引用本文:王少敏1,杜春晓1,刘贤贤1,刘冠萍2,毛,丹1,梁云飞2,黄晓静1,朱小凤2,陈钶1,季申1.QuEChERS-超高效液相色谱-串联质谱法同时测定三七中26种真菌毒素[J].世界中医药,2019,(04):. |
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QuEChERS-超高效液相色谱-串联质谱法同时测定三七中26种真菌毒素 |
Simultaneous Determination of 26 Mycotoxins in Notoginseng Radix et Rhizoma by QuEChERS-Ultra-High-performance Liquid Chromatography-Tandem Mass Spectrometry |
投稿时间:2019-03-10 |
DOI:10.3969/j.issn.1673-7202.2019.04.003 |
中文关键词: QuEChERS 真菌毒素 超高效液相色谱-串联质谱法 三七 同时测定 黄曲霉毒素 赭曲霉毒素 恩镰孢菌素 |
English Keywords:QuEChERS Mycotoxins Ultra-High-performance liquid chromatography-tandem mass spectrometry Notoginseng Radix et Rhizoma Simultaneous Determination aflatoxins Ochratoxins Enniatins |
基金项目:国家自然科学基金项目(81603292);科技部重点研发专项(2017YFC1700800);国家中药标准化项目(ZYBZH-C-GX-09) |
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中文摘要: |
目的:采用改良QuEChERS前处理技术,建立了超快速液相色谱-串联质谱(Ultra-High-performance Liquid Chromatography-TandemMass Spectrometry,UHPLC-MS/MS)检测中药三七中26种真菌毒素含量的分析方法。方法:样品用QuEChERS方法进行前处理,经15%甲酸乙腈溶液提取,用混合净化填料净化除杂,采用基质匹配标准曲线结合同位素内标法进行定量分析。结果:在低、中、高3个添加水平下,26种真菌毒素的平均加标回收率为80.1%~116.2%(n=5),平均回收率范围为26种真菌毒素在各自的线性范围内线性关系良好,相关系数(r2)≥0.99,检出限和定量限分别为0.05~6.25 μg/kg和0.2~20.0 μg/kg。结论:该法简单、快速、实用性强,适用于三七中26种真菌毒素的定量分析。 |
English Summary: |
To establish a method for the simultaneous determination of 26 kinds of mycotoxins in traditional Chinese medicine Notoginseng Radix et Rhizoma using a QuEChERS pretreatment procedure coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).Methods:The samples were pretreated with QuEChERS method,extracted with 15% formic acid in acetonitrile,purified by mixed absorbents,as well as analyzed by UHPLC-MS/MS.Matrix-matched calibration curves and internal standards were used for accurate quantification.Results:Satisfactory recoveries at low,medium and high spiked levels were ranged from 80.1% to 116.2%(n=5).Good linear relationships were obtained and the correlation coefficients(r2)were greater than 0.99.The limits of detection(LODs,S/N=3)and quantification(LOQs,S/N=10)ranged from 0.05 μg/kg to 6.25 μg/kg and from 0.2 μg/kg to 20.0 μg/kg,respectively.Conclusion:The proposed method is simple,rapid and valuable,which can be a powerful tool for quantitative analysis of the 26 mycotoxins in Notoginseng Radix et Rhizoma. |
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