Citation: SHAO Yang, YANG Guo-Sheng, HAN Shen, MA Ling-Ling, LUO Min, LIU Wei-Hua, XU Dian-Dou. Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Surface Water Using Accelerate Solvent Extraction Coupling with Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(5): 698-706. doi: 10.11895/j.issn.0253-3820.150805 shu

Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Surface Water Using Accelerate Solvent Extraction Coupling with Gas Chromatography-Mass Spectrometry

SHAO Yang ^1,2, ,
YANG Guo-Sheng ^1,2 ,
HAN Shen ³ ,
MA Ling-Ling ^1,2 ,
LUO Min ^1,2 ,
LIU Wei-Hua ³ ,
XU Dian-Dou ^1,2

1.
Division of Nuclear Technology and Applications, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China;
2.
Beijing Engineering Research Center of Radiographic Techniques and Equipment, Beijing 100049, China;
3.
Beijing Entry-Exit Inspection and Quarantine Bureau Technology Centre, Beijing 100026, China

Received Date: 13 October 2015
Revised Date: 26 December 2015

Fund Project: This work was supported by the National Natural Science Foundation of China (Nos. 11275216, 11575210, 11435002, 21407149)

A rapid and sensitive analytical method for the simultaneous determination of 15 organochlorine pesticides (OCPs) and 82 polychlorinated biphenyls (PCBs) in water using accelerate solvent extraction (ASE) and silica gel solid phase extraction (SPE) cleanup followed by gas chromatography-mass spectrometry (GC-MS) analysis was developed. The main potential influence parameters which affected the recoveries of OCPs and PCBs were investigated for the optimum ASE efficiency. Finally, 3 static extraction cycles, 100℃ of extraction temperature, mixture of acetone and hexane (1:1, V/V) as extraction solvent, and 10 min of static extraction time were used. Under the optimized conditions, the recoveries of 15 OCPs and 82 PCBs in spiked water were 70.9%-130% and 52.5%-89.1%, respectively. The intra-day and inter-day relative standard deviation was 1.7%-16.1% and 2.4%-33.3%, respectively. The correlation coefficients (R²) for OCPs and PCBs were above 0.995 in the range of 10-800 μg/L. And the method detection limits were characterized as 0.13-0.38 ng/L for OCPs and 0.10-0.32 ng/L for PCBs. Compared to the traditional methods, the developed method had the advantages of higher recoveries and less consumption of extraction time and toxic solvent. Subsequently, the developed method was applied to measure the concentrations of OCPs and PCBs in the surface water of Beijing. The concentrations of OCPs and PCBs were in the range of not detected (n.d.)-3.45 ng/L and n.d.-4.88 ng/L, respectively.
- Accelerate solvent extraction,
- Organochlorine pesticides,
- Polychlorinated biphenyls,
- Surface water,
- Gas chromatography/mass spectrometry,
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