首页|超高效液相色谱-串联质谱法快速测定建曲中的7个真菌毒素

超高效液相色谱-串联质谱法快速测定建曲中的7个真菌毒素

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目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS法)快速测定中药建曲中7个真菌毒素的残留.方法:样品用含0.1%甲酸的乙腈水溶液超声提取,再用QuEChERS提取盐包和Oasis PRiME HLB固相萃取柱处理,采用WATERS HSST3(100 mm×2.1 mm,1.8 μm)色谱柱分离,流动相A为乙腈,流动相B为5 mmol·L-1甲酸铵水溶液(含0.1%甲酸),梯度洗脱;采用电喷雾(ESI)正离子离子源电离,工作模式为多反应监测模式(MRM).结果:7个真菌毒素在各自的线性范围内呈良好的线性关系,相关系数在0.999 1~0.999 9.平均回收率为83.5%~113.8%,RSD在2.1%~5.2%.10批样品中有3批样品检出黄曲霉毒素B1,其含量最高达到了 6.15 μg·kg-1,最低的为1.32 μg·kg-1.结果提示建曲制品存在严重的安全风险.结论:本文建立了建曲中7个真菌毒素的测定方法,通过超高效液相色谱-串联质谱法可以快速检测建曲中的真菌毒素残留量,可适用于建曲中真菌毒素的风险监测.本文揭示了建曲中存在真菌毒素污染的现状,为中药的安全性控制提供了研究基础,建议有关部门加强相应的监管工作.
Rapid determination of 7 mycotoxin contaminants in Jianqu by UPLC-MS/MS
Objective:To establish a method for determination of 7 mycotoxin contaminants in Jianqu by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods:The samples were extracted with acetonitrile aqueous solution(containing 0.1%formic acid),and purified by QuEChERS ex-traction salt bag and Oasis PRiME HLB solid phase extraction column.The column of UPLC was WATERS HSS T3(100 mm ×2.1 mm,1.8 μm).Mobile phase was acetonitrile-5 mmol·L-1 ammonium formate solution(con-taining 0.1%formic acid)with gradient elution.Ionization mode was electrospray ionization(ESI)with positive mode.The work mode was multiple-reaction monitoring mode(MRM).Results:The developed method provided a good linearity for the 7 mycotoxins with their respective linear rangers.The correlation(r)ranged from 0.999 1 to 0.999 9.The average recoveries ranged from 83.5%to 113.8%,RSDs of 2.1%to 5.2%.Among 10 samples were selected for analysis,aflatoxin B1 was detected from 3 samples at concentration of 1.32 μg·kg-1 to 6.15μg·kg-1.The results indicated that there were serious safety risks in the Jianqu products.Conclusion:This paper establishes a method for the determination of 7 mycotoxins in Jianqu.The residual of mycotoxins in Jianqu can be rapid ly detected by UPLC-MS/MS which is suitable for the risk monitoring of mycotoxins in Jianqu.This article reveals the current situation of mycotoxins contamination in Jianqu,providing a research basis for the safety control of traditional Chinese medicine.It is recommended that the relevant departments should strengthen the corresponding supervision work.

UPLC-MS/MSrapid determinationJianqumycotoxinsquality controltraditional Chinese medicine

朱渊、陆益红、王俊虎

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江苏省食品药品监督检验研究院,南京 210019

中国人民解放军东部战区疾病预防控制中心,南京 210018

超高效液相色谱-质谱法 快速测定 建曲 真菌毒素 质量控制 中药材

江苏省药品监督管理局药品监管科学研究计划中国人民解放军东部战区疾病预防控制中心自主科研项目

2022102023YQFH03

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(3)
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