同位素内标-超高效液相色谱-串联质谱技术同时检测新鲜银耳中米酵菌酸和异米酵菌酸

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中文摘要：采用同位素内标-超高效液相色谱-串联质谱技术,建立了一种能够快速、稳定地检测新鲜银耳中米酵菌酸与异米酵菌酸的分析方法.样品中加入自制的混合内标工作液后,用含3％乙酸的正己烷振荡提取,经Oasis MAX柱富集净化,利用Waters Acquity UP-LC BEH C18柱(50 mm×2.1 mm,1.7 μm)进行分离,以乙腈-含0.1％甲酸的水溶液为流动相进行梯度洗脱,采用电喷雾负离子多反应监测模式进行扫描,内标法定量.结果显示,米酵菌酸与异米酵菌酸在1～100 ng/mL范围内的线性关系良好,相关系数的平方(r2)均大于0.999,方法的检出限和定量限分别为0.25和0.5 μg/kg.在0.5、5、50 μg/kg 3个浓度加标水平下,平均加标回收率为94.2％～107.3％,相对标准偏差为2.2％～5.7％.该法准确、灵敏、快速,适用于新鲜银耳中米酵菌酸与异米酵菌酸的检测.

外文标题：Simultaneous Determination of Bongkrekic Acid and Iso Bongkrekic Acid in Freshtremella Fuciformis Using Isotope Internal Standard Method by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

外文摘要：A method,using isotope internal standard method-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),was developed for the simultaneous determination of bongkrekic acid(BA)and iso bongkrekic acid(IsoBA)in fresh tremella fuciformis.After the self-prepared mixed internal standard working solution was added,the fresh tremella fuciformis sample was firstly subjected to shaking extraction by n-hexane containing 3％acetic acid,and then the extract solution was purified and enriched by Oasis MAX cartridges.Acetonitrile and 0.1％formic acid aqueous solution were used as mobile phases,and the gradient elution method was used to separate on a Waters ACQUITY BEH C18(50 mm×2.1 mm,l.7 μm)chromatographic column.The compounds were swept with electrospray ionization source in the negative ion and multiple reaction monitoring(MRM)modes,and analyzed by an internal standard method.The results showed that the compounds achieved great linearity in the linear ranges from 1 ng/mL to 100 ng/mL,with a correlation coefficient(r2)greater than 0.999.The limit of detection(LOD)and the limit of quantification(LOQ)were 0.25 μg/kg and 0.5 μg/kg.The average recoveries in samples spiked with 0.5,5,50 μg/kg BA and IsoBA in fresh tremella fuciformis ranged from 94.2％to 107.3％,while the relative standard deviations(RSDs)were between 2.2％and 5.7％.The method is accurate,sensitive,rapid,and suitable for the detection of BA and IsoBA in fresh tremella fuciformis.

外文关键词：

Ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)Isotope internal standardBongkrekic acid(BA)Iso bongkrekic acid(IsoBA)Fresh tremella fuciformis

作者：

夏宝林、杨娜、殷晶晶、汪仕韬、张维益

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作者单位：

江阴市食品安全检测中心,江苏江阴 214400

关键词：

超高效液相色谱-串联质谱同位素内标米酵菌酸异米酵菌酸新鲜银耳

基金：

江阴市社会发展科技示范项目江阴市社会发展科技示范项目

项目编号：

JY0603A011014230014PBJY0603A011014230027PB

出版年：

2024

DOI：

10.13526/j.issn.1006-6144.2024.01.014

分析科学学报

武汉大学,北京大学,南京大学

分析科学学报

CSTPCD北大核心

影响因子：0.717

ISSN：1006-6144

年,卷(期)：2024.40(1)

参考文献量15