固相萃取液质联用测定川产道地药材黄精、麦冬中10种真菌毒素  

Determination of 10 mycotoxins in Polygonati Rhizoma and Ophiopogonis Radix as a genuine regional drug of Sichuan by solid-phase extraction coupled with LC-MS/MS

作　　者：沈立[1] 汤燕[1] 陈铁柱[1] 崔红梅[1] 罗恒[1] SHEN Li;TANG Yan;CHEN Tie-zhu;CUI Hong-mei;LUO Hen(Sichuan Academy of China Medicine Sciences,Chengdu 610041,China)

机构地区：[1]四川省中医药科学院,成都610041

出　　处：《药物分析杂志》2023年第8期1369-1380,共12页Chinese Journal of Pharmaceutical Analysis

基　　金：四川省科技厅重点研发项目“川产道地药材国际标准研究”(2019YFS0025);四川省省级科研院所基本科研业务项目“川产道地中药材黄精、栀子、麦冬农药残留与真菌毒素限量GC-QQQ-MS/HPLC-QQQ-MS检测方法研究”(A-2021N-10)。

摘　　要：目的:建立固相萃取液质联用法同时测定黄精、麦冬中10种真菌毒素(伏马毒素B1、B2、B3,黄曲霉毒素B1、B2、G1、G2,T-2毒素、赭曲霉毒素A,玉米赤霉烯酮)。方法:在黄精、麦冬药材粉末中加入70%甲醇水溶液,涡旋及震荡提取,固相萃取柱(HLB)净化,正离子模式以0.01%甲酸水溶液(含0.5 mmol·L^(-1)乙酸胺)和乙腈-甲醇(50∶50)混合溶液为流动相;负离子模式以0.1%甲酸水溶液-乙腈为流动相,经C18色谱柱梯度洗脱分离,采用电喷雾(ESI)离子源、多反应监测(MRM)及正负离子模式采集数据,以基质匹配标准曲线外标法进行定量。结果:10种真菌毒素线性关系良好,相关系数(r)均≥0.99,麦冬和黄精的方法检测限为0.20~4.00μg·kg^(-1)和0.33~0.67μg·kg^(-1),低、中、高水平加样回收率分别为72.3%~130.8%和69.7%~122.7%;RSD分别为0.50%~7.7%和0.13%~8.7%。22批黄精样品中有一批检出玉米赤霉烯酮,检出值1.48μg·kg^(-1),检出率为5.0%;20批麦冬样品中有14批检出伏马毒素B2,检出值为4.99~378.99μg·kg^(-1),检出率为70.0%。结论:该方法简便、快速,实用性强,适用于黄精、麦冬中10种真菌毒素的检测。Objective:To establish a high-performance liquid chromatography(HPLC)coupled with electros⁃pray ionization(ESI)tandem triple quadrupole mass spectrometry(QQQ/MS)method for the simultaneous determination of multiple residues of ten mycotoxins(fumonisin B1,fumonisin B2,fumonisin B3,aflatoxin G1,aflatoxin G2,aflatoxin B1,aflatoxin B2,T-2 toxin,ochratoxin A and zearalenone)in Polygonati Rhizoma and Ophiopogonis Radix by solid-phase extraction.Methods:Samples were extracted with 70%methanol solution by vortex and oscillation.The concentrated liquid supernatant was purified by a hydrophilic-lipophilic balance(HLB)solid-phase extraction(SPE)column.HPLC separation was performed on an Agilent Eclipse plus C18 column.0.01%formic acid(containing 0.5 mmol·L^(-1)ammonium acetate)and acetonitrile-methanol(50∶50)solution was used as mobile phase in positive mode.0.1%acetic acid-acetonitrile was used as the mobile phase in negative mode.MS/MS was adopted for multiple reaction monitoring(MRM)in the positive/negative mode.The quantification was achieved using matrix-matched standard calibrations as the external standard.Results:Under the optimized conditions,the calibration curve showed good linearity with correlation coefficients above 0.99.The limits of detection(LODs)were 0.20-4.0μg·kg^(-1)(Ophiopogonis Radix)and 0.33-0.67μg·kg^(-1)(Polygonati Rhizoma).The recoveries of 10 mycotoxins at three levels were in the range of 72.3%-130.8%(Ophiopogonis Radix)and 69.7%-122.7%(Polygonati Rhizoma),and the relative standard deviation(RSDs)were 0.50%-7.7%(Ophiopogonis Radix)and 0.13%-8.7%(Polygonati Rhizoma).The result showed that among 14 batch of Polygonati Rhizoma samples,zearalenone was detected in one batch of sample,with a detection value of 1.48μg·kg^(-1)and the detection rate of 5.0%.Amang 20 batches of Ophiopogonis Ra⁃dix samples,fumonisin B2 were detected in 14 batches of samples,with a detection value of 4.99-378.99μg·kg^(-1)and the detection rate of 70.0%.Conclusion:This experiment provides a simple,rapid,and pra

关 键 词：黄精 麦冬 真菌毒素 伏马毒素 T-2毒素 黄曲霉毒素 赭曲霉毒素 玉米赤霉烯酮 固相萃取 高效液相色谱-三重四极杆联用质谱 

分 类 号：R917[医药卫生—药物分析学]