吡咯里西啶类生物碱的提取与定量分析研究.pdfVIP

158粮食与油脂2024年第37卷第4期

吡咯里西啶类生物碱的提取与定量分析研究

佟晓波，刘广福，周政秀

（辽宁省食品检验检测院，辽宁沈阳110161）

摘要：建立了高效液相色谱-串联质谱法同时检测蜂蜜和茶叶中5种常见吡咯里西啶类生物碱

(PAs)含量的方法。通过对不同净化、富集和分析技术的比较筛选，确定蜂蜜样品经体积分数

0.1%甲酸水溶液提取，茶叶样品经甲醇提取，采用SCX固相萃取柱净化,Ci8色谱柱分离，以体积

分数0.1%甲酸水溶液-体积分数0.1%甲酸乙睛溶液为流动相进行梯度洗脱，正离子模式扫描，

多反应监测模式(MRM)下进行检测,外标法定量。结果表明：5种PAs在一定质量浓度范围内线

101.3%,相对标准偏差(n=6)

偏差(n=6)为2.1%~8.3%。建立的方法可同时检测蜂蜜和茶叶中5种PAs含量。

关键词：生物碱；蜂蜜；茶叶；高效液相色谱-串联质谱法

Studyonextractionandquantitativeanalysisofpyrrolizidinealkaloids

TONGXiao-bo,LIUGuang-fu,ZHOUZheng-xiu

(LiaoningInstituteofFoodInspectionandTesting,Shenyang110161,Liaoning,China)

Abstract:Amethodforsimultaneousdeterminationoffivecommonpyrrolizidinealkaloids(PAs)inhon-

eyandteabyhighperformanceliquidchromatography-tandemmassspectrometrywasestablished.

Throughthecomparisonandscreeningofdifferentpurification,enrichmentandanalysistechnologies,

honeysampleswereextractedbyvolumefraction0.1%formicacidaqueoussolution,teasampleswere

extractedbymethanol,purifiedbySCXsolid-phaseextractioncolumn,separatedbyCiscolumn,gradi-

entelutedwithvolumefraction0.1%formicacidaqueoussolution-volumefraction0.1%formicacid

acetonitrilesolutionasmobilephase,scannedinpositiveionmode,detectedinmultiplereactionmonito-

ringmode(MRM),andquantifiedbyexternalstandardmethod.Theresultsshowedthatthefivekindsof

PAshadagoodlinearrelationshipwithinacertainmassconcentrationrange,andthecorrelationcoeffi-

cientsweregreaterthan0.995.Atthethreespikedlevelsoflow,mediumandhigh,therecoveryrateof

honeymatrixwas81.7%-101.3%,andtherelativestandarddeviation(n=6)was1.7%-5.5%.

Therecoveryr