曹叶中 蔡文

摘要 [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B1、B2、G1、G2、M1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（R2）均大于0.999 0;牛奶加标平均回收率为77.06%～101.28%，RSD为2.38%～722%;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。

关键词 液相色谱-质谱联用技术;牛奶;奶粉;黄曲霉毒素;测定

中图分类号 TS.252.7文献标识码 A文章编号 0517-6611（2021）02-0201-03

doi：10.3969/j.issn.0517-6611.2021.02.054

开放科学（资源服务）标识码（OSID）：

Optimization of Aflatoxin Determination Methods in Milk and Milk Powder by HPLCMS

CAO Yezhong， CAI Wen

（Suzhou Food Inspection and Testing Center， Suzhou， Jiangsu215000）

Abstract [Objective] To establish a high performance liquid chromatographymass spectrometry （HPLCMS） method for the detection of five aflatoxin B1， B2， G1， G2， M1 in milk and milk powder. [Method] The sample was extracted from acetonitrile containing 0.5% acetate， and the wateracetonitrile was stratified by magnesium sulfate and sodium chloride. Then the sample was purified by nhexane and then detected by HPLCMS. [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 R2 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.

Key words High performance liquid chromatographymass spectrometry;Milk;Milk powder;Aflatoxin;Determination

黃曲霉毒素（Aflatoxin，AFT）是由黄曲霉、寄生曲霉和少量特异曲霉产生的次生毒性代谢物[1]，常见类型分别为B1、B2、G1、G2、M1、M2等，其中B1对人类健康的危害最大，被世界卫生组织国际癌症研究机构列为1类致癌物[2]。人们接触黄曲霉毒素的主要来源是污染的食物，在热带和亚热带等湿热地区，黄曲霉毒素对花生、核桃、玉米、稻米、大豆、小麦等粮油产品的污染概率最高[3]。M1主要在牛奶中存在[4]，养殖奶牛的饲料在被AFB1污染后，奶中会产生AFB1的羟基化代谢产物AFM1[5]，对人类健康造成极大威胁。

目前国内外对牛奶和奶粉中的黄曲霉毒素，除了M1之外，其他均未单独制定残留限量标准。现行的行业标准SN/T 1664—2005[6]和国家标准GB/T 23212—2008[7]是采用液相色谱荧光检测法测定牛奶、奶粉中的5种黄曲霉毒素B1、B2、G1、G2、M1。此检测流程需要经过免疫亲和柱净化，再分别利用过溴化吡啶和三氟乙酸进行衍生化处理，最后通过带有荧光检测器的高效液相色谱仪测定[8-9]。……