QuEChERS-超高效液相色谱-串联质谱法测定牛羊肉中36种瘦肉精残留量

Determination of 36 clenbuterol residues in beef and mutton samples by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  多组分瘦肉精  QuEChERS  牛羊肉样品  超高效液相色谱-串联质谱法  食品安全

英文关键词:multi-component clenbuterol  QuEChERS  beef and mutton samples  ultra performance liquid chromatography-tandem mass spectrometry  food safety

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定牛羊肉中36种传统和新型瘦肉精残留量的分析方法。方法 样品酶解后, 用甲酸乙腈溶液进行提取, EMR-Lipid增强型脂质去除剂净化除脂, 与甲酸水溶液(1:1, V:V)混合后过滤。采用ZORBAX Eclipse Plus C18 (2.1 mm×100 mm, 1.8 μm)色谱柱为固定相, 0.1%甲酸水(含5 mmol/L乙酸铵)(A)和乙腈(B)作为流动相进行梯度洗脱, 质谱采用电喷雾正离子模式(electron spray ionization positive mode, ESI+), 动态多反应监测模式(dynamic multiple reaction monitoring, dMRM)进行测定。结果 36种瘦肉精在10 min内完成分离分析, 其在0.5、1.0和5.0 μg/kg添加水平的回收率为62.4%~116%之间, 相对标准偏差(relative standard deviation, RSD)在1.1%~20%之间(n=6), 方法检出限为0.5 μg/kg。结论 该方法简便快速, 准确度和精密度均满足食品检测要求, 适用于牛羊肉中多组分瘦肉精残留量的测定。

英文摘要:

      Objective To establish a method for the determination of 36 traditional and new clenbuterol residues in beef and mutton by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After enzymatic hydrolysis, the sample was extracted with formic acid-acetonitrile mixture, and degreased and purified with EMR-Lipid enhanced lipid remover, it was mixed with formic acid aqueous solution by volume ratio of 1:1 and then filtered. Using ZORBAX Eclipse Plus C18 (2.1 mm×100 mm, 1.8 μm) chromatographic column as the stationary phase, 0.1% formic acid water (containing 5 mmol/L ammonium acetate) (A) and acetonitrile (B) as mobile phases for gradient elution, and electron spray ionization positive mode (ESI+) and dynamic multiple reaction monitoring mode (dMRM) were selected for determination. Results The separation and analysis of 36 target compounds was completed within 10 minutes, and the recoveries at the addition levels of 0.5, 1.0 and 5.0 μg/kg were between 62.4%?116%, and the relative standard deviations (RSDs) were between 1.1%?20% (n=6). The limit of determination of the method was 0.5 μg/kg. Conclusion This method is simple and fast, with its accuracy and precision meeting the requirements of food testing, and is suitable for the determination of multi-component clenbuterol residues in beef and mutton samples.