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Citation: SONG Xiaojuan, HE Xinran, YIN Mingming, WAN Yanyan. Determination of organochlorine and organophosphorus pesticides in soil by gas chromatography-tandem mass spectrometry with accelerated solvent extraction[J]. Chinese Journal of Chromatography, ;2018, 36(10): 1038-1044. doi: 10.3724/SP.J.1123.2018.05012 shu

Determination of organochlorine and organophosphorus pesticides in soil by gas chromatography-tandem mass spectrometry with accelerated solvent extraction

1.
Lianyungang Municipal Environmental Monitoring Center Station, Lianyungang 222001, China;
2.
College of Environment, Hohai University, Nanjing 210098, China

Received Date: 12 May 2018

Fund Project: Decision Support Project on National Major Environmental Issues (No. 2023004017)

A method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) coupled with accelerated solvent extraction (ASE) was developed for the determination of eight organochlorine pesticides (OCPs) and five organophosphorus pesticides (OPPs) in soils. The soil samples were grinded after freeze-drying. Particles with diameters lower than 250 μm were chosen by ion-sieving. After this, 10.0 g soil mixed with 2.0 g diaomite was extracted with hexane-acetone (1:1, v/v). The extracts were dehydrated with anhydrous sodium sulfate and concentrated with a termovap sample concentrator. The concentrated solutions were further cleaned up with Si SPE columns and eluted with hexane-acetone (1:1, v/v). The purified solutions were then isolated by HP-5MS column (30 m×0.25 mm×0.25 μm) and detected using the multiple reaction monitoring mode at the electron impact source. It is observed that this method has good linearities in the range of 1.00-100 μg/L for the 13 compounds, and the correlation coefficients (R) were greater than 0.995. The spiked recoveries of the 13 compounds were in the range of 66.8%-88.4%, and the relative standard deviations were less than 10%. With 10.0 g of sampling weight, the method detection limits ranged from 0.02 to 0.04 μg/kg for the eight OCPs and from 0.06 to 0.12 μg/kg for the five OPPs. This method is suitable for the determination of trace OCPs and OPPs in soils.
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