同位素稀释气相色谱-串联质谱法测定动物源食品中克霉唑残留量

韩超; 胡贝贞; 李舟; 朱振瓯; 沈燕; 周秀锦

doi:10.13386/j.issn1002-0306.2020030010

同位素稀释气相色谱-串联质谱法测定动物源食品中克霉唑残留量

Determination of Clotrimazole Residue in Animal-Derived Food by Gas Chromatography-Tandem Mass Spectrometry with Isotope Dilution

摘要

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×0.25 μm）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1~100 μg/L浓度范围内线性良好，决定系数（R²）为0.9995，定量限（LOQ，S/N≥10）为2.0 μg/kg。在2.0、5.0、20.0 μg/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。

Abstract: 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×0.25 μm)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 1~100 μg/L with a correlation coefficient(R²)of 0.9995. The limit of quantitation(LOQ,S/N≥10)of the method was 2.0 μg/kg. The average recoveries at three spiking levels(2.0,5.0,20.0 μg/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.