首页|超高效液相色谱—串联质谱法测定动物源性食品中百菌清及其代谢物4-羟基百菌清残留量

超高效液相色谱—串联质谱法测定动物源性食品中百菌清及其代谢物4-羟基百菌清残留量

扫码查看
[目的]建立超高效液相色谱—串联质谱法同时测定动物源性食品中百菌清及其代谢物4-羟基百菌清残留的检测方法.[方法]样品经1%乙酸—乙腈溶液振荡提取,正己烷脱脂,基质分散固相萃取剂(PSA、无水硫酸镁)净化,通过Waters BEH C18色谱柱分离,以乙腈—0.1%甲酸水溶液为流动相进行梯度洗脱,采用大气压化学电离源(APCI)负离子多反应监测模式(MRM)进行测定,基质匹配外标法定量.[结果]百菌清及4-羟基百菌清在5~500 μg/L范围内线性关系良好,定量限均为0.005 mg/kg,平均回收率分别为69.3%~111.0%和65.3%~117.9%,相对标准偏差分别为1.6%~10.8%和1.1%~9.0%.[结论]该方法前处理简单快速,灵敏度高,准确可靠,可用于动物源性食品中百菌清及其代谢物4-羟基百菌清的同时测定.
Determination of chlorothalonil and its metabolite 4-hydroxychlorothalonil residues in animal-derived food by ultra-high performance liquid chromatography-tandem mass spectrometry
[Objective]To establish a method for simultaneous determination of chlorothalonil and its metabolite 4-hydroxychlorothalonil residues in animal-derived food by ultra-high performance liquid chromatography-tandem mass spectrometry.[Methods]The samples were extracted by oscillating with acetonitrile solution of 1%acetic acid,defatted with n-hexane,purified by matrix dispersible solid phase extractant(PSA,anhydrous magnesium sulfate),separated by Waters BEH C18 column under a gradient elution program using 0.1%formic acid aqueous solution and acetonitrile as the mobile phases.The anion multiple reaction monitoring model(MRM)of atmospheric pressure chemical ionization source(APCI)was used for the determination,and the matrix matching external standard method was used for quantitative determination.[Results]The linear relationships of chlorothalonil and 4-hydroxychlorothalonil were good in the range of 5~500 μg/L,and the limits of quantitation were 0.005 mg/kg.The average recoveries of chlorothalonil and 4-hydroxychlorothalonil were 69.3%~111.0%and 65.3%~117.9%,respectively.The relative standard deviations of chlorothalonil and 4-hydroxychlorothalonil were 1.6%~10.8%and 1.1%~9.0%,respectively.[Conclusion]The method is simple,rapid,sensitive,accurate and reliable for simultaneous determination of chlorothalonil and its metabolite 4-hydroxychlorothalonil in animal-derived food.

ultra-high performance liquid chromatography-tandem mass spectrometrychlorothalonil4-hydroxychlorothalonilanimal-derived food

刘小芳、李政、何浩、蒋军杰、陈媛媛

展开 >

湖南省产商品质量检验研究院,湖南 长沙 410007

食品安全监测与预警湖南省重点实验室,湖南 长沙 410007

超高效液相色谱—串联质谱 百菌清 4-羟基百菌清 动物源性食品

湖南省自然科学基金资助项目

2023JJ60530

2024

食品与机械
长沙理工大学

食品与机械

CSTPCD北大核心
影响因子:0.89
ISSN:1003-5788
年,卷(期):2024.40(9)