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牛奶中32种农药的气相色谱-离子阱串联质谱法测定
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作者单位
陈美瑜,林竹光 1.厦门大学材料学院高性能陶瓷纤维教育部重点实验室2.厦门大学化学化工学院化学系 
基金项目:国家自然科学基金青年基金资助项目(51603175)
中文摘要:建立了牛奶中有机氯、有机磷和拟除虫菊酯3类32种农药残留的气相色谱-离子阱串联质谱(GC-IT-MS/MS)分析方法。针对目标物灵敏度不同选择电子轰击电离源或化学电离源,系统地优化了串联质谱的分析条件,并分析了产生这些影响的机理。在优化条件下,32种农药在 25(10)~500(200) μg/L范围内线性关系良好,相关系数均大于0.994;倍硫磷和毒死蜱的方法检出限(MDL)分别为1.7 μg/kg和2.8 μg/kg,其它30种农药的MDL为0.026~1.2 μg/kg;当样品的加标浓度水平为50、200 μg/kg(有机氯类农药的加标浓度为20、100 μg/kg)时,32种目标物的平均加标回收率为71.5%~116%,相对标准偏差为1.9%~14%。将方法应用于实际样品的检测,其抗干扰能力强,能减少分析结果的假阳性。
中文关键词:气相色谱-离子阱串联质谱(GC-IT-MS/MS)  电子轰击电离  化学电离  有机氯  有机磷  拟除虫菊酯
 
Determination of 32 Pesticide Residues in Milk by Gas Chromatography-Ion Trap Tandem Mass Spectrometry
Abstract:A method was developed for the rapid determination of 32 pesticide residues,including organ ochlorine,organophosphate and pyrethroid pesticides,in milk based on gas chromatography-ion trap tandem mass spectrometry.Electron impact ionization or chemical ionization were selected for the analytes with different sensitivities.Experimental parameters influencing the behaviours of compounds in the analysis of MS/MS were investigated and optimized.The mechanisms for the influencing factors were also discussed.Under the optimal conditions,the calibration curves for 32 pesticides were linear in the ranges of 25(10)-500(200) μg/L with correlation coefficients more than 0994.The method detection limits(MDL) for fention and chlorpyriphos were 1.7 μg/kg and 2.8 μg/kg,respectively,while those for the other pesticides were in the range of 0.026-1.2 μg/kg.The recoveries for 32 pesticides at two spiked levels of 50 and 200 μg/kg(organochlorine pesticides were spiked at 20 and 100 μg/kg) ranged from 71.5% to 116% with relative standard deviations(RSDs) of 1.9%-14%.The proposed method was applied in the detection for real samples,and could reduce the possibility of false positive results with strong anti interference.
Key Words:gas chromatography-ion trap tandem mass spectrometry(GC-IT-MS/MS)  electron impact ionization  chemical ionization  organochlorine  organophosphate  pyrethroid
引用本文:陈美瑜,林竹光.牛奶中32种农药的气相色谱-离子阱串联质谱法测定[J].分析测试学报,2019,(2):182-187.
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