同位素内标-高效液相色谱-串联质谱法检测牛奶及奶粉中黄曲霉毒素M1

Determination of aflatoxin M1 in milk and milk powder by isotope internal standard-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  黄曲霉毒素M1  高效液相色谱-串联质谱法  同位素内标  牛奶  奶粉

英文关键词:aflatoxin M1  high performance liquid chromatography-tandem mass spectrometry  isotopic internal standard  milk  milk powder

中文摘要:

      目的 建立一种高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定奶及奶粉中黄曲霉毒素M1的方法。方法 样品经甲醇溶液提取后, 经离心机离心, 上层清液用MycoSep?226 AflaZon+Multifunctional净化柱净化, 在线添加黄曲霉毒素M1同位素内标后采用LC-MS/MS进行检测。结果 黄曲霉毒素M1在0.05~5.0 μg/L范围内线性关系良好, 相关系数大于0.995; 在0.02、0.05和0.10 μg/L添加水平的回收率为89.02%~118.85%, 相对标准偏差小于7.06%(n=6), 定量限为0.06 μg/kg。结论 该方法快速、准确、灵敏, 适合用于测定奶及奶粉中黄曲霉毒素M1。

英文摘要:

      Objective To establish a method for determination of aflatoxin M1 in milk and milk powder by isotope internal standard-high performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS). Methods After the sample was extracted with methanol solution, it was centrifuged in a centrifuge, and the supernatant was purified with a MycoSep ? 226 AflaZon + Multifunctional purification column, and then separated and detected by LC-MS/MS with isotope internal standard. Results Aflatoxin M1 had a good linear relationship in the range of 0.055.0 g/L, and the correlation coefficient was greater than 0.995. The recoveries at the addition levels of 0.02, 0.05 and 0.10 μg/L were 89.02%118.85%, the relative standard deviations were less than 7.06% (n=6), and the limit of quantification was 0.06 μg/kg. Conclusion This method is rapid, accurate and sensitive, and is suitable for the determination of aflatoxin M1 in milk and milk powder.