基于HPLC-MS测定牛奶和奶粉中黄曲霉毒素方法的优化

Optimization of Aflatoxin Determination Methods in Milk and Milk Powder by HPLC-MS

[目的]建立液相色谱-质谱联用技术(HPLC-MS)同时检测牛奶和奶粉中的5种黄曲霉毒素B 1、B 2、G 1、G 2、M 1的方法。[方法]样品用含0.5%乙酸乙腈为提取溶剂,通过硫酸镁和氯化钠促进水-乙腈分层,经正己烷除脂净化后用液质联用技术进行检测。[结果]各黄曲霉毒素线性范围为1.0~5.0 ng/mL,确定系数(R 2)均大于0.9990;牛奶加标平均回收率为77.06%~101.28%,RSD为2.38%~7.22%;奶粉加标平均回收率为57.00%~99.86%,RSD为2.00%~8.37%。[结论]该方法可同时测定牛奶和奶粉中的5种黄曲霉毒素,具有操作方便、分析速度快、选择性强、定性准确等优点,可用作牛奶和奶粉中黄曲霉毒素的定量测定。

[Objective]To establish a high performance liquid chromatography-mass spectrometry(HPLC-MS)method for the detection of five aflatoxin B 1,B 2,G 1,G 2,M 1 in milk and milk powder.[Method]The sample was extracted from acetonitrile containing 0.5%acetate,and the water-acetonitrile was stratified by magnesium sulfate and sodium chloride.Then the sample was purified by n-hexane and then detected by HPLC-MS.[Result]There was a good relationship between the area ratios of the monitored ion peaks and the mass concentration linearity in the linear range of 0-5.0 ng/mL.All the R 2 were better than 0.999.The recovery range of milk was 77.06%-101.28%,and RSD was 2.38%-7.22%;the recovery rate of milk powder was 57.00%-99.86%,RSD was 2.00%-8.37%.[Conclusion]The method can be used for the quantitative determination of five aflatoxin in milk and milk powder at the same time,with the advantages of convenient operation,fast analysis,strong selectivity and accurate qualitative determination.