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
张建莹,研究员,研究方向:食品中农兽药残留及污染物分析,E - mail:zhangjianying1001@163.com
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林丽敏,张建莹,肖锋等.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[J].分析测试学报,2022,41(11):1702-1706.
LIN Li-min,ZHANG Jian-ying,XIAO Feng,et al.Determination of Organophosphorus Amino Acids Herbicides Residues in Fruits and Vegetables by Underivatization/Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(11):1702-1706.
林丽敏,张建莹,肖锋等.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[J].分析测试学报,2022,41(11):1702-1706. DOI: 10.19969/j.fxcsxb.22042805.
LIN Li-min,ZHANG Jian-ying,XIAO Feng,et al.Determination of Organophosphorus Amino Acids Herbicides Residues in Fruits and Vegetables by Underivatization/Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(11):1702-1706. DOI: 10.19969/j.fxcsxb.22042805.
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 developed for the determination of 4 organophosphorus amino acids herbicides in fruits and vegetables.Samples were firstly extracted with water-dichloromethane solution,then purified by dichloromethane liquid-liquid extraction with HLB solid phase extraction column,and finally determined by liquid chromatography-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,simple,sensitive and accuracy,and it could be used for the determination and confirmation of organophosphorus amino acids herbicides in fruits and vegetables.
非衍生化氨基酸类有机磷除草剂液相色谱-串联质谱
underivatizationorganophosphorus amino acids herbicidesliquid chromatography-tandem mass spectrometry
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