scholarly journals Determination of OCPs and PCBs in environmental water samples by GC-DLLME optimized by Response Surface Methodology

2019 ◽  
Vol 20 (46) ◽  
pp. 13-23
Author(s):  
Dekun Hou ◽  
Otgonbayar Khureldavaa ◽  
Fujin Zhang ◽  
Jiang He ◽  
Badgaa Amarsanaa

A new sample preparation procedure to determine seven organochlorine pesticides and seven polychlorinated biphenyls in environmental water samples by using a combination of ultrasonic-assisted solvent extraction and dispersive liquid-liquid micro-extraction was established, and the extracted analytes were analyzed by gas chromatography coupled with electron capture detector. Some parameters influencing the extraction efficiency were studied and optimized utilizing response surface methodology. Under the optimum extraction conditions, the method showed wide linear ranges with r2 > 0.9989 and low limits of detection and quantification between 0.16 ~ 2.17 μg/L and 0.53 ~ 7.16 μg/L, respectively. Enrichment factors (EF) were high and ranged from 63 to 116. Relative standard deviations (RSDs) for the extraction of 25 μg/L of each selected OCPs and PCBs were less than 10.2 %. The proposed method was successfully used for targets contaminations determination in different water samples. α-HCH, β-HCH and p,p’-DDE were found in lake water closed to farmland with concentrations of 2.56 μg/L, 4.44 μg/L and 4.74 μg/L, respectively, and other OCPs and PCBs were not found in the corresponding water samples. The relative recoveries of OCPs and PCBs from tap water, river water and lake water at spiking levels of 10 μg/L were in the range of 81.9 ~ 109.7 %, within a relative standard deviation of 1.7 ~ 11.8 %. The results revealed that the proposed method was well suited for the determination of trace amounts of target contaminations in liquid samples.

2012 ◽  
Vol 518-523 ◽  
pp. 1379-1382
Author(s):  
Ying Chun Yang ◽  
Qian Sun ◽  
Chong Shu Yi ◽  
Zhi Xiang Ye ◽  
Li Mo

A rapid and effective method, the dispersive liquid-liquid microextraction(DLLME) with gas chromatography, has been developed for the extraction and determination of OCP in environmental water samples. The factors relevant to the efficiency of DLLME were investigated and optimized. Under the optimum conditions, such as 150μL of dichloromethane as extraction solvent, 1.2 mL acetone as dispersive agent, 8 minutes extraction time, and without salt addition, the linear response of this method was in the range of 0.5~5000μg L−1 (r = 0.9981), the relative standard deviation (RSD) for 500μg L−1 and 1000μg L−1 of OCP was 5.2% and 12.6% (n = 6), respectively. The detection limit (3σ) was 0.08 μg L−1. The developed method was successfully applied to the determination of trace amount of OCP in three kinds of real environmental water samples, the spiked recoveries were in the range of 87.4%~108.0%.


2013 ◽  
Vol 11 (3) ◽  
pp. 394-403 ◽  
Author(s):  
Yanling Ma ◽  
Yingying Wen ◽  
Jinhua Li ◽  
Hua Wang ◽  
Yangjun Ding ◽  
...  

AbstractAbstract An efficient method based on dispersive liquid-liquid microextraction coupled with micellar electrokinetic chromatography has been developed for determination of three phenoxyacid herbicides (PAs) of 2,4-dichlorophenoxybutyric acid (2,4-DB), dicamba and 2,4-dichlorophenoxyacetic acid (2,4-D), in environmental water samples. The types and volumes of extracting and dispersing solvents, ionic strength, extraction and centrifugation time and centrifugation speed were investigated. Successful separation of the three PAs was achieved within 7 min, by using the background electrolyte solution consisting of 10 mmol L−1 sodium tetraborate, 25 mmol L−1 sodium dodecyl sulfate and 15% (v/v) methanol, at pH 9.75. Excellent analytical performances were attained, such as good linear relationships (R ≥0.9993) between peak area and concentration for each PAs from 10–1000 ng mL−1, limits of detection of 1.56–1.91 ng mL−1, and intra-day precisions at two spiked levels in terms of migration time and peak area within the range of 0.22–0.42% and 3.88–6.39%, respectively. Enrichment factors of 2,4-DB, dicamba and 2,4-D were 180, 151 and 216, respectively. The method recoveries obtained at fortified 20.0, 50.0 and 100.0 ng mL−1 for lake, river and reservoir water samples varied from 67.91 to 119.07% with the relative standard deviation of 1.47–6.89%. Graphical abstract


Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1376
Author(s):  
Yue Wang ◽  
Qicai Zhang ◽  
Shanshan Chen ◽  
Lin Cheng ◽  
Xu Jing ◽  
...  

An effective and sensitive method is necessary for the determination of polybrominated diphenyl ethers (PBDEs) pollutants in water. In this study, effervescent-assisted dispersive liquid-liquid microextraction with solidification of the aqueous phase (EA-DLLME-SAP), followed by Gas Chromatography-Tandem Mass Spectrometry (GC-MS-MS) quantitative analysis, was established for the preconcentration and determination of PBDEs in real environmental water samples. 1,1,2,2-Tetrachloroethane was used as the extractant and directly dispersed into the water phase of the aqueous samples with the aid of a large number of carbon dioxide bubbles generated via the acid-base reaction of acetic acid and sodium bicarbonate, which did not require the use of a dispersant during the extraction process. The key factors affecting the extraction recovery were optimized, and an internal standard was used for quantitative analysis, which gave good linearity ranges of 1–100 ng·L−1 (BDEs 28, 47, 99, and 100), 2–200 ng·L−1 (BDEs 153, 154, and 183) and 5–500 ng·L−1 (BDE 209) with limits of quantification in the range of 1.0–5.0 ng·L−1. The accuracy was verified with relative standard deviations < 8.5% observed in tap, lake, river and reservoir water samples with relative recoveries ranging from 67.2 to 102.6%. The presented method contributes to the determination of PBDEs in environmental water samples.


2012 ◽  
Vol 457-458 ◽  
pp. 536-539 ◽  
Author(s):  
Rui Hua Zhang ◽  
Xiao Li Yang ◽  
Jin Liu ◽  
Xian Zhong Cheng

A simple solid phase extraction procedure for adsorption and preconcentration of manganese(II, VII) in environmental water samples has been proposed prior to inductively coupled plasma mass spectrometry. The procedure presented based on quantitative recoveries of manganese >95%. In this work, the potential use of eggshell membrane(ESM), a typical biomaterial, as solid-phase extraction (SPE) adsorbent is evaluated for analysis of trace manganese. The analytical variables, pH, flow rate, sample volume, elution, coexisting ions for optimum recoveries of manganese (II) and manganese (VII) were investigated. The preconcentration factor was 60. The detection limit (3) of manganese was 0.031 ng L-1. The relative standard deviations of determination was found to be 3.21%. The procedure was successfully applied to the adsorption and determination of manganese in environmental water samples.


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