, Sri; Ade Kurnia Putri, Rizki; Tamala, Riska

2018-01-01

Green mussel or Perna viridis is filter feeder, which is very susceptible to heavy metals. It takes an effort to release heavy metal contents on the green shell, one of method that can be used to release heavy metal from green shell is depuration proccess. In this research, the depuration process was conducted by continues method of depuration, discontinues method by using various kind of water and acid extraction. The optimum time of continues depuration method is 1.5 hours, with circulation speed 250 L/h and result of Pb metal content decreased is equal to 30.048% and 29.748% for Cu. In the discontinues method, the optimum result was reached at 100oC by using PAM water as the media at 3 h immersion period with decrease of Pb metal content 35.001% and Cu metal content 39.015%. In the acid extraction method, the optimum condition was achieved by 11% acetic acid solvent with decreasing of Pb and Cu levels are 88.224% and 76.298%. For the determination of protein content, the decrease of protein content obtained by treatment with 11% acetic acid extract showed decrease of protein content 36.656% with Kjeldahl method.

Microwave- and ultrasound-assisted extraction of vanillin and its quantification by high-performance liquid chromatography in Vanilla planifolia.

PubMed

Sharma, Anuj; Verma, Subash Chandra; Saxena, Nisha; Chadda, Neetu; Singh, Narendra Pratap; Sinha, Arun Kumar

2006-03-01

Microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and conventional extraction of vanillin and its quantification by HPLC in pods of Vanilla planifolia is described. A range of nonpolar to polar solvents were used for the extraction of vanillin employing MAE, UAE and conventional methods. Various extraction parameters such as nature of the solvent, solvent volume, time of irradiation, microwave and ultrasound energy inputs were optimized. HPLC was performed on RP ODS column (4.6 mm ID x 250 mm, 5 microm, Waters), a photodiode array detector (Waters 2996) using gradient solvent system of ACN and ortho-phosphoric acid in water (0.001:99.999 v/v) at 25 degrees C. Regression equation revealed a linear relationship (r2 > 0.9998) between the mass of vanillin injected and the peak areas. The detection limit (S/N = 3) and limit of quantification (S/N = 10) were 0.65 and 1.2 microg/g, respectively. Recovery was achieved in the range 98.5-99.6% for vanillin. Maximum yield of vanilla extract (29.81, 29.068 and 14.31% by conventional extraction, MAE and UAE, respectively) was found in a mixture of ethanol/water (40:60 v/v). Dehydrated ethanolic extract showed the highest amount of vanillin (1.8, 1.25 and 0.99% by MAE, conventional extraction and UAE, respectively).

An Improved Method for Extraction and Separation of Photosynthetic Pigments

ERIC Educational Resources Information Center

Katayama, Nobuyasu; Kanaizuka, Yasuhiro; Sudarmi, Rini; Yokohama, Yasutsugu

2003-01-01

The method for extracting and separating hydrophobic photosynthetic pigments proposed by Katayama "et al." ("Japanese Journal of Phycology," 42, 71-77, 1994) has been improved to introduce it to student laboratories at the senior high school level. Silica gel powder was used for removing water from fresh materials prior to…

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 ...

Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

PubMed

Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

2017-03-04

Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

Simultaneous determination of bisphenols and alkylphenols in water by solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry.

PubMed

Shan, Xiao Mei; Shen, Deng Hui; Wang, Bing Shuang; Lu, Bei Bei; Huang, Fa Yuan

2014-06-01

To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0 μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%. Relative standard deviations (RSDs) were between 1.26% and 3.67%. Applying this method to detect the source water of Chaohu Lake and drinking water of Hefei, six target compounds were detected in different levels. This method is simple with high sensitivity and selectivity, could be suitable for the determination of these compounds in source and drinking water. Copyright © 2014 The Editorial Board of Biomedical and Environmental Sciences. Published by China CDC. All rights reserved.

Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

2006-01-01

A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance (greater than 25 percent relative standard deviation), (2) reference standards prepared from technical mixtures, or (3) potential blank contamination. Samples were preserved by freezing to -20 degrees Celsius. The U.S. Geological Survey National Water Quality Laboratory has established a 1-year sample-holding time limit (prior to sample extraction) from the date of sample collection (if the sample is kept at -20?C) until a statistically accepted method can be used to determine the effectiveness of the sample-freezing procedure.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

PubMed

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

Zero valent Fe-reduced graphene oxide quantum dots as a novel magnetic dispersive solid phase microextraction sorbent for extraction of organophosphorus pesticides in real water and fruit juice samples prior to analysis by gas chromatography-mass spectrometry.

PubMed

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

2018-01-01

A selective and sensitive magnetic dispersive solid-phase microextraction (MDSPME) coupled with gas chromatography-mass spectrometry was developed for extraction and determination of organophosphorus pesticides (Sevin, Fenitrothion, Malathion, Parathion, and Diazinon) in fruit juice and real water samples. Zero valent Fe-reduced graphene oxide quantum dots (rGOQDs@ Fe) as a new and effective sorbent were prepared and applied for extraction of organophosphorus pesticides using MDSPME method. In order to study the performance of this new sorbent, the ability of rGOQDs@ Fe was compared with graphene oxide and magnetic graphene oxide nanocomposite by recovery experiments of the organophosphorus pesticides. Several affecting parameters in the microextraction procedure, including pH of donor phase, donor phase volume, stirring rate, extraction time, and desorption conditions such as the type and volume of solvents and desorption time were thoroughly investigated and optimized. Under the optimal conditions, the method showed a wide linear dynamic range with R-square between 0.9959 and 0.9991. The limit of detections, the intraday and interday relative standard deviations (n = 5) were less than 0.07 ngmL -1 , 4.7, and 8.6%, respectively. The method was successfully applied for extraction and determination of organophosphorus pesticides in real water samples (well, river and tap water) and fruit juice samples (apple and grape juice). The obtained relative recoveries were in the range of 82.9%-113.2% with RSD percentages of less than 5.8% for all the real samples.

Freeze-out extraction of monocarboxylic acids from water into acetonitrile under the action of centrifugal forces

NASA Astrophysics Data System (ADS)

Bekhterev, V. N.

2016-10-01

It is established that the efficiency of the freezing-out extraction of monocarboxylic acids C3-C;8 and sorbic acid from water into acetonitrile increases under the action of centrifugal forces. The linear growth of the partition coefficient in the homologous series of C2-C8 acids with an increase in molecule length, and the difference between the efficiency of extracting sorbic and hexanoic acid, are discussed using a theoretical model proposed earlier and based on the adsorption-desorption equilibrium of the partition of dissolved organic compounds between the resulting surface of ice and the liquid phase of the extract. The advantages of the proposed technique with respect to the degree of concentration over the method of low-temperature liquid-liquid extraction are explained in light of the phase diagram for the water-acetonitrile mixture.

A surprising method for green extraction of essential oil from dry spices: Microwave dry-diffusion and gravity.

PubMed

Farhat, Asma; Fabiano-Tixier, Anne-Sylvie; Visinoni, Franco; Romdhane, Mehrez; Chemat, Farid

2010-11-19

Without adding any solvent or water, we proposed a novel and green approach for the extraction of secondary metabolites from dried plant materials. This "solvent, water and vapor free" approach based on a simple principle involves the application of microwave irradiation and earth gravity to extract the essential oil from dried caraway seeds. Microwave dry-diffusion and gravity (MDG) has been compared with a conventional technique, hydrodistillation (HD), for the extraction of essential oil from dried caraway seeds. Essential oils isolated by MDG were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained by HD, but MDG was better than HD in terms of rapidity (45min versus 300min), energy saving, and cleanliness. The present apparatus permits fast and efficient extraction, reduces waste, avoids water and solvent consumption, and allows substantial energy savings. Copyright © 2010 Elsevier B.V. All rights reserved.

Monitoring trihalomethanes in chlorinated waters using a dispersive liquid-liquid microextraction method with a non-chlorinated organic solvent and gas chromatography-mass spectrometry.

PubMed

Pacheco-Fernández, Idaira; Herrera-Fuentes, Ariadna; Delgado, Bárbara; Pino, Verónica; Ayala, Juan H; Afonso, Ana M

2017-03-01

The environmental monitoring of trihalomethanes (THMs) has been performed by setting up a dispersive liquid-liquid microextraction method in combination with gas chromatography (GC)-mass spectrometry (MS). The optimized method only requires ∼26 µL of decanol as extractant solvent, dissolved in ∼1 mL of acetone (dispersive solvent) for 5 mL of the environmental water containing THMs. The mixture is then subjected to vortex for 1 min and then centrifuged for 2 min at 3500 rpm. The microdroplet containing the extracted THMs is then sampled with a micro-syringe, and injected (1 µL) in the GC-MS. The method is characterized for being fast (3 min for the entire sample preparation step) and environmentally friendly (low amounts of solvents required, being all non-chlorinated), and also for getting average relative recoveries of 90.2-106% in tap waters; relative standard deviation values always lower than 11%; average enrichment factors of 48-49; and detection limits down to 0.7 µg·L-1. Several waters: tap waters, pool waters, and wastewaters were successfully analyzed with the method proposed. Furthermore, the method was used to monitor the formation of THMs in wastewaters when different chlorination parameters, namely temperature and pH, were varied.

Determination of toxic compounds in paper-recycling process waters by gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

PubMed

Rigol, A; Latorre, A; Lacorte, S; Barceló, D

2002-07-19

Three analytical methods were developed for the determination of toxic compounds in recirculating waters of a paper-recycling industry. Three main groups of compounds were considered: (i) wood extractives originated from the raw material; (ii) biocides added during the production process and (iii) surfactants and other adjuvants present in the formulates of these biocides. Wood extractives considered in this study included fatty and resin acids. They were analysed by liquid-liquid extraction using methyl tert.-butyl ether, followed by gas chromatography-mass spectrometry for previous formation of the respective trimethylsilyl esters. Water samples were also extracted with Oasis HLB (copolymer [poly(divinylbenzene-co-N-vinylpyrrolidone]) solid-phase extraction cartridges of 60 mg and analysed by liquid chromatography-electrospray mass spectrometry for the determination of additives and biocides. Using these two approaches levels up to 15 mg/l for total resin and fatty acids, 5 mg/l for alkylbenzene sulfonates and 2-(thiocyanomethylthio)benzotiazol, 100 microg/l for bisphenol A and 2,2-dibromo-3-nitrilepropionamide, and 300 microg/l for nonylphenol ethoxycarboxylate were detected in process waters at different production treatment stages. These levels are of relevance since poor water quality affects the paper-recycling process, the primary water treatment process and eventually, the environmental water quality.

Ginsenoside extraction from Panax quinquefolium L. (American ginseng) root by using ultrahigh pressure.

PubMed

Zhang, Shouqin; Chen, Ruizhan; Wu, Hua; Wang, Changzheng

2006-04-11

A new method of ultrahigh pressure extraction (UPE) was used to extract the ginsenosides from Panax quinquefolium L. (American ginseng) root at room temperature. Several solvents, including water, ethanol, methanol, and n-butanol were used in the UPE. The ginsenosides were quantified by a HPLC equipped with UV-vis detector. The results showed that ethanol is the most efficient solvent among the used ones. Compared with other methods, i.e., Soxhlet extraction, heat reflux extraction, ultrasound-assisted extraction, microwave-assisted extraction, and supercritical CO2 extraction, the UPE has the highest extraction yield in the shortest time. The extraction yield of 0.861% ginsenoside-Rc in 2 min was achieved by the UPE, while the yields of 0.284% and 0.661% were obtained in several hours by supercritical CO2 extraction and the heat reflux extraction, respectively.

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Benzo(a)pyrene accumulation in soils of technogenic emission zone by subcritical water extraction method

NASA Astrophysics Data System (ADS)

Sushkova, Svetlana; Minkina, Tatiana; Kizilkaya, Ridvan; Mandzhieva, Saglara; Batukaev, Abdulmalik; Bauer, Tatiana; Gulser, Coskun

2016-04-01

The purpose of research is the assessment of main marker of polycyclic aromatic hydrocarbons contamination, benzo[a]pyrene (BaP) content in soils of emission zone of the power complex plant in soils with use of ecologically clean and effective subcritical water extraction method. Studies were conducted on the soils of monitoring plots subjected to Novocherkassk Power Plant emissions from burning coal. In 2000, monitoring plots were established at different distances from the NPS (1.0-20.0 km). Soil samples for the determination of soil properties and the contents of BaP were taken from a depth of 0-20 cm. The soil cover in the region under study consisted of ordinary chernozems, meadow-chernozemic soils, and alluvial meadow soils. This soil revealed the following physical and chemical properties: Corg-3.1-5.0%, pH-7.3-7.6, ECE-31.2-47.6 mmol(+)/100g; CaCO3-0.2-1.0%, the content of physical clay - 51-67% and clay - 3-37%. BaP extraction from soils was carried out by a subcritical water extraction method. Subcritical water extraction of BaP from soil samples was conducted in a specially developed extraction cartridge made of stainless steel and equipped with screw-on caps at both ends. It was also equipped with a manometer that included a valve for pressure release to maintain an internal pressure of 100 atm. The extraction cartridge containing a sample and water was placed into an oven connected to a temperature regulator under temperature 250oC and pressure 60 atm. The BaP concentration in the acetonitrile extract was determined by HPLC. The efficiency of BaP extraction from soil was determined using a matrix spike. The main accumulation of pollutant in 20 cm layer of soils is noted directly in affected zone on the plots situated at 1.2, 1.6, 5.0, 8.0 km from emission source in the direction of prevailing winds. The maximum quantity of a pollutant was founded in the soil of the plot located mostly close to a source of pollution in the direction of prevailing winds. Value from 2012 to 2013 reached to 316.5 mkg/kg in 5 cm soil layer and 217.8 mkg/kg in 5-20 cm soil layer that exceeded the BaP maximum concentration limit level in the soil up to 15 times. The maximum limited concentration of BaP in soil is 20 mkg/kg according Russian Federation legislation. Thus, a method of BaP determination in soils has been approved as based upon the subcritical water extraction under the optimum conditions. The efficiency of the given method involves the use of subcritical water as an environmentally friendly solvent, a shorter time for environmental analysis. BaP distribution and accumulation tendencies were investigated during the 2 years of monitoring researches in studied soils. The main factor of technogenic influence on the soil the investigated area are toxic emissions of a power complex plant from burning coal. Despite the environmental activities of in the enterprise, the impact of emissions on the environment location nearby today is still primary. This research was supported by projects of the Ministry of Education and Science of Russia, no. 5.885.2014/K and Grant of President of Russian Federation no. MK-6827.2015.4, RFBR no. 15-35-21134.

Determination of Triazine Herbicides in Drinking Water by Dispersive Micro Solid Phase Extraction with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometric Detection.

PubMed

Chen, Dawei; Zhang, Yiping; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

2015-11-11

A novel dispersive micro solid phase extraction (DMSPE) method based on a polymer cation exchange material (PCX) was applied to the simultaneous determination of the 30 triazine herbicides in drinking water with ultrahigh-performance liquid chromatography-high-resolution mass spectrometric detection. Drinking water samples were acidified with formic acid, and then triazines were adsorbed by the PCX sorbent. Subsequently, the analytes were eluted with ammonium hydroxide/acetonitrile. The chromatographic separation was performed on an HSS T3 column using water (4 mM ammonium formate and 0.1% formic acid) and acetonitrile (0.1% formic acid) as the mobile phase. The method achieved LODs of 0.2-30.0 ng/L for the 30 triazines, with recoveries in the range of 70.5-112.1%, and the precision of the method was better than 12.7%. These results indicated that the proposed method had the advantages of convenience and high efficiency when applied to the analysis of the 30 triazines in drinking water.

Magnetic solid-phase extraction of tetracyclines using ferrous oxide coated magnetic silica microspheres from water samples.

PubMed

Lian, Lili; Lv, Jinyi; Wang, Xiyue; Lou, Dawei

2018-01-26

A novel magnetic solid-phase extraction approach was proposed for extraction of potential residues of tetracyclines (TCs) in tap and river water samples, based on Fe 3 O 4 @SiO 2 @FeO magnetic nanocomposite. Characterized results showed that the received Fe 3 O 4 @SiO 2 @FeO had distinguished magnetism and core-shell structure. Modified FeO nanoparticles with an ∼5 nm size distribution were homogeneously dispersed on the surface of the silica shell. Owing to the strong surface affinity of Fe (II) toward TCs, the magnetic nanocomposite could be applied to efficiently extract three TCs antibiotics, namely, oxytetracycline, tetracycline and chlortetracycline from water samples. Several factors, such as sorbent amount, pH condition, adsorption and desorption time, desorption solvent, selectivity and sample volume, influencing the extraction performance of TCs were investigated and optimized. The developed method showed excellent linearity (R > 0.9992) in the range of 0.133-333 μg L -1 , under optimized conditions. The limits of detection were between 0.027 and 0.107 μg L -1 for oxytetracycline, tetracycline and chlortetracycline, respectively. The feasibility of this method was evaluated by analysis of tap and river water samples. The recoveries at the spiked concentration levels ranged from 91.0% to 104.6% with favorable reproducibility (RSD < 4%). Copyright © 2017 Elsevier B.V. All rights reserved.

Screening of crude extracts of six medicinal plants used in South-West Nigerian unorthodox medicine for anti-methicillin resistant Staphylococcus aureus activity

PubMed Central

Akinyemi, Kabir O; Oladapo, Olukayode; Okwara, Chidi E; Ibe, Christopher C; Fasure, Kehinde A

2005-01-01

Background Six Nigerian medicinal plants Terminalia avicennioides, Phylantus discoideus, Bridella ferruginea, Ageratum conyzoides, Ocimum gratissimum and Acalypha wilkesiana used by traditional medical practitioners for the treatment of several ailments of microbial and non-microbial origins were investigated for in vitro anti-methicillin Resistant Staphylococcus aureus (MRSA) activity. Methods Fresh plant materials were collected from the users. Water and ethanol extracts of the shredded plants were obtained by standard methods. The Bacterial cultures used were strains of MRSA isolated from patients. MRSA was determined by the reference broth microdilution methods using the established National Committee for Clinical Laboratory Standards break points. Staphylococcus aureus NCIB 8588 was used as a standard strain. Susceptibility testing and phytochemical screening of the plant extracts were performed by standard procedures. Controls were maintained for each test batch. Results Both water and ethanol extracts of T. avicennioides, P. discoideus, O. gratissimum, and A. wilkesiana were effective on MRSA. The Minimum Inhibition Concentration (MIC) and Minimum Bactericidal Concentration (MBC) of the ethanol extracts of these plants range from 18.2 to 24.0 mcg/ml and 30.4 to 37.0 mcg/ml respectively. In contrast, MIC range of 30.6 to 43.0 mcg/ml and 55.4 to 71.0 mcg/ml were recorded for ethanol and water extracts of B. ferruginea, and A. conyzoides respectively. Higher MBC values were obtained for the two plants. These concentrations were too high to be considered active in this study. All the four active plants contained at least trace amount of anthraquinones. Conclusion Our results offer a scientific basis for the traditional use of water and ethanol extracts of A. wilkesiana, O. gratissimum, T. avicennioides and P. discoideus against MRSA-associated diseases. However, B. ferruginea and A. conyzoides were ineffective in vitro in this study; we therefore suggest the immediate stoppage of their traditional use against MRSA-associated diseases in Lagos, Nigeria. PMID:15762997

A method for the extraction and quantitation of phycoerythrin from algae

NASA Technical Reports Server (NTRS)

Stewart, D. E.

1982-01-01

A summary of a new technique for the extraction and quantitation of phycoerythrin (PHE) from algal samples is described. Results of analysis of four extracts representing three PHE types from algae including cryptomonad and cyanophyte types are presented. The method of extraction and an equation for quantitation are given. A graph showing the relationship of concentration and fluorescence units that may be used with samples fluorescing around 575-580 nm (probably dominated by cryptophytes in estuarine waters) and 560 nm (dominated by cyanophytes characteristics of the open ocean) is provided.

Utilization of an ionic liquid in situ preconcentration method for the determination of the 15 + 1 European Union polycyclic aromatic hydrocarbons in drinking water and fruit-tea infusions.

PubMed

Germán-Hernández, Mónica; Crespo-Llabrés, Pilar; Pino, Verónica; Ayala, Juan H; Afonso, Ana M

2013-08-01

An ionic liquid (IL) in situ preconcentration method was optimized and applied to the monitoring of the 15 + 1 European Union polycyclic aromatic hydrocarbons in water and fruit-tea infusions. The optimized method utilizes 10 mL of water (or infusion) containing 38 μL of the IL 1-butyl-3-methylimidazolium chloride and a content of 36.1 g/L NaCl, which are mixed with Li-NTf2 (340 μL, 0.2 g/mL), followed by vortex (4 min) and centrifugation (5 min). The obtained microdroplet containing hydrocarbons is diluted with acetonitrile and injected into an HPLC with UV/Vis and fluorescence detection. The method presented average enrichment factors of 127 for water (tap water and bottled water) and 27 for two fruit-tea infusions; with average relative recoveries of 86.7 and 106% for water and fruit-tea infusions, respectively. The method was sensitive, with detection limits ranging from 0.001 to 0.050 ng/mL in water, and from 0.010 to 0.600 ng/mL in fruit-tea infusions, for the fluorescent hydrocarbons. Real extraction efficiencies ranged from 12.7 to 58.7% for water, and from 20.2 to 117% for the infusions. The method was also fast (~12 min) and free of organic solvents in the extraction step. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Occurrence of naproxen, ibuprofen, and diclofenac residues in wastewater and river water of KwaZulu-Natal Province in South Africa.

PubMed

Madikizela, Lawrence Mzukisi; Chimuka, Luke

2017-07-01

The present paper reports a detailed study that is based on the monitoring of naproxen, ibuprofen, and diclofenac in Mbokodweni River and wastewater treatment plants (WWTPs) located around the city of Durban in KwaZulu-Natal Province of South Africa. Target compounds were extracted from water samples using a multi-template molecularly imprinted solid-phase extraction prior to separation and quantification on a high-performance liquid chromatography equipped with photo diode array detector. The analytical method yielded the detection limits of 0.15, 1.00, and 0.63 μg/L for naproxen, ibuprofen, and diclofenac, respectively. Solid-phase extraction method was evaluated for its performance using deionized water samples that were spiked with 5 and 50 μg/L of target compounds. Recoveries were greater than 80% for all target compounds with RSD values in the range of 4.1 to 10%. Target compounds were detected in most wastewater and river water samples with ibuprofen being the most frequently detected pharmaceutical. Maximum concentrations detected in river water for naproxen, ibuprofen, and diclofenac were 6.84, 19.2, and 9.69 μg/L, respectively. The concentrations of target compounds found in effluent and river water samples compared well with some studies. The analytical method employed in this work is fast, selective, sensitive, and affordable; therefore, it can be used routinely to evaluate the occurrence of acidic pharmaceuticals in South African water resources.

A new method for concentration analysis of bacterial endotoxins in perfluorocarbon

NASA Astrophysics Data System (ADS)

Chen, Dan-Dan; Feng, Xiao-Ming; Wang, Chun-Ren; Huang, Qing-Quan; Yang, Zhao-Peng; Meng, Qing-Yuan

2014-12-01

This communication demonstrates the feasibility of the gel-clot method for the analysis of bacterial endotoxins in water extracts of perfluorocarbon which is a water insoluble liquid medical device. Perfluorocarbon (10 mL) was shaken with 10mL water for 15 min at 2000 r/min and the endotoxin present was extracted to the aqueous phase without interference inhibition/enhancement of the product and the recovery of endotoxin added to perfluorocarbon was determined. A validation study confirmed that endotoxins presented in perfluorocarbon pass over into the aqueous phase at concentrations of 20, 10 and 5 EU/mL with recoveries from 86.8% to 96.8%. Therefore, the gel-clot test is suitable for detecting bacterial endotoxins in perfluorocarbon which is a water insoluble medical device.

A robust method for determining water-extractable alkylphenol polyethoxylates in textile products by reaction-based headspace gas chromatography.

PubMed

Zhang, Shu-Xin; Chai, Xin-Sheng; Huang, Bo-Xi; Mai, Xiao-Xia

2015-08-07

Alkylphenol polyethoxylates (APEO), surfactants used in the production of textiles, have the potential to move from the fabric to the skin of the person wearing the clothes, posing an inherent risk of adverse health consequences. Therefore, the textile industry needs a fast, robust method for determining aqueous extractable APEO in fabrics. The currently-favored HPLC methods are limited by the presence of a mixture of analytes (due to the molecular weight distribution) and a lack of analytical standards for quantifying results. As a result, it has not been possible to reach consensus on a standard method for the determination of APEO in textiles. This paper addresses these limitations through the use of reaction-based head space-gas chromatography (HS-GC). Specifically, water is used to simulate body sweat and extract APEO. HI is then used to react the ethoxylate chains to depolymerize the chains into iodoethane that is quantified through HS-GC, providing an estimate of the average amount of APEO in the clothing. Data are presented to justify the optimal operating conditions; i.e., water extraction at 60°C for 1h and reaction with a specified amount of HI in the headspace vial at 135°C for 4h. The results show that the HS-GC method has good precision (RSD<10%) and good accuracy (recoveries from 95 to 106%) for the quantification of APEO content in textile and related materials. As such, the method should be a strong candidate to become a standard method for such determinations. Copyright © 2015 Elsevier B.V. All rights reserved.

Optimization of extraction conditions of some polyphenolic compounds from parsley leaves (Petroselinum crispum).

PubMed

Kuźma, Paula; Drużyńska, Beata; Obiedziński, Mieczysław

2014-01-01

Parsley leaf is a rich source of natural antioxidants, which serve a lot of functions in human body and prevent food from oxidation processes. The aim of the study was to investigate the influence of different extraction solvents and times of extraction on natural antioxidants content. Owing to the knowledge of the properties of extracted components and solvents, as well as their interactions, it is possible to achieve a high effectiveness of active compounds recovery. Three different extraction solvents (acetone 70% in water, methanol 80% in water and distilled water) and different times of extraction (30 and 60 minutes) were used to determine the efficiency of extraction of polyphenols and catechins, antioxidant activity against free radicals DPPH and ABTS and the ability to chelate ion Fe(2+) in dried parsley leaves. Other natural antioxidants contents in parsley leaves were also determined. In this study the best extraction solvent for polyphenols was acetone 70% and for catechins was distilled water. All extracts examined displayed the antioxidative activity, but water was the best solvent in the method of assaying the activity against ABTS(•+) and Fe(2+) ions chelating capability, whereas methanol turned out to be the least effective in this respect. Opposite results were observed in the case of determining the activity against DPPH(•). The prolongation of the extraction time enhanced or decreased antiradical activity in some cases. Additionally, important biologically active compounds in parsley leaves, such as vitamin C (248.31 mg/100 g dry matter), carotenoids (31.28 mg/100 g dry matter), chlorophyll (0.185 mg/g dry matter) were also analysed.

Isolation and characterization of potential antibiotic producing actinomycetes from water and sediments of Lake Tana, Ethiopia

PubMed Central

Gebreyohannes, Gebreselema; Moges, Feleke; Sahile, Samuel; Raja, Nagappan

2013-01-01

Objective To isolate, evaluate and characterize potential antibiotic producing actinomycetes from water and sediments of Lake Tana, Ethiopia. Methods A total of 31 strains of actinomycetes were isolated and tested against Gram positive and Gram negative bacterial strains by primary screening. In the primary screening, 11 promising isolates were identified and subjected to solid state and submerged state fermentation methods to produce crude extracts. The fermented biomass was extracted by organic solvent extraction method and tested against bacterial strains by disc and agar well diffusion methods. The isolates were characterized by using morphological, physiological and biochemical methods. Results The result obtained from agar well diffusion method was better than disc diffusion method. The crude extract showed higher inhibition zone against Gram positive bacteria than Gram negative bacteria. One-way analysis of variance confirmed most of the crude extracts were statistically significant at 95% confidence interval. The minimum inhibitory concentration and minimum bactericidal concentration of crude extracts were 1.65 mg/mL and 3.30 mg/mL against Staphylococcus aureus, and 1.84 mg/mL and 3.80 mg/mL against Escherichia coli respectively. The growth of aerial and substrate mycelium varied in different culture media used. Most of the isolates were able to hydrolysis starch and urea; able to survive at 5% concentration of sodium chloride; optimum temperature for their growth was 30 °C. Conclusions The results of the present study revealed that freshwater actinomycetes of Lake Tana appear to have immense potential as a source of antibacterial compounds. PMID:23730554

Stable and accurate methods for identification of water bodies from Landsat series imagery using meta-heuristic algorithms

NASA Astrophysics Data System (ADS)

Gamshadzaei, Mohammad Hossein; Rahimzadegan, Majid

2017-10-01

Identification of water extents in Landsat images is challenging due to surfaces with similar reflectance to water extents. The objective of this study is to provide stable and accurate methods for identifying water extents in Landsat images based on meta-heuristic algorithms. Then, seven Landsat images were selected from various environmental regions in Iran. Training of the algorithms was performed using 40 water pixels and 40 nonwater pixels in operational land imager images of Chitgar Lake (one of the study regions). Moreover, high-resolution images from Google Earth were digitized to evaluate the results. Two approaches were considered: index-based and artificial intelligence (AI) algorithms. In the first approach, nine common water spectral indices were investigated. AI algorithms were utilized to acquire coefficients of optimal band combinations to extract water extents. Among the AI algorithms, the artificial neural network algorithm and also the ant colony optimization, genetic algorithm, and particle swarm optimization (PSO) meta-heuristic algorithms were implemented. Index-based methods represented different performances in various regions. Among AI methods, PSO had the best performance with average overall accuracy and kappa coefficient of 93% and 98%, respectively. The results indicated the applicability of acquired band combinations to extract accurately and stably water extents in Landsat imagery.

Efficient screening method for determination of polycyclic aromatic hydrocarbons (PAHs) in airborne particles. Application in real samples of Santiago-Chile metropolitan urban area

NASA Astrophysics Data System (ADS)

Romero, Rodrigo; Sienra, Rosario; Richter, Pablo

A rapid analytical approach for determination of polycyclic aromatic hydrocarbons (PAHs) present in real samples of particulate matter (PM10 filters) was investigated, based on the use of water under sub critical conditions, and the subsequent determination by GC-MS (SIM). The method avoids the use of large volumes of organic solvents as dichloromethane, toluene or other unhealthy liquid organic mixtures which are normally used in time-consuming conventional sample preparation methods. By using leaching times <1 h, the method allows determination of PAHs in the range of ng/m 3 (detection limits between 0.05 and 0.2 ng/m 3 for 1458 m 3 of sampled air) with a precision expressed as RSD between 5.6% and 11.2%. The main idea behind this approach is to raise the temperature and pressure of water inside a miniaturized laboratory-made extraction unit and to decrease its dielectric constant from 80 to nearly 20. This effect allows an increase in the solubility of low polarity hydrocarbons such as PAHs. In this way, an extraction step of a few minutes can be sufficient for a quantitative extraction of airborne particles collected in high volume PM10 samplers. Parameters such as: extraction flow, static or dynamic extraction times and water volume were optimized by using a standard reference material. Technical details are given and a comparison using real samples is made between the conventional Soxhlet extraction method and the proposed approach. The proposed approach can be used as a quantitative method to characterize low molecular PAHs and simultaneously as a screening method for high molecular weight PAHs, because the recoveries are not quantitative for molecular weights over 202. In the specific case of the Santiago metropolitan area, due to the frequent occurrence of particulate matter during high pollution episodes, this approach was applied as an efficient short-time screening method for urban PAHs. Application of this screening method is recommended especially during the winter, when periods of clear detriment of the atmospheric and meteorological conditions occur in the area.

Polyaniline/cyclodextrin composite coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the analysis of trace polychlorinated biphenyls in environmental waters.

PubMed

Lei, Yun; He, Man; Chen, Beibei; Hu, Bin

2016-04-01

A novel polyaniline/α-cyclodextrin (PANI/α-CD) composite coated stir bar was prepared by sol-gel process for the analysis of polychlorinated biphenyls (PCBs) in this work. The preparation reproducibility of the PANI/α-CD-coated stir bar was good, with relative standard deviations (RSDs) ranging from 2.3% to 3.7% (n=7) and 2.0% to 3.8% (n=7) for bar to bar and batch to batch, respectively. Based on it, a novel method of PANI/α-CD-coated stir bar sorptive extraction (SBSE) followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for the determination of trace PCBs in environmental waters. To obtain the best extraction performance for target PCBs, several parameters affecting SBSE, such as extraction time, stirring rate, and ionic strength were investigated. Under optimal experimental conditions, the limits of detection (LODs) of the proposed method for seven PCBs were in the range of 0.048-0.22 μg/L, and the RSDs were 5.3-9.8% (n=7, c=1 μg/L). Enrichment factors (EFs) ranging from 39.8 to 68.4-fold (theoretical EF, 83.3-fold) for target analytes were achieved. The proposed method was successfully applied for the determination of seven target PCBs in Yangtze River water and East Lake water, and the recoveries were in the range of 73.0-120% for the spiked East Lake water samples and 82.7-121% for the spiked Yangtze River water samples, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Antihyperglycemic action of rhodiola-aqeous extract in type1-like diabetic rats

PubMed Central

2014-01-01

Background Rhodiola rosea (Rhodiola) is a plant in the Crassulaceae family that grows in cold regions of the world. It is mainly used in clinics as an adaptogen. Recently, it has been mentioned that Rhodiola increases plasma β-endorphin to lower blood pressure. Thus, the present study aims to investigate the antidiabetic action of Rhodiola in relation to opioids in streptozotocin-induced diabetic rats (STZ-diabetic rats). Methods In the present study, the plasma glucose was analyzed with glucose oxidase method, and the determination of plasma β-endorphin was carried out using a commercially available enzyme-linked immunosorbent assay. The adrenalectomy of STZ-diabetic rats was used to evaluate the role of β-endorphin. In addition, quantitative reverse transcription-polymerase chain reaction (qRT-PCR) and western blotting analysis were performed to investigate mRNA and protein expressions. Results Rhodiola-water extract dose-dependently lowered the plasma glucose in STZ-diabetic rats and this action was reversed by blockade of opioid μ-receptors using cyprodime. An increase of plasma β-endorphin by rhodiola-water extract was also observed in same manner. The plasma glucose lowering action of rhodiola-water extract was attenuated in bilateral adrenalectomized rats. In addition, continuous administration of rhodiola-water extract for 3 days in STZ-diabetic rats resulted in an increased expression of glucose transporter subtype 4 (GLUT 4) in skeletal muscle and a marked reduction of phosphoenolpyruvate carboxykinase (PEPCK) expression in liver. These effects were also reversed by blockade of opioid μ-receptors. Conclusions Taken together, rhodiola-water extract improves hyperglycemia via an increase of β-endorphin secretion from adrenal gland to activate opioid μ-receptors in STZ-diabetic rats. PMID:24417880

Simultaneous Determination of 13 Priority Polycyclic Aromatic Hydrocarbons in Tehran’s Tap Water and Water for Injection Samples Using Dispersive Liquid-Liquid Micro Extraction Method and Gas Chromatography-Mass Spectrometry

PubMed Central

Sadeghi, Ramezan; Kobarfard, Farzad; Yazdanpanah, Hassan; Eslamizad, Samira; Bayate, Mitra

2016-01-01

Polycyclic aromatic hydrocarbons (PAHs) are classified as persistent and carcinogenic organic pollutants. PAHs contamination has been reported in water. Many of relevant regulatory bodies such as EU and EPA have regulated the limit levels for PAHs in drinking water. In this study, 13 priority polycyclic aromatic hydrocarbons (PAHs) were determined in tap water samples of Tehran and water for injection. Dispersive liquid-liquid microextraction procedure combined with gas chromatography-mass spectrometry was used for the extraction and determination of PAHs in the samples. Under the optimized conditions, the range of extraction recoveries and relative standard deviations (RSDs) of PAHs in water using internal standard (anthracene-d10) were in the range of 71-90% and 4-16%, respectively. Limit of detection for different PAHs were between 0.03 and 0.1 ngmL-1. The concentration of PAHs in all tap water as well as water for injection samples were lower than the limit of quantification of PAHs. This is the first study addressing the occurrence of PAHs in water for injection samples in Iran using dispersive liquid-liquid micro extraction procedure combined with gas chromatography-mass spectrometry. PMID:27642318

Optimization of extraction of polysaccharides from fruiting body of Cordyceps militaris (L.) link using response surface methodology

NASA Astrophysics Data System (ADS)

Nguyen, Hoang Chinh; Thi, Dinh Huynh Mong; Pham, Dinh Chuong

2018-04-01

Polysaccharides from fruiting body of Cordyceps militaris (L.) Link possess various pharmaceutical activities. In this study, polysaccharides from the fruiting body of C. militaris were extracted with different solvents. Of those solvents tested, distilled water was identified as the most efficient solvent for the extraction, resulting in a significant increase in polysaccharides yield. Response surface methodology was then used to optimize the extraction conditions and establish a reliable mathematical model for prediction. A maximum polysaccharides yield of 11.07% was reached at a ratio of water to raw material of 23.2:1 mL/g, an extraction time of 76 min, and a temperature of 93.6°C. This study indicates that the obtained optimal extraction conditions are an efficient method for extraction of polysaccharides from the fruiting body of C. militaris.

Anti-inflammatory effect of bee pollen ethanol extract from Cistus sp. of Spanish on carrageenan-induced rat hind paw edema

PubMed Central

2010-01-01

Background Bee pollen, a honeybee product, is the feed for honeybees prepared themselves by pollens collecting from plants and has been consumed as a perfect food in Europe, because it is nutritionally well balanced. In this study, we aimed to investigate the anti-inflammatory effect of bee pollen from Cistus sp. of Spanish origin by a method of carrageenan-induced paw edema in rats, and to investigate the mechanism of anti-inflammatory action and also to elucidate components involved in bee pollen extracted with ethanol. Methods The bee pollen bulk, its water extract and its ethanol extract were administered orally to rats. One hour later, paw edema was produced by injecting of 1% solution of carrageenan, and paw volume was measured before and after carrageenan injection up to 5 h. The ethanol extract and water extract were measured COX-1 and COX-2 inhibitory activities using COX inhibitor screening assay kit, and were compared for the inhibition of NO production in LPS-stimulated RAW 264.7 cells. The constituents of bee pollen were purified from the ethanol extract subjected to silica gel or LH-20 column chromatography. Each column chromatography fractions were further purified by repeated ODS or silica gel column chromatography. Results The bee pollen bulk mildly suppressed the carrageenan-induced paw edema and the water extract showed almost no inhibitory activity, but the ethanol extract showed relatively strong inhibition of paw edema. The ethanol extract inhibited the NO production and COX-2 but not COX-1 activity, but the water extract did not affect the NO production or COX activities. Flavonoids were isolated and purified from the ethanol extract of bee pollen, and identified at least five flavonoids and their glycosides. Conclusions It is suggested that the ethanol extract of bee pollen show a potent anti-inflammatory activity and its effect acts via the inhibition of NO production, besides the inhibitory activity of COX-2. Some flavonoids included in bee pollen may partly participate in some of the anti-inflammatory action. The bee pollen would be beneficial not only as a dietary supplement but also as a functional food. PMID:20573205

Switchable hydrophilicity solvents for lipid extraction from microalgae for biofuel production.

PubMed

Boyd, Alaina R; Champagne, Pascale; McGinn, Patrick J; MacDougall, Karen M; Melanson, Jeremy E; Jessop, Philip G

2012-08-01

A switchable hydrophilicity solvent (SHS) was studied for its effectiveness at extracting lipids from freeze-dried samples of Botryococcus braunii microalgae. The SHS N,N-dimethylcyclohexylamine extracted up to 22 wt.% crude lipid relative to the freeze-dried cell weight. The solvent was removed from the extract with water saturated with carbon dioxide at atmospheric pressure and recovered from the water upon de-carbonation of the mixture. Liquid chromatography-mass spectrometry (LC-MS) showed that the extracted lipids contained high concentrations of long chain tri-, di- and mono-acylglycerols, no phospholipids, and only 4-8% of residual solvent. Unlike extractions with conventional organic solvents, this new method requires neither distillation nor the use of volatile, flammable or chlorinated organic solvents. Copyright © 2012 Elsevier Ltd. All rights reserved.

Extracting cross sections and water levels of vegetated ditches from LiDAR point clouds

NASA Astrophysics Data System (ADS)

Roelens, Jennifer; Dondeyne, Stefaan; Van Orshoven, Jos; Diels, Jan

2016-12-01

The hydrologic response of a catchment is sensitive to the morphology of the drainage network. Dimensions of bigger channels are usually well known, however, geometrical data for man-made ditches is often missing as there are many and small. Aerial LiDAR data offers the possibility to extract these small geometrical features. Analysing the three-dimensional point clouds directly will maintain the highest degree of information. A longitudinal and cross-sectional buffer were used to extract the cross-sectional profile points from the LiDAR point cloud. The profile was represented by spline functions fitted through the minimum envelop of the extracted points. The cross-sectional ditch profiles were classified for the presence of water and vegetation based on the normalized difference water index and the spatial characteristics of the points along the profile. The normalized difference water index was created using the RGB and intensity data coupled to the LiDAR points. The mean vertical deviation of 0.14 m found between the extracted and reference cross sections could mainly be attributed to the occurrence of water and partly to vegetation on the banks. In contrast to the cross-sectional area, the extracted width was not influenced by the environment (coefficient of determination R2 = 0.87). Water and vegetation influenced the extracted ditch characteristics, but the proposed method is still robust and therefore facilitates input data acquisition and improves accuracy of spatially explicit hydrological models.

Determination of Wastewater Compounds in Whole Water by Continuous Liquid-Liquid Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.

2006-01-01

A method for the determination of 69 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals on aquatic organisms in wastewater. This method also is useful for evaluating the effects of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are indicators of wastewater or have endocrine-disrupting potential. These compounds include the alkylphenol ethoxylate nonionic surfactants, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Wastewater compounds in whole-water samples were extracted using continuous liquid-liquid extractors and methylene chloride solvent, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 0.5 microgram per liter averaged 72 percent ? 8 percent relative standard deviation. The concentration of 21 compounds is always reported as estimated because method recovery was less than 60 percent, variability was greater than 25 percent relative standard deviation, or standard reference compounds were prepared from technical mixtures. Initial method detection limits averaged 0.18 microgram per liter. Samples were preserved by adding 60 grams of sodium chloride and stored at 4 degrees Celsius. The laboratory established a sample holding-time limit prior to sample extraction of 14 days from the date of collection.

Application of NaClO-treated multiwalled carbon nanotubes as solid phase extraction sorbents for preconcentration of trace 2,4-dichlorophenoxyacetic acid in aqueous samples.

PubMed

Lu, Ping; Deng, Dayi; Ni, Xiaodan

2012-09-01

Multiwalled carbon nanotubes functionalized by oxidation of original multiwalled carbon nanotubes with NaClO were prepared and their application as solid phase extraction sorbent for 2,4-dichlorophenoxyacetic acid (2,4-D) was investigated systemically, and a new method was developed for the determination of trace 2,4-D in water samples based on extraction and preconcentration of 2,4-D with solid phase extraction columns packed with NaClO-treated multiwalled carbon nanotubes prior to its determination by HPLC. The optimum experimental parameters for preconcentration of 2,4-D, including the column activating conditions, the amount of the sorbent, pH of the sample, elution composition, and elution volume, were investigated. The results indicated 2,4-D could be quantitatively retained by 100 mg NaClO-treated multiwalled carbon nanotubes at pH 5, and then eluted completely with 10 mL 3:1 (v/v) methanol-ammonium acetate solution (0.3 mol/L). The detection limit of this method for 2,4-D was 0.15 μg/L, and the relative standard deviation was 2.3% for fortified tap water samples and 2.5% for fortified riverine water sample at the 10 μg/L level. The method was validated using fortified tap water and riverine water samples with known amount of 2,4-D at the 0.4, 10, and 30 μg/L levels, respectively. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of C₁₈-functionalized magnetic polydopamine microspheres for the enrichment and analysis of alkylphenols in water samples.

PubMed

Wang, Xianying; Deng, Chunhui

2016-02-01

In this work, C18-functionalized magnetic polydopamine microspheres (Fe3O4@PDA@C18) were successfully synthesized and applied to the analysis of alkylphenols in water samples. The magnetic Fe3O4 particles coated with hydrophilic surface were synthesized via a solvothermal reaction and the self-polymerization of dopamine. And then the C18 groups were fabricated by a silylanization method. Benefit from the merits of Fe3O4 particles, polydopamine coating and C18 groups, the Fe3O4@PDA@C18 material possessed several properties of super magnetic responsiviness, good water dispersibility, π-electron system and hydrophobic C18 groups. Thus, the materials had great potential to be developed as the adsorbent for the magnetic solid-phase extraction (MSPE) technique. Here, we selected three kinds of alkylphenols (4-tert-octylphenol, 4-n-nonylphenol, 4-n-octylphenol) to be the target analyst for evaluating the performance of the prepared material. In this study, various extraction parameters were investigated and optimized, such as pH values of water sample solution, amount of adsorbents, adsorption and desorption time, the species of desorption solution. Meanwhile, the method validations were studied, including linearity, limit of detection and method precision. From the results, Fe3O4@PDA@C18 composites were successfully applied as the adsorbents for the extraction of alkylphenols in water samples. The proposed material provided an approach for a simple, rapid magnetic solid-phase extraction for hydrophobic compounds in environmental samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparison of pore water samplers and cryogenic distillation under laboratory and field conditions for soil water stable isotope analysis.

PubMed

Thoma, Michael; Frentress, Jay; Tagliavini, Massimo; Scandellari, Francesca

2018-02-15

We used pore water samplers (PWS) to sample for isotope analysis (1) only water, (2) soil under laboratory conditions, and (3) soil in the field comparing the results with cryogenic extraction (CE). In (1) and (2), no significant differences between source and water extracted with PWS were detected with a mean absolute difference (MAD) always lower than 2 ‰ for δ 2 H and 1 ‰ for δ 18 O. In (2), CE water was more enriched than PWS-extracted water, with a MAD respect to source water of roughly 8 ‰ for δ 2 H and 4 ‰ for δ 18 O. In (3), PWS water was enriched relative to CE water by 3 ‰ for δ 2 H and 0.9 ‰ for δ 18 O. The latter result may be due to the distinct water portions sampled by the two methods. Large pores, easily sampled by PWS, likely retain recent, and enriched, summer precipitation while small pores, only sampled by CE, possibly retain isotopically depleted water from previous winter precipitation or irrigation inputs. Accuracy and precision were greater for PWS relative to CE. PWS is therefore suggested as viable tool to extract soil water for stable isotope analysis, particularly for soils used in this study (sandy and silty loams).

[Analysis of sulfonamids and their metabolites in drinking water by high Performance liquid chromatography tandem mass spectrometry].

PubMed

Wang, Shuo; Li, Shuming; Zhang, Xiangming; Wei, Yunfang; Zhang, Meiyun; Zhang, Jing

2015-07-01

To develop a comprehensive method for simultaneous analysis of sulfonamides and their metabolites in drinking water by high performance liquid chromatography tandem mass spectrometry (LC-MS/MS). Different solid-phase extraction columns were compared with respect to the recovery of target drugs from drinking water. The drinking water samples were adjusted to 3 by HCl and purified by a mix mode cation-ion exchange solid-phase extraction (SPE), following determination using LG-MS/MS. A total of 21 sulfonamides were separated by a C15 column (2.1 mm x 100 mm, 1.7 µm) and analyzed under positive ion mode with multi-reaction monitoring. The matrix-matched external standard calibration was used for quantification. The method quantification limits for 21 analytes were 0.03-0.63 ng/L with overall recoveries of 50.1%-114.9%, and the relative standard deviations less than 20%. The method was finally used to analyze sulfonamides in drinking water in Beijing, and 5 target compounds (sulfadiazine, sulfathiazole, sulfapyridine, trimethoprim and sulfamethazine) were detected at a concentration range of 0.08-32.54 ng/L. This method could be applied in simultaneous analysis of sulfonamides and their metabolites in drinking water samples.

Trace analysis of trimethoprim and sulfonamide, macrolide, quinolone, and tetracycline antibiotics in chlorinated drinking water using liquid chromatography electrospray tandem mass spectrometry

USGS Publications Warehouse

Ye, Z.; Weinberg, H.S.; Meyer, M.T.

2007-01-01

A multirun analytical method has been developed and validated for trace determination of 24 antibiotics including 7 sulfonamides, 3 macrolides, 7 quinolones, 6 tetracyclines, and trimethoprim in chlorine-disinfected drinking water using a single solid-phase extraction method coupled to liquid chromatography with positive electrospray tandem mass spectrometry detection. The analytes were extracted by a hydrophilic-lipophilic balanced resin and eluted with acidified methanol (0.1% formic acid), resulting in analyte recoveries generally above 90%. The limits of quantitation were mostly below 10 ng/L in drinking water. Since the concentrated sample matrix typically caused ion suppression during electrospray ionization, the method of standard addition was used for quantitation. Chlorine residuals in drinking water can react with some antibiotics, but ascorbic acid was found to be an effective chlorine quenching agent without affecting the analysis and stability of the antibiotics in water. A preliminary occurrence study using this method revealed the presence of some antibiotics in drinking waters, including sulfamethoxazole (3.0-3.4 ng/L), macrolides (1.4-4.9 ng/L), and quinolones (1.2-4.0 ng/L). ?? 2007 American Chemical Society.

Multi-residue analysis method for analysis of pharmaceuticals using liquid chromatography-time of flight/mass spectrometry (LC-TOF/MS) in water sample

NASA Astrophysics Data System (ADS)

Al-Qaim, Fouad Fadhil; Abdullah, Md Pauzi; Othman, Mohamed Rozali

2013-11-01

In this work, a developed method using solid - phase extraction (SPE) followed by liquid chromatography - time of flight mass spectrometry (LC-ESI-TOF/MS) was developed and validated for quantification and confirmation of eleven pharmaceuticals with different therapeutic classes in water samples, Malaysia. These compounds are caffeine (CAF), prazosin (PRZ), enalapril (ENL), carbamazepine (CBZ), nifedipine (NFD), levonorgestrel (LNG), simvastatin (SMV), hydrochlorothiazide (HYD), gliclazide (GLIC), diclofenac-Na (DIC-Na) and mefenamic acid (MEF). LC was performed on a Dionex Ultimate 3000/LC 09115047 (USA) system. Chromatography was performed on a Thermo Scientific C18 (250 mm × 2.1 mm, i.d.: 5μm) column. Several parameters were optimised such as; mobile phase, gradient elution, collision energy and solvent elution for extraction of compounds from water. The recoveries obtained ranged from 30-148 % in river water. Five pharmaceutical compounds were detected in the surface water samples: caffeine, prazosin, enalpril, diclofenac-Na and mefenamic acid. The developed method is precise and accepted recoveries were got. In addition, this method is suitable to identify and quantify trace concentrations of pharmaceuticals in surface water.

Determination of azoxystrobin and chlorothalonil using a methacrylate-based polymer modified with gold nanoparticles as solid-phase extraction sorbent.

PubMed

Catalá-Icardo, Mónica; Gómez-Benito, Carmen; Simó-Alfonso, Ernesto Francisco; Herrero-Martínez, José Manuel

2017-01-01

This paper describes a novel and sensitive method for extraction, preconcentration, and determination of two important widely used fungicides, azoxystrobin, and chlorothalonil. The developed methodology is based on solid-phase extraction (SPE) using a polymeric material functionalized with gold nanoparticles (AuNPs) as sorbent followed by high-performance liquid chromatography (HPLC) with diode array detector (DAD). Several experimental variables that affect the extraction efficiency such as the eluent volume, sample flow rate, and salt addition were optimized. Under the optimal conditions, the sorbent provided satisfactory enrichment efficiency for both fungicides, high selectivity and excellent reusability (>120 re-uses). The proposed method allowed the detection of 0.05 μg L -1 of the fungicides and gave satisfactory recoveries (75-95 %) when it was applied to drinking and environmental water samples (river, well, tap, irrigation, spring, and sea waters).

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.

Experimental and molecular docking investigation on metal-organic framework MIL-101(Cr) as a sorbent for vortex assisted dispersive micro-solid-phase extraction of trace 5-nitroimidazole residues in environmental water samples prior to UPLC-MS/MS analysis.

PubMed

Lu, Nan; Wang, Ting; Zhao, Pan; Zhang, Lianjun; Lun, Xiaowen; Zhang, Xueli; Hou, Xiaohong

2016-11-01

In the presented work, metal-organic framework (MOF) material MIL-101(Cr) (MIL, Matérial Institute Lavoisier) was used as a sorbent for vortex assisted dispersive micro-solid-phase extraction (VA-D-μ-SPE) of trace amount of metronidazole (MNZ), ronidazole (RNZ), secnidazole (SNZ), dimetridazole (DMZ), tinidazole (TNZ), and ornidazole (ONZ) in different environmental water samples. Ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was used to quantify the target analytes. The extraction conditions, including type of sorbents, amount of MIL-101(Cr), solution pH, extraction method, extraction time, effect of salt, and elution conditions were investigated. Upon the optimal conditions, the developed method showed an excellent extraction performance with the average recovery ranging from 75.2 to 98.8 %. Good sensitivity levels were achieved with the detection limits of 0.03∼0.06 μg/L and the quantitation limits of 0.09∼0.20 μg/L. The linear ranges were varied from 0.1 to 20 for SNZ and ONZ and from 0.2 to 40 μg/L for MNZ, RNZ, DMZ, and TNZ (r 2  > 0.992), and repeatability of the method was satisfactory with the relative standard deviations (RSD) <8 %. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of 5-nitroimidazoles (5-NDZs) in 12 real water samples, showing the positive findings of MNZ and TNZ ranging from 0.3 to 1.0 μg/L. Furthermore, molecular docking was applied to explain the molecular interactions and free binding energies between MIL-101(Cr) and 5-NDZs, providing a deep insight into the adsorption mechanism. The proposed method exhibited the advantages of simplicity, rapidly, less solvent consumption, ease of operation, higher sensitivity, and lower matrix effect. Graphical abstract Schematic diagram of the extraction process and molecular docking investigation.

Development of a new extraction method based on counter current salting-out homogenous liquid-liquid extraction followed by dispersive liquid-liquid microextraction: Application for the extraction and preconcentration of widely used pesticides from fruit juices.

PubMed

Farajzadeh, Mir Ali; Feriduni, Behruz; Mogaddam, Mohammad Reza Afshar

2016-01-01

In this paper, a new extraction method based on counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) followed by dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and preconcentration of widely used pesticides in fruit juice samples prior to their analysis by gas chromatography-flame ionization detection (GC-FID). In this method, initially, sodium chloride as a separation reagent is filled into a small column and a mixture of water (or fruit juice) and acetonitrile is passed through the column. By passing the mixture sodium chloride is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected organic phase (acetonitrile) is removed with a syringe and mixed with 1,1,2,2-tetrachloroethane (extraction solvent at µL level). In the second step, for further enrichment of the analytes the above mixture is injected into 5 mL de-ionized water placed in a test tube with conical bottom in order to dissolve acetonitrile into water and to achieve a sedimented phase at µL-level volume containing the enriched analytes. Under the optimal extraction conditions (extraction solvent, 1.5 mL acetonitrile; pH, 7; flow rate, 0.5 mL min(-1); preconcentration solvent, 20 µL 1,1,2,2-tetrachloroethane; NaCl concentration; 5%, w/w; and centrifugation rate and time, 5000 rpm and 5 min, respectively), the extraction recoveries and enrichment factors ranged from 87% to 96% and 544 to 600, respectively. Repeatability of the proposed method, expressed as relative standard deviations, ranged from 2% to 6% for intra-day (n=6, C=250 or 500 µg L(-1)) and inter-days (n=4, C=250 or 500 µg L(-1)) precisions. Limits of detection are obtained between 2 and 12 µg L(-1). Finally, the proposed method is applied for the determination of the target pesticide residues in the juice samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

Antioxidant activity of extracts from the bark of Chamaecyparis lawsoniana (A. Murrary) Parl.

Treesearch

Heng Gao; Todd F. Shupe; Chung Y. Hse; Thomas L. Eberhardt

2006-01-01

The bark of Chamaecyparis lawsoniana (A. Murray) Parl. was extracted with methanol and sequentially partitioned with n-hexane, ethyl acetate, n-butanol and deionized water. The antioxidant activities of the four extracts were evaluated using the DPPH• and ABTS+• methods. The total phenolic...

An On-Line Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of Perfluoroalkyl Acids in Drinking and Surface Waters

PubMed Central

Mazzoni, Michela; Rusconi, Marianna; Valsecchi, Sara; Martins, Claudia P. B.; Polesello, Stefano

2015-01-01

An UHPLC-MS/MS multiresidue method based on an on-line solid phase extraction (SPE) procedure was developed for the simultaneous determination of 9 perfluorinated carboxylates (from 4 to 12 carbon atoms) and 3 perfluorinated sulphonates (from 4 to 8 carbon atoms). This work proposes using an on-line solid phase extraction before chromatographic separation and analysis to replace traditional methods of off-line SPE before direct injection to LC-MS/MS. Manual sample preparation was reduced to sample centrifugation and acidification, thus eliminating several procedural errors and significantly reducing time-consuming and costs. Ionization suppression between target perfluorinated analytes and their coeluting SIL-IS were detected for homologues with a number of carbon atoms less than 9, but the quantitation was not affected. Total matrix effect corrected by SIL-IS, inclusive of extraction efficacy, and of ionization efficiency, ranged between −34 and +39%. The percentage of recoveries, between 76 and 134%, calculated in different matrices (tap water and rivers impacted by different pollutions) was generally satisfactory. LODs and LOQs of this on-line SPE method, which also incorporate recovery losses, ranged from 0.2 to 5.0 ng/L and from 1 to 20 ng/L, respectively. Validated on-line SPE-LC/MS/MS method has been applied in a wide survey for the determination of perfluoroalkyl acids in Italian surface and ground waters. PMID:25834752

Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

PubMed

Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

2015-12-24

A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). Copyright © 2015 Elsevier B.V. All rights reserved.

Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2006-07-11

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2002-01-01

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

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.

Development and Multi-laboratory Verification of U.S. EPA Method 540 for the Analysis of Drinking Water Contaminants by Solid Phase Extraction-LC/MS/MS

EPA Science Inventory

A drinking water method for 12 chemicals, predominately pesticides, is presented that addresses the occurrence monitoring needs of the U.S. Environmental Protection Agency (EPA) for a future Unregulated Contaminant Monitoring Regulation (UCMR). The method employs solid phase ext...

Development and Multi-laboratory Verification of US EPA Method 543 for the Analysis of Drinking Water Contaminants by Online Solid Phase Extraction-LC–MS-MS

EPA Science Inventory

A drinking water method for seven pesticides and pesticide degradates is presented that addresses the occurrence monitoring needs of the US Environmental Protection Agency (EPA) for a future Unregulated Contaminant Monitoring Regulation (UCMR). The method employs online solid pha...

Water Leakage Diagnosis in Metro Tunnels by Intergration of Laser Point Cloud and Infrared Thermal Imaging

NASA Astrophysics Data System (ADS)

Yu, P.; Wu, H.; Liu, C.; Xu, Z.

2018-04-01

Diagnosis of water leakage in metro tunnels is of great significance to the metro tunnel construction and the safety of metro operation. A method that integrates laser scanning and infrared thermal imaging is proposed for the diagnosis of water leakage. The diagnosis of water leakage in this paper is mainly divided into two parts: extraction of water leakage geometry information and extraction of water leakage attribute information. Firstly, the suspected water leakage is obtained by threshold segmentation based on the point cloud of tunnel. And the real water leakage is obtained by the auxiliary interpretation of infrared thermal images. Then, the characteristic of isotherm outline is expressed by solving Centroid Distance Function to determine the type of water leakage. Similarly, the location of leakage silt and the direction of crack are calculated by finding coordinates of feature points on Centroid Distance Function. Finally, a metro tunnel part in Shanghai was selected as the case area to make experiment and the result shown that the proposed method in this paper can be used to diagnosis water leakage disease completely and accurately.

Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry.

PubMed

Vidal, Lorena; Ahmadi, Mazaher; Fernández, Elena; Madrakian, Tayyebeh; Canals, Antonio

2017-06-08

This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L -1 for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L -1 for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L -1 for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L -1 and 50 ng L -1 spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L -1 . Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects. Copyright © 2017 Elsevier B.V. All rights reserved.

Extraction and demulsification of oil from wheat germ, barley germ, and rice bran using an aqueous enzymatic method

USDA-ARS?s Scientific Manuscript database

An aqueous enzymatic method was developed to extract oil from wheat germ. The parameters that influence oil yield were investigated, including wheat germ pretreatment, comparison of various industrial enzymes, pH, ratio of wheat germ to water, reaction time and demulsification. Pretreatment at 180ºC...

Solid-phase microextraction based on polyaniline doped with perfluorooctanesulfonic acid coupled to HPLC for the quantitative determination of chlorophenols in water samples.

PubMed

He, Huan; Zhuang, Yuan; Peng, Ying; Gao, Zhanqi; Yang, Shaogui; Sun, Cheng

2014-02-01

A porous and highly efficient polyaniline-based solid-phase microextraction (SPME) coating was successfully prepared by the electrochemical deposition method. A method based on headspace SPME followed by HPLC was established to rapidly determine trace chlorophenols in water samples. Influential parameters for the SPME, including extraction mode, extraction temperature and time, pH and ionic strength procedures, were investigated intensively. Under the optimized conditions, the proposed method was linear in the range of 0.5-200 μg/L for 4-chlorophenol and 2,4,6-trichlorophenol, 0.2-200 μg/L for 2,4-dichlorophenol and 2-200 μg/L for 2,3,4,6-tetrachlorophenol and pentachlorophenol, with satisfactory correlation coefficients (>0.99). RSDs were <15% (n = 5) and LODs were relatively low (0.10-0.50 μg/L). Compared to commercial 85 μm polyacrylate and 60 μm polydimethylsiloxane/divinylbenzene fibers, the homemade polyaniline fiber showed a higher extraction efficiency. The proposed method has been successfully applied to the determination of chlorophenols in water samples with satisfactory recoveries. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Packed in-tube solid phase microextraction with graphene oxide supported on aminopropyl silica: Determination of target triazines in water samples.

PubMed

De Toffoli, Ana L; Fumes, Bruno H; Lanças, Fernando M

2018-02-22

On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2-4.0 µg L -1 ) and low detection limits (1.1-2.9 ng L -1 ). The high extraction efficiency was determined with enrichment factors ranging from 1.2-2.9 for the lowest level, 1.3-4.9 intermediate level and 1.2-3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.

Sorptive extraction using polydimethylsiloxane/metal-organic framework coated stir bars coupled with high performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

PubMed

Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

2014-08-22

In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Online in-tube microextractor coupled with UV-Vis spectrophotometer for bisphenol A detection.

PubMed

Poorahong, Sujittra; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

2013-01-01

A simple and high extraction efficiency online in-tube microextractor (ITME) was developed for bisphenol A (BPA) detection in water samples. The ITME was fabricated by a stepwise electrodeposition of polyaniline, polyethylene glycol and polydimethylsiloxane composite (CPANI) inside a silico-steel tube. The obtained ITME coupled with UV-Vis detection at 278 nm was investigated. By this method, the extraction and pre-concentration of BPA in water were carried out in a single step. Under optimum conditions, the system provided a linear dynamic range of 0.1 to 100 μM with a limit of detection of 20 nM (S/N ≥3). A single in-tube microextractor had a good stability of more than 60 consecutive injections for 10.0 μM BPA with a relative standard deviation of less than 4%. Moreover, a good tube-to-tube reproducibility and precision were obtained. The system was applied to detect BPA in water samples from six brands of baby bottles and the results showed good agreement with those obtained from the conventional GC-MS method. Acceptable percentage recoveries from the spiked water samples were obtained, ranging from 83-102% for this new method compared with 73-107% for the GC-MS standard method. This new in-tube CPANI microextractor provided an excellent extraction efficiency and a good reproducibility. In addition, it can also be easily applied for the analysis of other polar organic compounds contaminated in water sample.

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.

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments NAC/SETAC 2012

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments (SETAC Europe 22nd Annual Meeting)

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Phytomedical investigation of Najas minor All. in the view of the chemical constituents

PubMed Central

Topuzovic, Marina D.; Radojevic, Ivana D.; Dekic, Milan S.; Radulovic, Niko S.; Vasic, Sava M.; Comic, Ljiljana R.; Licina, Braho Z.

2015-01-01

Plants are an abundant natural source of effective antibiotic compounds. Phytomedical investigations of certain plants haven't still been conducted. One of them is Najas minor (N. minor), an aquatic plant with confirmed allelopathy. Research conducted in this study showed the influence of water and ethyl acetate extracts of N. minor on microorganisms, in the view of chemical profiling of volatile constituents and the concentrations of total phenols, flavonoids and tannins. Antimicrobial activity was defined by determining minimum inhibitory and minimum microbicidal concentrations using microdilution method. Influence on bacterial biofilm formation was performed by tissue culture plate method. The total phenolics, flavonoids and condensed tannins were determined by Folin-Ciocalteu, aluminum chloride and butanol-HCl colorimetric methods. Chemical profiling of volatile constituents was investigated by GC and GC-MS. Water extract didn't have antimicrobial activity below 5000 µg/mL. Ethyl acetate extract has shown strong antimicrobial activity on G+ bacteria - Staphylococcus aureus PMFKGB12 and Bacillus subtilis (MIC < 78.13 µg/mL). The best antibiofilm activity was obtained on Escherichia coli ATCC25922 (BIC50 at 719 µg/mL). Water extract had higher yield. Ethyl acetate extract had a significantly greater amount of total phenolics, flavonoids and tannins. As major constituent hexahydrofarnesyl acetone was identified. The ethyl acetate extract effected only G+ bacteria, but the biofilm formation of G-bacteria was suppressed. There was a connection between those in vivo and in vitro effects against pathogenic bacterial biofilm formation. All of this points to a so far unexplored potential of N. minor. PMID:26535038

Optimization of ultrasound-assisted aqueous two-phase system extraction of polyphenolic compounds from Aronia melanocarpa pomace by response surface methodology.

PubMed

Xu, Yan-Yang; Qiu, Yang; Ren, Hui; Ju, Dong-Hu; Jia, Hong-Lei

2017-03-16

Aronia melanocarpa berries are abundant in polyphenolic compounds. After juice production, the pomace of pressed berries still contains a substantial amount of polyphenolic compounds. For efficient utilization of A. melanocarpa berries and the enhancement of polyphenolic compound yields in Aronia melanocarpa pomace (AMP), total phenolics (TP) and total flavonoids (TF) from AMP were extracted, using ultrasound-assisted aqueous two-phase system (UAE-ATPS) extraction method. First, the influences of ammonium sulfate concentration, ethanol-water ratio, ultrasonic time, and ultrasonic power on TP and TF yields were investigated. On this basis, process variables such as ammonium sulfate concentration (0.30-0.35 g mL -1 ), ethanol-water ratio (0.6-0.8), ultrasonic time (40-60 min), and ultrasonic power (175-225 W) were further optimized by implementing Box-Benhnken design with response surface methodology. The experimental results showed that optimal extraction conditions of TP from AMP were as follows: ammonium sulfate concentration of 0.324 g mL -1 , ethanol-water ratio of 0.69, ultrasonic time of 52 min, and ultrasonic power of 200 W. Meanwhile, ammonium sulfate concentration of 0.320 g mL -1 , ethanol-water ratio of 0.71, ultrasonic time of 50 min, and ultrasonic power of 200 W were determined as optimum extraction conditions of TF in AMP. Experimental validation was performed, where TP and TF yields reached 68.15 ± 1.04 and 11.67 ± 0.63 mg g -1 , respectively. Close agreement was found between experimental and predicted values. Overall, the present results demonstrated that ultrasound-assisted aqueous two-phase system extraction method was successfully used to extract total phenolics and flavonoids in A. melanocarpa pomace.

Antioxidant properties of aqueous and ethanolic extracts of tara (Caesalpinia spinosa) pods in vitro and in model food emulsions.

PubMed

Skowyra, Monika; Falguera, Víctor; Gallego, Gabriela; Peiró, Sara; Almajano, María Pilar

2014-03-30

The successful replacement of some synthetic food antioxidants by safe natural antioxidants has fostered intensive search for new vegetable sources of antioxidants. In our study the phenol and flavonoid content of extracts of tara pods was determined. The antioxidant activity was also studied by three different analytical assays: the measurement of scavenging capacity against a radical ABTS⁺ , the oxygen radical absorbance capacity (ORAC) and the ferric reducing antioxidant power (FRAP). All analyzed samples showed a good antioxidant capacity, but the use of a solution of ethanol 75% in a 1 h ultrasonic process allowed achieving the greatest quantity of phenolics (0.464 mg gallic acid equivalent (GAE) g⁻¹ dry weight (DW) ) and the highest antioxidant activity measured by the ABTS⁺ and ORAC methods (10.17 and 4.29 mmol L⁻¹ Trolox equivalents (TE) g⁻¹ DW, respectively). The best method for efficient extraction of flavonoids (3.08 mg catechin equivalent (CE) g⁻¹ DW) was a 24 h maceration in cold water. Two extracts obtained with ethanol 75% and water were added to a model food system (oil-in-water emulsion) and the oxidative stability was studied during storage at 38 °C. Oxidation was monitored by determination of the peroxide value. The addition of 48 µg mL⁻¹ ethanol extract to the emulsion delayed oxidation to the same extent as 17.8 µg mL⁻¹ of Trolox, while water extract was only effective in the early stages of the oxidation process. The results of this study indicate that ethanolic tara extracts may be suitable for use in food, cosmetic and nutraceutical applications. © 2013 Society of Chemical Industry.

A chemical extraction method for mimicking bioavailability of polycyclic aromatic hydrocarbons to wheat grown in soils containing various amounts of organic matter

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

Shu Tao; Fuliu Xu; Wenxin Liu

Severe contamination of agricultural soils by polycyclic aromatic hydrocarbons (PAHs) occurs in many places in China mainly as a result of coal and biomass combustion. Because ingestion is the main source of human exposure to PAHs and vegetables are basic ingredients for the Chinese diet, it is important to know how and to what extent PAHs are accumulated in vegetables produced in contaminated soils. This study, evaluated the extent to which organic matter contents in soils influence the accumulation of PAHs by the roots of wheat plants and have developed a rapid chemical method for determining the bioavailability of PAH.more » Four PAHs, naphthalene, acenaphthylene, fluorene, and phenanthrene, were added to natural soil samples with different amounts of organic matter for pot experiments to evaluate apparent bioavailability of PAHs to wheat roots (Triticum aestivum L.). The extractabilities of PAHs in the soil were tested by a sequential extraction scheme using accelerated solvent extraction with water, n-hexane, and a mixture of dichloromethane and acetone as solvents. The water or n-hexane-extractable PAHs were positively correlated to dissolved organic matter (DOM) and negatively correlated to total organic matter (TOM), indicating mobilization and immobilization effects of DOM and TOM on soil PAHs, respectively. The apparent accumulation of PAHs by wheat roots was also positively and negatively correlated to DOM and TOM, respectively. As a result, there are positive correlations between the amounts of PAHs extracted by water or n-hexane and the quantities accumulated in plant roots, suggesting the feasibility of using water- or n-hexanes-extractable fractions as indicators of PAH availability to plants. 19 refs., 8 figs., 1 tab.« less

PFOS and PFOS: Analytics | Science Inventory | US EPA

EPA Pesticide Factsheets

This presentation describes the drivers for development of Method 537, the extraction and analytical procedure, performance data, holding time data as well as detection limits. The purpose of this presentation is to provide an overview of EPA drinking water Method 537 to the U.S. EPA Drinking Water Workshop participants.

Comparison of micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction and modified quick, easy, cheap, effective, rugged, and safe method for the determination of difenoconazole in cowpea.

PubMed

Chen, Xiaochu; Bian, Yanli; Liu, Fengmao; Teng, Peipei; Sun, Pan

2017-10-06

Two simple sample pretreatment for the determination of difenoconazole in cowpea was developed including micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction (ME-IL-VALLME) prior to high performance liquid chromatography (HPLC), and modified quick, easy, cheap, effective, rugged, and safe method (QuEChERS) coupled with HPLC-MS/MS. In ME-IL-VALLME method, the target analyte was extracted by surfactant Tween 20 micellar solution, then the supernatant was diluted with 3mL water to decrease the solubility of micellar solution. Subsequently, the vortex-assisted liquid-liquid microextraction (VALLME) procedure was performed in the diluted extraction solution by using the ionic liquid of 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIM]PF 6 ) as the extraction solvent and Tween 20 as an emulsifier to enhance the dispersion of the water-immiscible ionic liquid into the aqueous phase. Parameters that affect the extraction have been investigated in both methods Under the optimum conditions, the limits of quantitation were 0.10 and 0.05mgkg -1 , respectively. And good linearity was achieved with the correlation coefficient higher than 0.9941. The relative recoveries ranged from 78.6 to 94.8% and 92.0 to 118.0% with the relative standard deviations (RSD) of 7.9-9.6% and 1.2-3.2%, respectively. Both methods were quick, simple and inexpensive. However, the ME-IL-VALLME method provides higher enrichment factor compared with conventional QuEChERS method. The ME-IL-VALLME method has a strong potential for the determination of difenoconazole in complex vegetable matrices with HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of macrolide antibiotics in water by magnetic solid-phase extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Pérez, Rosa Ana; Albero, Beatriz; Férriz, Macarena; Tadeo, José Luis

2017-11-30

Macrolides are one of the most commonly used families of antibiotics employed in human and veterinary treatment. These compounds are considered emerging contaminants with potential ecological and human health risks that could be present in surface water. This paper describes the development and application of a simple and efficient extraction procedure for the determination of tilmicosin; erythromycin, tylosin and erythromycin-H 2 O from water samples. Sample extraction was carried out using magnetic solid-phase extraction using oleate functionalized magnetic nanoparticles followed by LC-MS/MS analysis. The effects of several parameters on the extraction efficiency of MLs from water were evaluated. The recovery results obtained were >84% for most of the compounds, except for erytromycin. The LOD and LOQ values ranged from 11.5 to 26ngL -1 and from 34 to 77ngL -1 , respectively. The selected method was applied to monitor these contaminants in water samples from different sources. Tilmicosin and tylosin were not detected in any of the samples, but erythromycin and erythromycin-H 2 O were found in 50% of the surface water samples at levels from

Combination of solvent extractants for dispersive liquid-liquid microextraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry.

PubMed

Pastor-Belda, Marta; Garrido, Isabel; Campillo, Natalia; Viñas, Pilar; Hellín, Pilar; Flores, Pilar; Fenoll, José

2017-10-15

A multiresidue method was developed to determine twenty-five fungicides belonging to three different chemical families, oxazoles, strobilurins and triazoles, in water and fruit samples, using dispersive liquid-liquid microextraction (DLLME) and liquid chromatography/tandem mass spectrometry (LC-MS 2 ). Solid-liquid extraction with acetonitrile was used for the analysis in fruits, the extract being used as dispersant solvent in DLLME. Since some of the analytes showed high affinity for chloroform and the others were more efficiently extracted with undecanol, a mixture of both solvents was used as extractant in DLLME. After evaporation of CHCl 3 , the enriched phase was analyzed. Enrichment factors in the 23-119 and 12-60 ranges were obtained for waters and fruits, respectively. The approach was most sensitive for metominostrobin with limits of quantification of 1ngL -1 and 5ngkg -1 in waters and fruits, respectively, while a similar sensitivity was attained for tebuconazole in fruits. Recoveries of the fungicides varied between 86 and 116%. Copyright © 2017 Elsevier Ltd. All rights reserved.

Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Krawczyk-Coda, Magdalena

2017-03-01

In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

Complex admixtures of clathrate hydrates in a water desalination method

DOEpatents

Simmons, Blake A [San Francisco, CA; Bradshaw, Robert W [Livermore, CA; Dedrick, Daniel E [Berkeley, CA; Anderson, David W [Riverbank, CA

2009-07-14

Disclosed is a method that achieves water desalination by utilizing and optimizing clathrate hydrate phenomena. Clathrate hydrates are crystalline compounds of gas and water that desalinate water by excluding salt molecules during crystallization. Contacting a hydrate forming gaseous species with water will spontaneously form hydrates at specific temperatures and pressures through the extraction of water molecules from the bulk phase followed by crystallite nucleation. Subsequent dissociation of pure hydrates yields fresh water and, if operated correctly, allows the hydrate-forming gas to be efficiently recycled into the process stream.

Lab-on-a-Chip Sensor for Monitoring Perchlorate in Ground and Surface Water

DTIC Science & Technology

2012-02-01

uses zwitterionic surfactants was immobilized on either a conventional or membrane-based stationary phase (electrostatic ion chromatography ) em...substantially higher than that of drinking water. A novel extraction method incorporat- ing the fundamentals of electrostatic ion chromatography (EIC) was...electrostatic ion chromatography (EIC), is presented as a way to overcome this challenge. Two extraction formats, employing either a packed bed or a monolith

Analysis of trifluralin, methyl paraoxon, methyl parathion, fenvalerate and 2,4-D dimethylamine in pond water using solid-phase extraction

USGS Publications Warehouse

Swineford, D.M.; Belisle, A.A.

1989-01-01

A method was developed for the simultaneous extraction of trifluralin, methyl paraoxon, methyl parathion, fenvalerate, and 2,4-D dimethylamine salt in pond water using a solid-phase C18 column. After elution from the C18 column, the eluate was analyzed on a capillary gas chromatograph equipped with an electron-capture or flame photometric detector.

One-pot polymerization of monolith coated stir bar for high efficient sorptive extraction of perfluoroalkyl acids from environmental water samples followed by high performance liquid chromatography-electrospray tandem mass spectrometry detection.

PubMed

Yao, Xuezi; Zhou, Zhen; He, Man; Chen, Beibei; Liang, Yong; Hu, Bin

2018-06-08

In this work, poly(1-vinylimidazole-ethyleneglycol dimethacrylate) (poly(VI-EDMA)) monolith coated stir bars were synthesized by one-pot polymerization, and they exhibited higher extraction efficiency and faster extraction dynamics for selected PFAAs than commercial ethylene glycol modified silicone (EG-silicone) and polydimethylsiloxane (PDMS) coated stir bars. Taking eleven PFAAs as target analytes, including C4-C12 perfluoroalkyl carboxylates (PFCAs) and C6, C8 perfluoroalkane sulfonates (PFSAs), a method combining monolith-based stir bar sorptive extraction (SBSE) with high performance liquid chromatography (HPLC) - electrospray tandem mass spectrometry (ESI-MS/MS) was proposed for the determination of multiplex PFAAs in environmental water samples. Under the optimized conditions, low limits of detection (0.06-0.40 ng/L) and wide linear range (0.6-400 ng/L) were obtained for target PFAAs with. The developed method was then applied for the analysis of target PFAAs in environmental water samples, and recoveries of 80.1-117% and 80.3-122% were obtained for target PFAAs in spiked Yangtze River and East Lake water samples respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

Total alkaloid content in various fractions of Tabernaemonata sphaerocarpa Bl. (Jembirit) leaves

NASA Astrophysics Data System (ADS)

Salamah, N.; Ningsih, D. S.

2017-11-01

Tabernaemontana sphaerocarpa Bl. (Jembirit) is one of the Apocynaceae family plants containing alkaloid compound. Traditionally, it is used as an anti-inflammatory medicine. It is found to have a new bisindole alkaloid compound that shows a potent cytotoxic activity in human cancer. This study aimed to know the total alkaloid content in some fractions of ethanolic extract of T. sphaerocarpa Bl. leaf powder was extracted by maceration method in 70% ethanol solvent. Then, the extract was fractionated in a separatory funnel using water, ethyl acetate, and hexane. The total alkaloid content in each fraction was analyzed with visible spectrophotometric methods based on the reaction with Bromocresol Green (BCG). The total alkaloids in water fraction and ethyl acetate fraction were (0.0312±0.0009)% and (0.0281±0.0014)%, respectively. Meanwhile, the total alkaloid content in hexane was not detected. The statistical analysis, performed in SPSS, resulted in a significant difference between the total alkaloids in water fraction and ethyl acetate fraction. The total alkaloid in water fraction of T. sphaerocarpa Bl. was higher than the one in ethyl acetate fraction.

Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

PubMed

Washington, John W; Henderson, W Matthew; Ellington, J Jackson; Jenkins, Thomas M; Evans, John J

2008-02-15

With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorooctanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary phases, two different liquid chromatography-tandem mass spectrometry (LC/MS/MS) systems, and eight combinations of sample-extract pretreatments, extractions and cleanups on three test soils. For the columns and systems we tested, we achieved the greatest analytical sensitivity for PFCAs using a column with a C(18) stationary phase in a Waters LC/MS/MS. In this system we achieved an instrument detection limit for PFOA of 270 ag/microL, equating to about 14 fg of PFOA on-column. While an elementary acetonitrile/water extraction of soils recovers PFCAs effectively, natural soil organic matter also dissolved in the extracts commonly imparts significant noise that appears as broad, multi-nodal, asymmetric peaks that coelute with several PFCAs. The intensity and elution profile of this noise is highly variable among soils and it challenges detection of low concentrations of PFCAs by decreasing the signal-to-noise contrast. In an effort to decrease this background noise, we investigated several methods of pretreatment, extraction and cleanup, in a variety of combinations, that used alkaline and unbuffered water, acetonitrile, tetrabutylammonium hydrogen sulfate, methyl-tert-butyl ether, dispersed activated carbon and solid-phase extraction. For the combined objectives of complete recovery and minimization of background noise, we have chosen: (1) alkaline pretreatment; (2) extraction with acetonitrile/water; (3) evaporation to dryness; (4) reconstitution with tetrabutylammonium-hydrogen-sulfate ion-pairing solution; (5) ion-pair extraction to methyl-tert-butyl ether; (6) evaporation to dryness; (7) reconstitution with 60/40 acetonitrile/water (v/v); and (8) analysis by LC/MS/MS. Using this method, we detected in all three of our test soils, endogenous concentrations of all of our PFCA analytes, C(6) through C(10)-the lowest concentrations being roughly 30 pg/g of dry soil for perfluorinated hexanoic and decanoic acids in an agricultural soil.

Liquid Metering Centrifuge Sticks (LMCS): A Centrifugal Approach to Metering Known Sample Volumes for Colorimetric Solid Phase Extraction (C-SPE)

NASA Technical Reports Server (NTRS)

Gazda, Daniel B.; Schultz, John R.; Clarke, Mark S.

2007-01-01

Phase separation is one of the most significant obstacles encountered during the development of analytical methods for water quality monitoring in spacecraft environments. Removing air bubbles from water samples prior to analysis is a routine task on earth; however, in the absence of gravity, this routine task becomes extremely difficult. This paper details the development and initial ground testing of liquid metering centrifuge sticks (LMCS), devices designed to collect and meter a known volume of bubble-free water in microgravity. The LMCS uses centrifugal force to eliminate entrapped air and reproducibly meter liquid sample volumes for analysis with Colorimetric Solid Phase Extraction (C-SPE). C-SPE is a sorption-spectrophotometric platform that is being developed as a potential spacecraft water quality monitoring system. C-SPE utilizes solid phase extraction membranes impregnated with analyte-specific colorimetric reagents to concentrate and complex target analytes in spacecraft water samples. The mass of analyte extracted from the water sample is determined using diffuse reflectance (DR) data collected from the membrane surface and an analyte-specific calibration curve. The analyte concentration can then be calculated from the mass of extracted analyte and the volume of the sample analyzed. Previous flight experiments conducted in microgravity conditions aboard the NASA KC-135 aircraft demonstrated that the inability to collect and meter a known volume of water using a syringe was a limiting factor in the accuracy of C-SPE measurements. Herein, results obtained from ground based C-SPE experiments using ionic silver as a test analyte and either the LMCS or syringes for sample metering are compared to evaluate the performance of the LMCS. These results indicate very good agreement between the two sample metering methods and clearly illustrate the potential of utilizing centrifugal forces to achieve phase separation and metering of water samples in microgravity.

Simultaneous determination of estrogenic odorant alkylphenols, chlorophenols, and their derivatives in water using online headspace solid phase microextraction coupled with gas chromatography-mass spectrometry.

PubMed

Yuan, Su-Fen; Liu, Ze-Hua; Lian, Hai-Xian; Yang, Chuangtao; Lin, Qing; Yin, Hua; Dang, Zhi

2016-10-01

A simple online headspace solid-phase microextraction (HS-SPME) coupled with the gas chromatography-mass spectrometry (GC-MS) method was developed for simultaneous determination of trace amounts of nine estrogenic odorant alkylphenols and chlorophenols and their derivatives in water samples. The extraction conditions of HS-SPME were optimized including fiber selection, extraction temperature, extraction time, and salt concentration. Results showed that divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was the most appropriate one among the three selected commercial fibers, and the optimal extraction temperature, time, and salt concentration were 70 °C, 30 min, and 0.25 g/mL, respectively. The developed method was validated and showed good linearity (R (2) > 0.989), low limit of detection (LOD, 0.002-0.5 μg/L), and excellent recoveries (76-126 %) with low relative standard deviation (RSD, 0.7-12.9 %). The developed method was finally applied to two surface water samples and some of these target compounds were detected. All these detected compounds were below their odor thresholds, except for 2,4,6-TCAS and 2,4,6-TBAS wherein their concentrations were near their odor thresholds. However, in the two surface water samples, these detected compounds contributed to a certain amount of estrogenicity, which seemed to suggest that more attention should be paid to the issue of estrogenicity rather than to the odor problem.

Quantitative 31P NMR for Simultaneous Trace Analysis of Organophosphorus Pesticides in Aqueous Media Using the Stir Bar Sorptive Extraction Method

NASA Astrophysics Data System (ADS)

Ansari, S.; Talebpour, Z.; Molaabasi, F.; Bijanzadeh, H. R.; Khazaeli, S.

2016-09-01

The analysis of pesticides in water samples is of primary concern for quality control laboratories due to the toxicity of these compounds and their associated public health risk. A novel analytical method based on stir bar sorptive extraction (SBSE), followed by 31P quantitative nuclear magnetic resonance (31P QNMR), has been developed for simultaneously monitoring and determining four organophosphorus pesticides (OPPs) in aqueous media. The effects of factors on the extraction efficiency of OPPs were investigated using a Draper-Lin small composite design. An optimal sample volume of 4.2 mL, extraction time of 96 min, extraction temperature of 42°C, and desorption time of 11 min were obtained. The results showed reasonable linearity ranges for all pesticides with correlation coefficients greater than 0.9920. The limit of quantification (LOQ) ranged from 0.1 to 2.60 mg/L, and the recoveries of spiked river water samples were from 82 to 94% with relative standard deviation (RSD) values less than 4%. The results show that this method is simple, selective, rapid, and can be applied to other sample matrices.

Selenium speciation methods and application to soil saturation extracts from San Joaquin Valley, California

USGS Publications Warehouse

Fio, John L.; Fujii, Roger

1990-01-01

Methods to determine soluble concentrations of selenite, selenate, and organic Se were evaluated on saturation extracts of soil samples collected from three sites on the Panoche Creek alluvial fan in the western San Joaquin Valley, California. The methods were used in combination with hydride-generation atomic-absorption spectrometry for detection of Se, and included a selective chemical-digestion method and three chromatographic methods using XAD-8 resin, Sep-Pak C18 cartridge, and a combination of XAD-8 resin and activated charcoal. The chromatography methods isolate dissolved organic matter that can inhibit Se detection by hydride-generation atomic-absorption spectrometry. Isolation of hydrophobic organic matter with XAD-8 did not affect concentrations of selenite and selenate, and the isolated organic matter represents a minimal estimation of organic Se. Ninety-eight percent of the Se in the extracts was selenate and about 100% of the isolated organic Se was associated with the humic acid fraction of dissolved organic matter. The depth distribution of Se species in the soil saturation extracts support a hypothesis that the distribution of soluble Se and salinity in these soils is the result of evaporation from a shallow water table and leaching by irrigation water low in Se and salinity.

Liquid chromatographic method for determining the concentration of bisazir in water

USGS Publications Warehouse

Scholefield, Ronald J.; Slaght, Karen S.; Allen, John L.

1997-01-01

Barrier dams, traps, and lampricides are the techniques currently used by the Great Lakes Fishery Commission to control sea lampreys (Petromyzon marinus) in the Great Lakes. To augment these control techniques, a sterile-male-release research program was initiated at the Lake Huron Biological Station. Male sea lampreys were sterilized by intraperitoneal injection of the chemical sterilant P,P-bis(1-aziridinyl)-N-methylphosphinothioic amide (bisazir). An analytical method was needed to quantitate the concentration of bisazir in water and to routinely verify that bisazir (>25 μg/L) does not persist in the treated effluent discharged from the sterilization facility to Lake Huron. A rapid, accurate, and sensitive liquid chromatographic (LC) method was developed for determining bisazir in water. Bisazir was dissolved in Lake Huron water; extracted and concentrated on a C18 solid-phase extraction column; eluted with methanol; and quantitated by reversed-phase LC using a C18 column, a mobile phase of 70% water and 30% methanol (v/v), and UV detection (205 nm). Bisazir retention time was 7-8 min; total run time was about 20 min. Method detection limit for bisazir dissolved in Lake Huron water was about 15 μg/L. Recovery from Lake Huron water fortified with bisazir at 100 μg/L was 94% (95% confidence interval, 90.2-98.2%).

Estimation of evapotranspiration rate in irrigated lands using stable isotopes

NASA Astrophysics Data System (ADS)

Umirzakov, Gulomjon; Windhorst, David; Forkutsa, Irina; Brauer, Lutz; Frede, Hans-Georg

2013-04-01

Agriculture in the Aral Sea basin is the main consumer of water resources and due to the current agricultural management practices inefficient water usage causes huge losses of freshwater resources. There is huge potential to save water resources in order to reach a more efficient water use in irrigated areas. Therefore, research is required to reveal the mechanisms of hydrological fluxes in irrigated areas. This paper focuses on estimation of evapotranspiration which is one of the crucial components in the water balance of irrigated lands. Our main objective is to estimate the rate of evapotranspiration on irrigated lands and partitioning of evaporation into transpiration using stable isotopes measurements. Experiments has done in 2 different soil types (sandy and sandy loam) irrigated areas in Ferghana Valley (Uzbekistan). Soil samples were collected during the vegetation period. The soil water from these samples was extracted via a cryogenic extraction method and analyzed for the isotopic ratio of the water isotopes (2H and 18O) based on a laser spectroscopy method (DLT 100, Los Gatos USA). Evapotranspiration rates were estimated with Isotope Mass Balance method. The results of evapotranspiration obtained using isotope mass balance method is compared with the results of Catchment Modeling Framework -1D model results which has done in the same area and the same time.

Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

PubMed

Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

2016-09-01

In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 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).

Scavenging capacity of strawberry tree (Arbutus unedo L.) leaves on free radicals.

PubMed

Oliveira, Ivo; Coelho, Valentim; Baltasar, Raquel; Pereira, José Alberto; Baptista, Paula

2009-07-01

Despite strawberry tree (Arbutus unedo L.) leaves had a long use in traditional medicine due to its antiseptic, diuretic, astringent and depurative properties, the potential of their antioxidant activity are still lacking. Our study goals to assess the antioxidant and free radical scavenging potential of water, ethanol, methanol and diethyl ether extracts of A. unedo leaves. Total phenols content was achieved spectrophotometrically using Folin-Ciocalteau reagent with gallic acid as standard. Antioxidant activity was evaluated using three different methods: reducing power of iron (III)/ferricyanide complex assay, scavenging effect on DPPH (2,2-diphenyl-1-picrylhydrazyl) radicals and scavenging effect on superoxide radicals by using the PMS-NADH-nitroblue tetrazolium system. Ethanol extracts of A. unedo leaves were the highest in reducing power (IC(50) 232.7 microg/mL) and DPPH scavenging effect (IC(50) 63.2 microg/mL) followed by water extracts (with IC(50) of 287.7 and 73.7 microg/mL, respectively); whereas diethyl ether extracts were the lowest. In the scavenging on superoxide radical assay, methanol extracts obtained the best results (IC(50) 6.9 microg/mL). For all the methods tested the antioxidant activity was concentration dependent. In accordance with antioxidant activity, highest total phenols content were found in ethanol, followed by water, methanol and diethyl ether extract. The results indicated that A. unedo leaves are a potential source of natural antioxidants.

Pressurized hot water extraction followed by miniaturized membrane assisted solvent extraction for the green analysis of alkylphenols in sediments.

PubMed

Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

2015-02-27

A novel and Green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol) in sediments was developed and validated. The method was based on pressurized hot water extraction (PHWE) followed by miniaturized membrane assisted solvent extraction (MASE) and liquid chromatography-electrospray ionization tandem mass spectrometry detection (LC-ESI-MS/MS). The extraction conditions were optimized by a Plackett-Burman design in order to minimize the number of assays according to Green principles. Matrix effect was studied and compensated using deuterated labeled standards as surrogate standards for the quantitation of the target compounds. The analytical features of the method were satisfactory: relative recoveries varied between 92 and 103% and repeatability and intermediate precision were <9% for all compounds. Quantitation limits of the method (MQL) ranged from 0.061 (4-n-nonylphenol) to 1.7ngg(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of the exposed methodology. Reagent consumption, analysis time and waste generation were minimized. The "greenness" of the proposed method was evaluated using an analytical Eco-Scale approach and satisfactory results were obtained. The applicability of the proposed method was demonstrated analysing sediment samples of Galicia coast (NW of Spain) and the ubiquity of alkylphenols in the environment was demonstrated. Copyright © 2015 Elsevier B.V. All rights reserved.

Method of simultaneous stir bar sorptive extraction of phenethylamines and THC metabolite from urine.

PubMed

Goto, Yoshiyuki; Takeda, Shiho; Araki, Toshinori; Fuchigami, Takayuki

2011-10-01

Stir bar sorptive extraction is a technique used for extracting target substances from various aqueous matrixes such as environmental water, food, and biological samples. This type of extraction is carried out by rotating a coated stir bar is rotated in the sample solution. In particular, Twister bar is a commercial stir bar that is coated with polydimethylsiloxane (PDMS) and used to perform sorptive extraction. In this study, we developed a method for simultaneous detection of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and a Δ(9)-tetrahydrocannabiniol (THC) metabolite in human urine. For extracting the target analytes, the Twister bar was simply stirred in the sample in the presence of a derivatizing agent. Using this technique, phenethylamines and the acidic THC metabolite can be simultaneously extracted from human urine. This method also enables the extraction of trace amounts of these substances with good reproducibility and high selectivity. The proposed method offers many advantages over other extraction-based approaches and is therefore well suited for screening psychoactive substances in urine specimens.

Hydrophilic microspheres from water-in-oil emulsions by the water diffusion technique.

PubMed

Trotta, Michele; Chirio, Daniela; Cavalli, Roberta; Peira, Elena

2004-08-01

In this study, we developed and evaluated a novel method to produce insulin-loaded hydrophilic microspheres allowing high encapsulation efficiency and the preservation of peptide stability during particle processing. The preparation method used the diffusion of water by an excess of solvent starting from a water-in-solvent emulsion. The water dispersed phase containing albumin or lactose, or albumin-lactose in different weight ratios, and insulin was emulsified in water-saturated triacetin with and without emulsifiers, producing a water-in-triacetin emulsion. An excess of triacetin was added to the emulsion so that water could be extracted into the continuous phase, allowing the insulin-loaded microsphere precipitation. Insulin stability within the microspheres after processing was evaluated by reverse-phase and size-exclusion high-performance liquid chromatography. The water diffusion extraction process provided spherical microparticles of albumin or albumin-lactose. The mean diameter of the microspheres prepared with or without emulsifiers ranged from 2 to 10 microm, and the encapsulation efficiency of insulin was between 60% and 75%, respectively. The analysis of microsphere content after processing showed that insulin did not undergo any chemical modification within microspheres. The use of lactose alone led to the formation of highly viscous droplets that coalesced during the purification step. The water extraction procedures successfully produced insulin-loaded hydrophilic microspheres allowing the preservation of peptide stability. The type of excipient and the size of the disperse phase of the primary w/o emulsion were crucial determinants of microsphere characteristics.

Comparison of Composition and Anticaries Effect of Galla Chinensis Extracts with Different Isolation Methods

PubMed Central

Huang, Xuelian; Deng, Meng; Liu, Mingdong; Cheng, Lei; Exterkate, R.A.M.; Li, Jiyao; Zhou, Xuedong; Ten Cate, Jacob. M.

2017-01-01

Objectives: Galla chinensis water extract (GCE) has been demonstrated to inhibit dental caries by favorably shifting the demineralization/remineralization balance of enamel and inhibiting the biomass and acid formation of dental biofilm. The present study focused on the comparison of composition and anticaries effect of Galla chinensis extracts with different isolation methods, aiming to improve the efficacy of caries prevention. Methods: The composition of water extract (GCE), ethanol extract (eGCE) and commercial tannic acid was compared. High performance liquid chromatography coupled to electrospray ionization-time of flight-mass spectrometry (HPLC-ESI-TOF-MS) analysis was used to analyze the main ingredients. In vitro pH-cycling regime and polymicrobial biofilms model were used to assess the ability of different Galla chinensis extracts to inhibit enamel demineralization, acid formation and biofilm formation. Results: All the GCE, eGCE and tannic acid contained a high level of total phenolics. HPLC-ESI-TOF-MS analysis showed that the main ingredients of GCE were gallic acid (GA), while eGCE mainly contained 4-7 galloylglucopyranoses (GGs) and tannic acid mainly contained 5-10 GGs. Furthermore, eGCE and tannic acid showed a better effect on inhibiting enamel demineralization, acid formation and biofilm formation compared to GCE. Conclusions: Galla chinensis extracts with higher tannin content were suggested to have higher potential to prevent dental caries. PMID:28979574