摘要
目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定中药茯苓中74种真菌毒素的残留。方法:样品用1%乙酸溶液和乙腈涡旋提取,再用QuEChERS提取盐包处理,采用WATERS CORTECS C_(18)色谱柱(150 mm×4.6 mm,2.7μm),以0.05%甲酸溶液(含10 mmol·L^(-1)甲酸铵)(A)-0.05%甲酸的甲醇溶液(含10 mmol·L^(-1)甲酸铵)(B)为流动相,梯度洗脱;采用电喷雾电离源,工作模式为多反应监测模式。结果:74种真菌毒素质量浓度在5~200 ng·m L^(-1)范围内呈良好的线性关系,相关系数r>0.9904。平均回收率为61.2%~127.8%,重复性RSD为1.1%~12.0%。10批样品中共有17种真菌毒素残留检出,残留检出范围为0.07~22.02μg·kg^(-1)。结果提示茯苓制品存在严重的安全风险。结论:本文建立了茯苓中74种真菌毒素的测定方法,通过HPLC-MS/MS法可以快速、准确检测茯苓中的真菌毒素残留量,可用于茯苓中真菌毒素的风险监测。
Objective:To establish a high performance liquid chromatography-tandem mass spectrometry(HPLCMS/MS)method for the detection of 74 mycotoxin residues in Poria.Methods:The samples were extracted with 1%acetic acid solution and acetonitrile by vortex and then treated with QuEChERS extraction salt package.The WATERS CORTECS C18 column(150 mm×4.6 mm,2.7μm)was used for gradient elution with 0.05%formic acid solution(containing 10 mmol·L^(-1)ammonium formate)as the mobile phase A and 0.05%formic acid methanol solution(containing 10 mmol·L^(-1)ammonium formate)as the mobile phase B.Electrospray ionization source was used and the working mode was multiple reaction monitoring.Results:The 74 mycotoxins showed good linear relationships within the concentration range of 5200 ng·mL^(-1),with the correlation coefficient r>0.9904.The average recovery rate ranged from 61.2%to 127.8%,and the repeatability RSD varied within the range of 1.1%–12.0%.A total of 17 mycotoxin residues were detected in 10 batches of samples,with the residue range of 0.07-22.02μg·kg^(-1).The results suggested that there were serious safety risks in Poria products.Conclusion:A method for the detection of 74 mycotoxins in Poria is established.The HPLC-MS/MS method can quickly and accurately detect the mycotoxin residues in Poria and can be applied to the risk monitoring of mycotoxins in Poria.
作者
赵欢
吴玉强
罗轶
白桂昌
吕轶峰
ZHAO Huan;WU Yu-qiang;LUO Yi;BAI Gui-chang;LÜYi-feng(Guangxi University of Chinese Medicine,Nanning 530001,China;Guangxi University of Chinese Medicine Bainianle Pharmaceutical Co.,Ltd.,Nanning 530023,China;Guangxi Institute for Drug Control,Nanning 530021,China)
出处
《药物分析杂志》
2025年第12期2152-2165,共14页
Chinese Journal of Pharmaceutical Analysis
基金
广西壮族自治区食品药品监督管理局“科研计划”(桂药监科2022-02)。
关键词
高效液相色谱-串联质谱法
检测
茯苓
真菌毒素
质量控制
high performance liquid chromatography-tandem mass spectrometry
detection
Poria
mycotoxins
quality control
