液相色谱-串联质谱测定枸杞、大青叶等中药材中6种黄曲霉毒素.pdf

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1、JOURNAlOFINSPECTIONANDQUARANTINE检验检疫学刊v0Il24N0．42014年第4期液相色谱一串联质谱测定枸杞、大青叶等中药材中6种黄曲霉毒素聂福平易廷辉唐柏彬杨俊王昱1,2郗存显李贤良王国民(1重庆m入境检验检疫局／重庆市进出口食品安全工程技术研究中心重庆400020；2．重庆大学生物医学工程学院3．重庆市农业环境保护监测站)摘要建立了中药材中6种黄曲霉素毒素的液相色谱串联质谱测定方法。中药材样品经粉碎后，采用70％的甲醇溶液高速搅拌、超声提取，提取液经免疫亲和柱净化后采用液

2、相色谱一串联质谱仪测定黄曲霉毒素，外标法定量。可同时检测样品中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、黄曲霉毒素M1、黄曲霉毒素M2等6种黄曲霉毒素。方法的检出限为0I3t．tg／kg，定量限为1ug／kg，各基质在1p-g／kg、51．tg／kg、10ug／kg等3个水平的添加回收率(n=5)为78．9％．100_2％，相对标准偏差为4．2％．12．6％。该方法的检测速度快，基质干扰较少，结果准确、可靠，定量限可满足国内外对中药材黄曲霉毒素相关限量的要求。关键词液相色谱．串联质谱

3、；中药材；黄曲霉毒素中图分类号0657．7Determinationof6AflatoxinsinChineseHerbsbyLiquidChromatographyTandemMassSpectrometryNieFuping一，YiTinghui，TangBobin，YangJun，WangYu，XiCunxian，LiXianliang，WangGuominf】．ChongqinEntry—ExitInspectionandQuarantineBureau／ChongqingImportandExp

4、ortFoodSafetyEngineeringTechnologyResearchCenter,Chongqing，400020；2．CollegeOfBioengineering，ChongqingUniversity；3．ChongqingMunicipalEnvironmentalProtectionMonitoringStationofAgriculture1Abstract：Liquidchromatographytandemmassspectrometrymethodwasestablish

5、edtodetermineaflatoxinsof6Chineseherbssamplesaftercrushing，highspeedstirring，ultrasonicextractionwith70％methanolsolution，wereextracted．Theextractionswerepurifiedbyimmuneafinitycolumnandthenaflatoxinwasdeterminedbyliquidchromatography—tandemmassspectrometr

6、y(LC／MS／MS)fwithexternalstandardmethodofquantitation．ThemethodcoulddetectaflatoxinB1，aflatoxinB2，aflatoxinG1，aflatoxinG2，aflatoxinM1andM2ofsamplesatthesametime．Thelimitofquantification(LOQs)ofthe6aflatoxinwere1gg／kg，andthelimitofdetection(LOD)，0_3gg／kg．Th

7、eaveragerecoveriesofthe6aflatoxinsspikedinChineseherbs(Wolfberry,Folium，Citrus，Astragalus)rangedfrom78．9％tol00．2％atthethreespikedlevelsof1．0，5．0，10．Ogg／kgrespectively,andtherelativestandarddeviations(RSDs，n5)werebetween4．2％and12．6％．Themethodisrapid，sensit

8、iveandaccurate，andsuitableforthedeterminationofthe6aflatoxinsinChinesemedicines．Thequantificationlimitsofaflatoxinscanmeetthedomesticandforeignrequirements．KeyWords：LC—MS／MS；ChineseHerbalMedicine1前言中药的生产加工过程缺乏监管力度，也