摘要
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.
作者
何雯倩
韦誉
邬晓莹
涂冬漫
HE Wenqian;WEI Yu;WU Xiaoying;TU Dongman(Guangdong Provincial Public Laboratory of Food Industry,Guangzhou 511442,China;Guangdong Food Industry Institute Co.,Ltd.,Guangzhou 511442,China;Guangdong Food Quality Supervision and Inspection Station,Guangzhou 511442,China)
出处
《现代食品》
2022年第23期175-179,共5页
Modern Food
关键词
高效液相色谱-串联质谱
快速测定
畜肉
抗真菌药物
high performance liquid chromatography-tandem mass spectrometry
rapid determination
livestock meat
antifungal drugs