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目的:建立同时测定不同中药中真菌毒素玉米赤酶烯酮(ZON)和α-玉米赤霉烯醇(α-ZOL)的高效液相色谱法,并采用高效液相色谱-串联质谱法(HPLC-ESI-MS/MS)对阳性结果进行确证。方法:样品经甲醇-水溶液(80:20,v/v)提取,免疫亲和柱净化,C18分析色谱柱分离,以水-乙腈(50:50,v/v)为流动相,检测波长236nm,测定结果采用HPLC-ESI-MS/MS进行确证。结果:在0.02-2.50μg/mL范围内,ZON和α-ZOL的线性相关系数均为0.9998。通过添加回收试验,ZON 3个添加水平的回收率为83.8%-98.1%,相对标准偏差为0.9%-7.3%;α-ZOL 3个添加水平的回收率为88.4%-95.5%,相对标准偏差为1.9%-6.2%。ZON和α-ZOL的定量限(S/N=10)分别为18μg/kg和15μg/kg。结论:该方法简便,准确,适用于中药中微量真菌毒素ZON和α-ZOL的检测。
OBJECTIVE: To establish a HPLC method for the simultaneous determination of myricetin, ZON and α-ZOL in different traditional Chinese medicines (TCMs), and to establish a HPLC-MS / -ESI-MS / MS) to confirm the positive result. METHODS: The samples were extracted with methanol-water (80:20, v / v), purified by immunoaffinity column and separated by C18 column. The mobile phase was water-acetonitrile (50:50, v / v) The results were confirmed by HPLC-ESI-MS / MS. Results: The linear correlation coefficients of ZON and α-ZOL were 0.9998 in the range of 0.02-2.50μg / mL. The recoveries of three levels of ZON were 83.8% -98.1% and the relative standard deviations (RSDs) were 0.9% -7.3% by adding recovery test. The recoveries of three ZON supplementation levels were 88.4% -95.5%, the relative standard deviations 1.9% -6.2%. The limits of quantitation (S / N = 10) for ZON and α-ZOL were 18 μg / kg and 15 μg / kg, respectively. Conclusion: The method is simple and accurate and suitable for the detection of trace mycotoxins ZON and α-ZOL in traditional Chinese medicine.