College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China.
Anal Chim Acta. 2010 Apr 7;664(2):165-71. doi: 10.1016/j.aca.2010.02.009. Epub 2010 Feb 23.
An ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous determination of aflatoxins B1, B2, G1, G2, M1 and M2 in traditional Chinese medicines (TCMs) was developed. The approach was characterized in details and a special focus was placed on the recovery rates of isolation procedure in different TCM matrices, i.e. rhizomes and roots, seeds, flowers, grasses and leaves. For this purpose, [(13)C(17)]-aflatoxinB1 was employed as the internal standard and a reliable solid phase extraction-based clean-up method was developed. The observed recovery rates of the six aflatoxins ranged from 85.6% to 117.6% in different matrices. Then, the established method was successfully applied to the determination of the six aflatoxins in various TCMs. For 30 commercial samples analyzed, 16 were contaminated with aflatoxins. The mean levels (incidence) of aflatoxins B1, B2, G1 and G2 in positive samples were 1.40 (68.8%), 1.27 (50.0%), 0.50 (43.8%) and 0.94 (43.8%) microg kg(-1), respectively. Interestingly, aflatoxin M1 was detected in two samples with the maximal content of 0.70 microg kg(-1). No sample was contaminated with aflatoxin M2. Meanwhile, a possible association between the contamination levels and the selected herbs was clarified in the present study.
建立了一种超高效液相色谱-串联质谱法(UHPLC-MS/MS),用于同时测定中药材中黄曲霉毒素 B1、B2、G1、G2、M1 和 M2。该方法进行了详细的特征描述,特别关注不同中药材基质(根茎和根、种子、花、草和叶)中分离程序的回收率。为此,采用 [(13)C(17)]-黄曲霉毒素 B1 作为内标,并开发了一种可靠的基于固相萃取的净化方法。在不同基质中,六种黄曲霉毒素的回收率范围为 85.6%至 117.6%。然后,该方法成功应用于各种中药材中六种黄曲霉毒素的测定。对 30 个商业样品进行分析,其中 16 个样品受到黄曲霉毒素的污染。阳性样品中黄曲霉毒素 B1、B2、G1 和 G2 的平均水平(发生率)分别为 1.40(68.8%)、1.27(50.0%)、0.50(43.8%)和 0.94(43.8%)μg kg(-1)。有趣的是,在两个样品中检测到黄曲霉毒素 M1,其最大含量为 0.70μg kg(-1)。没有样品受到黄曲霉毒素 M2 的污染。同时,本研究还阐明了污染水平与所选草药之间的可能关联。