色谱2017，Vol.35Issue(11)：1177-1183,7.DOI:10.3724/SP.J.1123.2017.07011
气相色谱-电子轰击电离/正化学电离质谱法测定白菜和苹果中3种有机锡类农药残留
Determination of three organotin pesticide residues in apples and cabbages by gas chromatography-electron impact/ positive chemical ionization mass spectrometry
摘要
Abstract
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 tetraethylbo-rate 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 50-1000μg/L in cabbages and 50-500μg/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 corre-sponding 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.关键词
气相色谱-质谱/电子轰击电离源/正化学电离源/苯丁锡/三苯锡/三环锡Key words
gas chromatography-mass spectrometry ( GC-MS )/electron impact ionization ( EI)/positive chemical ionization ( PCI)/fentutatin oxide/triphenyltin/cyhexatin分类
化学化工引用本文复制引用
蔡理胜,沈伟健,王正萍,张睿,丁涛,余可垚,王红,张文俊,龚玉霞..气相色谱-电子轰击电离/正化学电离质谱法测定白菜和苹果中3种有机锡类农药残留[J].色谱,2017,35(11):1177-1183,7.基金项目
上海市长三角科技合作项目(15395810100). Shanghai Yangtze River Delta Science and Technology Cooperation Project ( No. 15395810100) . （15395810100）
