SPE结合UPLC-MS/MS同时测定半夏曲中24种真菌毒素含量  

Simultaneous Determination of 24 Mycotoxins in Pinelliae Rhizoma Fermentata Using SPE and UPLC-MS/MS

作　　者：南文萍 倪倩 张俐 孙晶 冯有龙 NAN Wenping;NI Qian;ZHANG Li;SUN Jing;FENG Youlong(College of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023,China;Jiangsu Institute for Food and Drug Control,Nanjing 210019,China)

机构地区：[1]南京中医药大学药学院,江苏南京210023 [2]江苏省食品药品监督检验研究院,江苏南京210019

出　　处：《现代中药研究与实践》2023年第3期59-65,共7页Research and Practice on Chinese Medicines

基　　金：江苏省药品监督管理局科研计划课题项目(202010)。

摘　　要：目的 建立固相萃取-超高效液相色谱-串联质谱法测定半夏曲中24种真菌毒素的方法。方法 样品经84%乙腈水溶液提取后经Oasis HLB固相萃取柱净化,Agilent Poroshell 120 EC-C_(18)色谱柱(150 mm×2.1 mm,2.7μm)分离,0.1%甲酸水-乙腈为流动相进行梯度洗脱,采用基质匹配外标法进行定量分析。结果 24种真菌毒素在各自浓度范围内线性关系良好,相关系数为0.998 8~1.000 0,检测限为0.02~4.17μg/kg,定量限为0.03~9.92μg/kg。加标水平下的回收率为69.20%~118.20%,RSD为0.51%~12.98%。精密度、重复性和稳定性均符合相关要求。采用所建立的方法对半夏曲样品进行检测,10批半夏曲被检出8种真菌毒素,污染水平为0.30~115.55μg/kg。结论 该方法简便、灵敏、准确,适用于半夏曲样品的检测。Objective To develop a method based on Solid Phase Extraction(SPE) and Ultra performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS) for determination of 24 mycotoxins in Pinelliae Rhizoma Fermentata.Methods Samples were extracted with 84% acetonitrile aqueous solution and purified by Oasis HLB cartridge.Then the target compounds were separated on an Agilent Poroshell 120 EC-C_(18)column(150 mm × 2.1 mm,2.7 μm) with mobile phase of 0.1% formic acid aqueous and acetonitrile.Finally,24mycotoxins were quantified by the matrix-matched external standard method.Results The proposed method showed a good linear relationship of the 24 mycotoxins in a concentration range,with correlation coefficients(r) were 0.998 8-1.000 0.The limits of detection(LOD) ranged was 0.02-4.17 μg/kg.The limits of quantitation(LOQ) ranged was 0.03-9.92 μg/kg.The recoveries ranged from 69.20% to 118.20% at three levels,with the RSD were 0.51% to 12.98%.Precision,repeatability and stability met relevant requirements.The established method was applied to detect 24 mycotoxins in Pinelliae Rhizoma Fermentata.8 kinds of mycotoxins were detected in 10batches and the contamination level was 0.30-115.55 μg/kg.Conclusion The method is sensitive,accurate and suitable for the detection of Pinelliae Rhizoma Fermentata.

关 键 词：固相萃取 超高效液相色谱-串联质谱 真菌毒素 半夏曲 

分 类 号：R284.1[医药卫生—中药学]