摘要
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 aflatoxin G2,G1,B2,B1 in Persicae Semen.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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2011年第5期907-911,共5页
Chinese Journal of Pharmaceutical Analysis
基金
国家科技重大专项课题项目(2009ZX09502-024)
