HPLC-MS/MS法测定中药桃仁中黄曲霉毒素G₂、G₁、B₂、B₁

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,4 μm)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/z 331.1→313.1、m/z 329.1→243.1、m/z 315.0→287.1、m/z 313.1→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 aflatoxin G₂,G₁,B₂,B₁ in Persicae Seme n. Methods: Aflatoxins were extracted by 70% methanol,purified by an immunoaffinity column and then separation was carried on a Kromasil C₁₈ (2.0 mm×50 mm,4 μm) column with a mobile phase of methanol-10 mmol·L^-1 formic ammonate(by a gradient program) at a rate of 0.5 mL·min^-1.Aflatoxins were analysed by HPLC-triple quadrupole MS with an ESI ion source in MRM mode,the ion combinations of m/z 331.1→313.1,m/z 329.1→243.1,m/z 315.0→287.1,m/z 313.1→241.0 were used to qualify aflatoxin G₂,G₁,B₂,B₁,respectively. Results: Good linear relationships were obtained within the ranges of 0.375-30 pg for aflatoxin G₂ and B₂, and 1.25-100 pg for aflatoxin G₁ and B₁.The recoveries were between 88.5%-103.9%. Conclusion: The method is sensitive, rapid, accurate and specific for the determination of aflatoxins in traditional Chinese medicine Persicae Semen.