高效液相色谱-串联质谱法快速测定畜肉中的唑类抗真菌药物

Rapid Determination of Azole Antifungal Drugs in Meat by High Performance Liquid Chromatography Tandem Mass Spectrometry

目的:建立快速测定畜肉中唑类抗真菌药物的高效液相色谱-串联质谱法。方法:样品经乙腈超声提取后,使用Eclipse Plus C18色谱柱(150 mm×4.6 mm,5μm)分离,流动相为乙腈-甲酸铵/甲酸,在HPLCMS/MS上采用多反应监测模式对唑类抗真菌药物进行定性和定量检测。结果:4种唑类化合物在2.0~200.0μg·L^(-1)呈良好线性关系,相关系数R2均≥0.999。在质量浓度为30μg·kg^(-1)、60μg·kg^(-1)、300μg·kg^(-1)的添加水平下,加标回收率为88.9%~99.5%,相对标准偏差在2.92%~8.55%。通过信噪比法计算,该方法检出限为5~10μg·kg^(-1),定量限为15~30μg·kg^(-1)。结论:该方法回收率高,重现性好,灵敏度高,适用于畜肉中唑类抗真菌药物的分析测定。

Objective: A high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) method was established for the rapid determination of azole antifungal drugs in animal meat. Method: After the samples were ultrasonically extracted with acetonitrile, then separated by Eclipse Plus C18chromatographic column(150 mm×4.6 mm,5 μm), and finally determined by HPLC-MS/MS. the multiple reaction monitoring(MRM) mode was used for qualitatively and quantitatively detect azole antifungal drugs. Result: Four azole compounds exhibited good linear relationship in the range of 2.0~ 200.0 μg·L^(-1)besides the correlation coefficients R~2 were both ≥ 0.999. At spiked level of 30 μg·kg^(-1),60 μg·kg^(-1), 300 μg·kg^(-1), the recoveries were ranged from 88.9% to 99.5%, with relative standard deviations(RSDs) of 2.92%~ 8.55%. The detection limit(LOD) and limit of quantitation(LOQ) were 5~ 10 μg·kg^(-1)and 15~ 30 μg·kg^(-1)respectively through signal-to-noise ratio method. Conclusion: The method had high recovery, good reproducibility and high sensitivity, and it was suitable for the analysis and determination of azole antifungal drugs in meat.