免疫亲和净化-液相色谱-串联质谱法测定广式莲蓉月饼中黄曲霉毒素

Determination of aflatoxins in moon paste cake containing lotus seed produced in Canton by liquid chromatography-tandem mass spectrometry with immunoaffinity purification

目的建立广式莲蓉月饼中的4种黄曲霉毒素（黄曲霉毒素B1、B2、G1、G2）定性和定量的液相色谱-串联质谱检测方法。方法样品经甲醇-水（7:3,v:v）提取后,用免疫亲和柱净化,经甲醇洗脱,在C18色谱柱上梯度洗脱分离,采用电喷雾正离子多反应监测（MRM）模式测定。结果标准曲线在0.120.0 ng/mL范围内线性良好;用本法测定4种黄曲霉毒素的回收率在78.4%107.8%之间,相对标准偏差在2.5%9.8%之间。采用该方法对市售5种广式莲蓉月饼中黄曲霉毒素进行分析,其中1份月饼样品能够检测到含有少量的黄曲霉毒素B1（1.2μg/kg）和B2（0.21μg/kg）。结论该方法具有简单快速,准确可靠等特点,适用于广式莲蓉月饼中4种黄曲霉毒素的同时测定。

Objective A method for the determination of four aflatoxins in moon paste cake containing lotus seed produced in Canton using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. Methods The sample was extracted with methanol-water (7:3, v:v) solution, followed by a cleanup procedure with immunoaffinity column, and then eluted with 1 mL methanol. Four aflatoxins were separated on a C18 column within 7 min using a mobile phase of acetonitrile and ammonium acetate solution and then detected using electrospray ionization (ESI) MS/MS in positive ion mode with multiple reaction monitoring (MRM). Results The linear ranges of aflatoxin were 0.1~20.0 ng/mL, and the recovery rates for the four aflatoxins were 78.4%~107.8%, while the relative standard deviations were 2.5%~9.8%. Little amounts of aflatoxin B1 (1.2 μg/kg) and B2 (0.21 μg/kg) were detected in one of five moon paste cakes containing lotus seed using this method. Conclusion The developed method is simple, fast, accurate, and it can be applied for the simultaneous determination of four aflatoxins in Cantonese moon paste cake.