Citation: CAI Lisheng, SHEN Weijian, WANG Zhengping, ZHANG Rui, DING Tao, YU Keyao, WANG Hong, ZHANG Wenjun, GONG Yuxia. Determination of three organotin pesticide residues in apples and cabbages by gas chromatography-electron impact/positive chemical ionization mass spectrometry[J]. Chinese Journal of Chromatography, ;2017, 35(11): 1177-1183. doi: 10.3724/SP.J.1123.2017.07011 shu

Determination of three organotin pesticide residues in apples and cabbages by gas chromatography-electron impact/positive chemical ionization mass spectrometry

CAI Lisheng ^1,2, ,
SHEN Weijian ² ,
WANG Zhengping ¹ ,
ZHANG Rui ² ,
DING Tao ² ,
YU Keyao ² ,
WANG Hong ² ,
ZHANG Wenjun ² ,
GONG Yuxia ²

1.
Nanjing University of Science and Technology, Nanjing 210094, China;
2.
Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China

Received Date: 13 July 2017

Fund Project: Shanghai Yangtze River Delta Science and Technology Cooperation Project (No. 15395810100).

A method for the simultaneous determination of fenbutatin oxide, triphenyltin and cyhexatin in apples and cabbages was developed by gas chromatography-mass spectrometry coupled with two different ionization techniques, electron impact (EI) ionization and positive chemical ionization (PCI). At first, the samples were digested by hydrobromic acid, and extracted by acetone-hexane (1:2, v/v). The extracts were derivatized by sodium tetraethylborate as the derivatization reagent, and cleaned up by the Florisil SPE columns. Finally, the samples were analyzed by GC-EI/MS and GC-PCI/MS in selected ion monitoring (SIM) mode. The results showed that good linearities were obtained with correlation coefficients (r²) greater than 0.997 for fenbutatin oxide in the range of 75-500 μg/L in both foods, triphenyltin in the range of 50-1000 μg/L in cabbages and 50-500 μg/L in apples and cyhexatin in the range of 50-1000 μg/L in the two foods. The accuracy was checked at three spiked levels (50, 100 and 200 μg/kg) in cabbages and apples. The limits of detection (LODs, S/N=3) were 0.01-0.05 mg/kg (EI) and 0.01-0.02 mg/kg (PCI), and the limits of quantifications (LOQs, S/N=10) were 0.03-0.16 mg/kg (EI) and 0.02-0.06 mg/kg (PCI). The average recoveries ranged from 59.24%-97.36% (apples) and 50.54%-94.54% (cabbages) in the mode of EI, and the corresponding values were 65.38%-95.86% and 62.56%-90.44% in the mode of PCI. The relative standard deviations (RSDs) were all less than 6.9% (n=6). The PCI method can be used to improve the accuracy in comparing with the EI, in terms of good selectivity and high sensitivity.
- gas chromatography-mass spectrometry (GC-MS),
- electron impact ionization (EI),
- positive chemical ionization (PCI),
- fentutatin oxide,
- triphenyltin,
- cyhexatin
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