Wang Shufang, Cheng Ling, Ji Shen, Wang Ke
College of Pharmaceutical Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058, China.
College of Pharmaceutical Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058, China.
J Pharm Biomed Anal. 2014 Sep;98:201-9. doi: 10.1016/j.jpba.2014.05.037. Epub 2014 Jun 2.
This work reported an efficient and accurate liquid chromatography tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of seventeen mycotoxins in Puerariae lobatae radix, a frequently used traditional Chinese medicine (TCM). The effects of four different clean-up methods, including TC-M160, TC-T220, Mycosep 227, and QuEChERS method, on the recoveries of mycotoxins were investigated and compared. Finally, TC-M160 was chosen for better recovery and repeatability for mycotoxins analysis. The analytes were separated on an Agilent ZORBAX SB C18 column (4.6mm×250mm, 5μm particle size), and eluted with a mobile phase consisting of (A) water containing 0.1% formic acid and (B) acetonitrile containing 0.1% formic acid at a flow rate of 0.6mL/min. The separated compounds were detected by a triple quadrupole mass spectrometer operating in positive electrospray ionization with multiple reaction monitoring (MRM) mode. The results of method validation accorded with the requirement of analytical method for mycotoxins in COMMISSION REGULATION (EC) No 401/2006. The developed method was successfully applied for determination of mycotoxins in seventeen batches of Puerariae lobatae radix collected from different provinces of China. Three batches of them were found with contamination of mycotoxins AFB1 at (0.751±0.176)μg/kg, T-2 at (1.10±0.01)μg/kg, and T-2 at (0.853±0.044)μg/kg, respectively. The results demonstrated that the proposed method was suitable for monitoring mycotoxins residues in Puerariae lobatae radix.
本研究报道了一种高效、准确的液相色谱串联质谱（LC-MS/MS）方法，用于同时测定常用中药葛根中17种霉菌毒素。研究并比较了四种不同净化方法，即TC-M160、TC-T220、Mycosep 227和QuEChERS方法，对霉菌毒素回收率的影响。最终，选择TC-M160用于霉菌毒素分析，因其具有更好的回收率和重复性。分析物在安捷伦ZORBAX SB C18柱（4.6mm×250mm，5μm粒径）上分离，以由（A）含0.1%甲酸的水和（B）含0.1%甲酸的乙腈组成的流动相，以0.6mL/min的流速进行洗脱。分离的化合物通过在正电喷雾电离和多反应监测（MRM）模式下运行的三重四极杆质谱仪进行检测。方法验证结果符合欧盟委员会法规（EC）No 401/2006中霉菌毒素分析方法的要求。所建立的方法成功应用于测定从中国不同省份采集的17批葛根中的霉菌毒素。其中三批样品分别被发现受到黄曲霉毒素B1（0.751±0.176）μg/kg、T-2毒素（1.10±0.01）μg/kg和T-2毒素（0.853±0.044）μg/kg的污染。结果表明，所提出的方法适用于监测葛根中的霉菌毒素残留。
