摘要
目的建立中药瓜蒌皮及提取物中6种玉米赤霉烯酮类真菌毒素的超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定方法。方法收集瓜蒌皮样品,采用水煎法制备相应的提取物,用乙腈-水溶剂提取瓜蒌皮样品及提取物中玉米赤霉烯酮类真菌毒素,采用免疫亲和柱净化富集,用UHPLC-MS/MS测定。结果6种玉米赤霉烯酮类真菌毒素在0.25 ng/ml^125 ng/ml线性关系良好(r>0.99),在低、中、高3种加标浓度水平下的回收率为92.17%~104.53%,相对标准偏差为1.02%~4.15%,检出限为0.1μg/kg^0.25μg/kg。样品测定结果显示,在阳性瓜蒌皮和对应水煎提取物中玉米赤霉烯酮类真菌毒素存在一定的转移关系。结论本法灵敏、快速、准确、专属性强,可用于中药瓜蒌皮及提取物中玉米赤霉烯酮类真菌毒素的测定。
Objective To establish a UHPLC-MS/MS method for the determination of 6 zearalenones and related mycotoxins in Chinese herb trichosanthis pericarpium and its extractives.Methods The collected samples of trichosanthis pericarpium and the extractive of corresponding decoction were extracted with acetoniture water solution,purified by zearalenone immnuoaffinitychromatographic column(IAC),and analyzed by UHPLC-triple quadrupole mass spectrometry.Results The correlation coefficients of the 6 mycotoxins were greater than 0.99 within 0.25 ng/ml-125 ng/ml.The recoveries at the three levels of low,medium and high spiked concentrations were within 92.17%-104.53%,and the relative standard deviations were within 1.02%~4.15%.The LODs were in the range of 0.1μg/kg-0.25μg/kg..The actual sample testing results showed that there was a certain relationship between the transfection of zearalenone and related mycotoxins in trichosanthis pericarpium and the extractive of corresponding decoction.Conclusion The method is sensitive,rapid,accurate and specific,which is enough to determine zearalenone and related mycotoxins in trichosanthis pericarpium and its extactives.
作者
王少敏
杜春晓
周恒
毛丹
陈钶
季申
WANG Shao-min;DU Chun-xiao;ZHOU Heng;MAO Dan;CHEN Ke;JI Shen(Shanghai Institute for Food and Drug Inspection,Shanghai 201203,China)
出处
《中国卫生检验杂志》
CAS
2020年第12期1424-1427,共4页
Chinese Journal of Health Laboratory Technology
基金
国家自然科学基金项目(81603292)
上海市科委研发平台专项(18DZ2292200)
上海市科委研发平台专项(18DZ2200900)。
关键词
玉米赤霉烯酮
超高效液相色谱-串联质谱法
瓜蒌皮及提取物
Zeranols
Ultra high performance liquid chromatography-triple quadrupole mass spectrometer
Richosanthis pericarpium and its extacts
