食品科学 ›› 2022, Vol. 43 ›› Issue (12): 334-335.doi: 10.7506/spkx1002-6630-20210408-100

• 安全检测 • 上一篇    

QuEChERS结合UPLC-MS/MS法测定畜肉中8 种抗真菌药物残留

黄永桥,宋光林,毛敏霞,杨昌彪,马凯,高亮   

  1. (1.贵州省检测技术研究应用中心,贵州 贵阳 550016;2.贵州省分析测试研究院,贵州 贵阳 550016)
  • 发布日期:2022-07-01
  • 基金资助:
    贵州省科技计划项目(黔科合服企[2019]4001)

Determination of Eight Antifungal Drug Residues in Meat by QuEChERS Extraction Coupled with UPLC-MS/MS

HUANG Yongqiao, SONG Guanglin, MAO Minxia, YANG Changbiao, MA Kai, GAO Liang   

  1. (1. Guizhou Testing Technology Research and Application Center, Guiyang 550016, China; 2. Guizhou Academy of Testing and Analysis, Guiyang 550016, China)
  • Published:2022-07-01

摘要: 建立QuEChERS结合超高效液相色谱-串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法快速测定猪肉、牛肉和羊肉中8 种抗真菌药物(氟康唑、酮康唑、萘替芬、联苯苄唑、克霉唑、益康唑、灰黄霉素、咪康唑)残留量的分析方法。利用加标样品对提取溶剂、提取时间、吸附剂种类、吸附剂用量及加盐量等参数进行优化,在最佳提取和检测条件下,采用正离子多反应监测模式分析和外标法定量,8 种抗真菌药物在7 min内完成测定,在0.05~10.00 ng/mL质量浓度范围内线性关系良好(r>0.998),检出限为0.1 μg/kg,定量限为0.3 μg/kg。在畜肉样品中添加8 种抗真菌药物具有良好的重复性和稳定性,准确度在15%以内,日内(n=6)平均回收率为85.7%~113.6%,日间(n=3)平均回收率为87.6%~107.9%,变异系数为1.2%~14.8%。QuEChERS结合UPLC-MS/MS处理过程简单、快速、高效、准确,可用于畜肉中8 种抗真菌药物残留量的快速定性和定量分析。

关键词: QuEChERS;超高效液相色谱-串联质谱法;畜肉;抗真菌药物

Abstract: An analytical method was developed for the rapid determination of the residues of eight antifungal drugs (fluconazole, ketoconazole, naftifen, bifonazole, clotrimazole, econazole, griseofulvin, and miconazole) in pork, beef and mutton by quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). In this study, several important experimental parameters were effectively optimized using spiked samples, including the type of extraction solvent, extraction time, adsorbent type, adsorbent dosage and salt dosage. Under the optimum extraction and detection conditions, the detection process was completed within 7 minutes in the positive ion multiple reaction monitoring mode and quantification was performed by an external standard method. Good linearity was observed over the concentration range of 0.05–10.00 ng/mL (r > 0.998), the limit of detection (LOD) was 0.1 μg/kg, and the limit of quantitation (LOQ) was 0.3 μg/kg. When this method was used to detect meat samples spiked with the analytes, good repeatability and stability was obtained, with accuracy within 15%, average recoveries of 85.7%–113.6% for the intra-day assay (n = 6) and 87.6%–107.9% for the inter-day assay (n = 3) and coefficient of variation (CV) of 1.2%–14.8%. The QuEChERS-UPLC-MS/MS method is simple, rapid, efficient and accurate, and can be used for the rapid qualitative and quantitative analysis of the eight antifungal drug residues in meat.

Key words: quick, easy, cheap, effective, rugged and safe; ultra-high performance liquid chromatography-tandem mass-spectrometry; meat; antifungal drugs

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