非衍生化/液相色谱-串联质谱法测定果蔬中氨基酸类有机磷除草剂残留  

Determination of Organophosphorus Amino Acids Herbicides Residues in Fruits and Vegetables by Underivatization/Liquid Chromatography-Tandem Mass Spectrometry

作　　者：林丽敏 张建莹 肖锋 黄科 叶刚 洪小柳 吕飞 LIN Li-min;ZHANG Jian-ying;XIAO Feng;HUANG Ke;YE Gang;HONG Xiao-liu;LÜFei(Food Inspection&Quarantine Center,Shenzhen Customs,Shenzhen 518045,China;Comprehensive Technology Center of Huizhou Customs,Huizhou 516006,China)

机构地区：[1]深圳海关食品检验检疫技术中心,广东深圳518045 [2]惠州海关技术中心,广东惠州516006

出　　处：《分析测试学报》2022年第11期1702-1706,共5页Journal of Instrumental Analysis

基　　金：深圳海关科技项目(2021SZHK007)。

摘　　要：建立了果蔬中4种氨基酸类有机磷除草剂的非衍生化/液相色谱-串联质谱分析方法。样品采用水-二氯甲烷混合溶液提取,经二氯甲烷液液萃取法结合HLB固相萃取柱净化后,进行液相色谱-串联质谱测定。最佳实验条件下,4种化合物在0.010~0.200 mg/L质量浓度范围内呈良好线性关系,相关系数(r)均大于0.996,方法检出限为0.01 mg/kg,定量下限为0.05 mg/kg。在0.050、0.100、0.200 mg/kg 3个加标水平下的平均回收率为72.2%~109%,相对标准偏差(RSD,n=6)为2.2%~11%。该方法快速、简便、灵敏、准确,可用于水果、蔬菜中氨基酸类有机磷除草剂的定量检测和确证。An underivatization/liquid chromatography-tandem mass spectrometric method was devel⁃oped for the determination of 4 organophosphorus amino acids herbicides in fruits and vegetables.Sam⁃ples were firstly extracted with water-dichloromethane solution,then purified by dichloromethane liq⁃uid-liquid extraction with HLB solid phase extraction column,and finally determined by liquid chro⁃matography-mass spectrometry.At the optimal conditions,the linear correlation coefficients(r)for all compounds were more than 0.996 in the concentration range of 0.010-0.200 mg/L.The limits of detection and quantitation of the method were 0.01 mg/kg and 0.05 mg/kg,respectively.The average recoveries for all compounds at spiked levels of 0.050,0.100 and 0.200 mg/kg ranged from 72.2%to 109%,with relative standard deviations(RSDs,n=6)of 2.2%-11%.The method is rapid,sim⁃ple,sensitive and accuracy,and it could be used for the determination and confirmation of organo⁃phosphorus amino acids herbicides in fruits and vegetables.

关 键 词：非衍生化 氨基酸类有机磷除草剂 液相色谱-串联质谱 

分 类 号：O652.7[理学—分析化学] TS201.6[理学—化学]