中国药业2025，Vol.34Issue(11)：72-77,6.DOI:10.3969/j.issn.1006-4931.2025.11.015
超高效液相色谱串联质谱法快速筛查土鳖虫及其中药制剂中23种真菌毒素
Rapid Screening of 23 Mycotoxins in Eupolyphaga Steleophaga and Its Chinese Medicinal Preparations by UPLC-MS/MS
摘要
Abstract
Objective To establish an EMR-Lipid QuEChERS pretreatment combined with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for rapid screening of 23 mycotoxins in Eupolyphaga Steleophaga and its Chinese medicinal preparations.Methods EMR-Lipid QuECHERS purification kit was used for sample pretreatment.The chromatographic column was Waters Acquity UPLC® BEH C18 column(100 mm×2.1 mm,1.7 μm),the mobile phase was acetonitrile-water(gradient elution),the flow rate was 0.3 mL/min,the column temperature was 30℃,the automatic sampler temperature was 10℃,and the injection volume was 2 μL.Multiple reaction monitoring(MRM),electric spray ionization(ESI),positive ion and negative ion modes were used for simultaneous detection,the atomization voltage was 5 500 V(positive ion mode)and 4 500 V(negative ion mode),and the ion transfer temperature was 500℃.Results The extraction,purification,and detection analysis of 23 mycotoxins in a single sample could be completed within 60 min.The 23 mycotoxins showed good linearity within their respective concentration range(r≥0.999 0).The limit of detection(LOD)was in the range of 0.1-21.8 μg/kg,and the limit of quantification(LOQ)was in the range of 0.4-72.5 μg/kg.The RSDs of repeatability and stability test results should not exceed 10％(n=6).The average recoveries of 23 mycotoxins were in the range of 71.14％-100.71％,with RSDs of 1.64％-9.23％(n=18).Ten batches of samples have detected mycotoxins,including four batches of Eupolyphaga Steleophaga medicinal materials or decoction pieces and six batches of traditional Chinese medicine preparations containing Eupolyphaga Steleophaga,of which four batches of samples had aflatoxin exceeding the limit standard.Conclusion The method is simple,rapid and accurate,which can be used for rapid screening of 23 mycotoxins in Eupolyphaga Steleophaga and its Chinese medicinal preparations.关键词
超高效液相色谱串联质谱法/土鳖虫/中药制剂/真菌毒素Key words
UPLC-MS/MS/Eupolyphaga Steleophaga/Chinese medicinal preparations/mycotoxins分类
医药卫生引用本文复制引用
胡珀,贾云云,李佳,王萍,王玉,赵祥杰..超高效液相色谱串联质谱法快速筛查土鳖虫及其中药制剂中23种真菌毒素[J].中国药业,2025,34(11):72-77,6.基金项目
江苏省市场监督管理局科技计划项目[KJ2022048]. （）
