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目的:建立中药桃仁中黄曲霉毒素G2、G1、B2、B1的HPLC-MS/MS测定方法。方法:样品经有机溶剂提取及免疫亲和柱净化后,以高效液相色谱-串联三重四极杆质谱进行分析测定。采用Phenomenex SB-C18(2.0 mm×50 mm,4μm)色谱柱,流动相为甲醇-10 mmol.L-1醋酸铵溶液,梯度洗脱,流速0.5 mL.min-1;质谱条件为电喷雾离子源(ESI源),正离子模式检测,扫描方式为多反应监测(MRM),黄曲霉毒素G2、G1、B2、B1的定量分析离子分别为m/z331.1→313.1、m/z329.1→243.1、m/z315.0→287.1、m/z313.1→241.0。结果:黄曲霉毒素G2、B2进样量在0.375~30 pg范围内与峰面积呈良好的线性关系,黄曲霉毒素G1、B1进样量在1.25~100 pg范围内与峰面积呈良好的线性关系,r>0.999;回收率在88.5%~103.9%之间。结论:本法灵敏、快速、准确,专属性强,可用于中药桃仁中黄曲霉毒素的测定。
Objective: To establish an HPLC-MS / MS method for determination of aflatoxins G2, G1, B2 and B1 in Peach kernel. Methods: After the samples were extracted with organic solvents and purified by immunoaffinity column, the samples were analyzed by high performance liquid chromatography-tandem triple quadrupole mass spectrometry. The mobile phase was methanol-10 mmol.L-1 ammonium acetate solution with a gradient elution at a flow rate of 0.5 mL · min-1 using a Phenomenex SB-C18 (2.0 mm × 50 mm, 4 μm) column. The mass spectrometry conditions were electrospray ionization Source (ESI source), positive ion mode detection, scanning mode for multiple reaction monitoring (MRM), aflatoxin G2, G1, B2, B1 quantitative analysis of ions were m / z331.1 → 313.1, m / z 329.1 → 243.1, m / z 315.0 → 287.1, m / z 313.1 → 241.0. Results The aflatoxins G2 and B2 showed a good linear relationship with the peak area in the range of 0.375-30 pg. The aflatoxins G1 and B1 showed a good linearity with the peak area in the range of 1.25-100 pg Relationship, r> 0.999; recovery rate between 88.5% ~ 103.9%. Conclusion: This method is sensitive, rapid, accurate and specific, and can be used for the determination of aflatoxin in Peach kernel.