摘要
建立了动物源食品(猪肉、鸡肉、猪脂肪、猪心、猪肝、猪肾)中克霉唑残留量的同位素稀释气相色谱-串联质谱(GC-MS/MS)测定方法。样品经加速溶剂提取后,用凝胶渗透色谱净化。采用HP-5 MS色谱柱(30 m×0.25 mm×0.25μm)进行分离,多反应监测(MRM)模式检测,同位素内标法定量。实验结果表明,克霉唑在1~100μg/L浓度范围内线性良好,决定系数(R 2)为0.9995,定量限(LOQ,S/N≥10)为2.0μg/kg。在2.0、5.0、20.0μg/kg加标水平下,回收率在82.6%~116.5%之间,相对标准偏差为5.2%~13.5%。该方法灵敏度高、准确性好,能够满足动物源食品中克霉唑残留量的确证和定量分析。
An isotope dilution gas chromatography-tandem mass spectrometry(GC-MS/MS)method for the determination of clotrimazole residues in animal-derived food(Pork,chicken,pig fat,pig heart,pig liver,pig kidney)was established.The samples were extracted with accelerated solvent extraction,and cleaned up by gel permeation chromatography.HP-5 MS chromatographic column(30 m×0.25 mm×0.25μm)was used for separation,multi-reaction monitoring(MRM)mode detection,and isotope internal standard method for quantification.Results showed that there was a good linearity for clotrimazole in the range of 1~100μg/L with a correlation coefficient(R 2)of 0.9995.The limit of quantitation(LOQ,S/N≥10)of the method was 2.0μg/kg.The average recoveries at three spiking levels(2.0,5.0,20.0μg/kg)were 82.6%~116.5%.Relative standard deviation(RSD)were 5.2%~13.5%.This method has high sensitivity and accuracy,and can be used for the confirmation and quantitative analysis of clotrimazole residues in animal-originated foodstuffs.
作者
韩超
胡贝贞
李舟
朱振瓯
沈燕
周秀锦
HAN Chao;HU Beizhen;LI Zhou;ZHU Zhen’ou;SHEN Yan;ZHOU Xiujin(College of Biological and Environmental Engineering,Zhejiang Shuren University,Hangzhou 310015,China;Shaoxing Customs Comprehensive Technical Service Center,Shaoxing 312000,China;Wenzhou Customs Comprehensive Technical Service Center,Wenzhou 325027,China;Zhoushan Customs Comprehensive Technical Service Center,Zhoushan 316000,China)
出处
《食品工业科技》
CAS
北大核心
2021年第5期216-220,共5页
Science and Technology of Food Industry
基金
浙江树人大学人才引进基金项目(2019R024)。
关键词
动物源食品
克霉唑
残留
同位素稀释
气相色谱-串联质谱法
animal-derived food
clotrimazole
residue
isotope dilution
gas chromatography-tandem mass spectrometry
