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1、UHPLCLTQOrbitrap鉴定苦碟子注射液化学成分及其在大鼠血浆中的移行成分[摘要]应用UHPLCHRMSn技术分析检测苦碟子注射液中原型成分及其在大鼠体内的代谢物。尾静脉注射苦碟子注射液后,收集给药前后的大鼠血浆,经固相萃取进行处理后,采用ACQUITYUPLCBEHC18(21mmX100mm,17um)色谱柱和01%甲酸水溶液(A)乙腊(B)流动相系统进行梯度洗脱。应用LTQOrbitrap质谱负离子模式检测苦碟子注射液中的化学成分以及血浆样品中的原型成分和代谢产物。根据精确相对分子质量数据和多级质谱碎片,结合对照品比对,从
2、苦碟子注射液中分析鉴定了53个成分,包括18个有机酸、15个黄酮、18个倍半站内酯、2个核甘;从大鼠血浆中分析检测了38个原型及代谢产物,主要代谢途径为甲基化、羟基化、水解、葡萄糖酸酸化及它们的复合反应等。应用UHPLCLTQOrbitrap高分辨液质联用技术较为全面地阐明了苦碟子注射液化学成分及其在大鼠血浆中的移行成分,为进一步研究苦碟子注射液体内代谢过程以及药效物质基础提供了科学依据。[关键词]苦碟子注射液;液质联用技术;化学成分;代谢产物鉴定Rapidcharacterizationofchemicalconstituentsan
3、dratsmetabolitesofKudieziinjectionbyUHPLCLTQOrbitrapLlUSiyil,ZHANGXiupingl,SHANGZhanpengl,WANGFeil,ZHANGXiaoxinl,ZHANGJiayu2*,LUJianqiu3*(1SchoolofChinesePharmacy,BeijingUniversityofChineseMedicine,Beijing100102,China;2BeijingInstitutionofChineseMedicine,BeijingUniversit
4、yofChineseMedicine,Beijing100029,China;3LibraryofBeijingUniversityofChineseMedicine,Beijing100029,China)[Abstract]ArapidandsensitiveUHPLCHRMSnmethodwasusedfortheidentificationofKudieziinjectionanditsmainmetabolitesinratplasmaAfterthetailintravenousinjectionofKudiezi,ACQU
5、ITYUHPLCBEHC18(21mmX100mm,17um)wasused,with01%formicacidacetonitrilesolutionasthemobilephaseforgradientelutionKudieziinjectionandplasmaweredetectedbyESILTQOrbitrapequippedwithanESIionsourceinanegativemodeBasedontheaccuratemassmeasurements,theretentiontimeandthemassfragme
6、ntationpatterns,atotalof53compoundsweretentativelyidentifiedandcharacterizedFurthermore,metabolitesinratplasmaaftertheintravenousadministrationofKudieziinjectionwerealsoanalyzedAtotalof38compoundswereidentified,including27prototypesand11metabolitesthroughmetabolicpathway
7、sofmethylation,glucuronideconjugation,sulfateconjugationandhydrolysisAsaresult,UHPLCLTQOrbitraptechniquewasappliedtocomprehensivelyexpoundKudieziinjection'schemicalcomponentsandconstituentsmigratingtoratplasma,andprovidescientificbasisforfurtherstudiesonKudieziinjection1
8、sinvivometabolicprocessandeffectivematerialbase[Keywords]Kudieziinjection;UHPLCLTQOrbitrap;chemicalcons