超高效液相色谱检测黄樟素方法研究.pdf

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1、别事技术2015年第40卷第3期ForensicSconceandTechnology·论著·DOI：10．16467／j．1008—3650．2015．03．008超高效液相色谱检测黄樟素方法研究翟晚枫，李彭，贺剑锋，高利生(公安部物证鉴定中心，北京100038)DeterminationofSafrolebyUltraPerformanceLiquidChromatographyZHAIWanfeng，LIPeng，HEJianfeng，GAOLisheng(InstituteofForensi

2、cScience,MinistryofPublicSecurity,Beijing10003&China)ABSTRACT：Toestablishaquantitativemethodfordeterminationofsafrolebyultraperformanceliquidchromatography(UPLC)．safrolesamplesweredilutedbymethanol，oscillatedwiththespeedof1500r／minforl0minutesorultraso

3、und—assistedoscillatedfor3minutes．thenfilteredthesolutionwith0．22ummembraneanddrew1。5mLforautomaticinjection．TheseparationwasoptimizedandperformedonaShimadzuODS—SPcolumn(250mmx4．6nnn，5m)．Themobilephasewaspurewater(A)一acetonitrile(B)andthemodeofelutionw

4、asgradient．Theinitialconditionwas60％B，andthegradientsteepnessoforganicphasewas0．5％／minbetween0-13min，thentheorganicphase’scontentwasraisedto95％immediatelyandheldonfor7minutes．Thecompletegradientelutionprocedurewas60％Br0．01min)-66．5％Bf13min)-95％B(13．01m

5、in)～95％B(20min)．Flowratewassetas1mL／min．columntemperaturewassetas40ocandiniectionvolumewassetas5uL．TheprimaryquantitativewavelengthofUVdetectorwassetas210nmandtheauxiliaryonewassetas235nm．Whentheorganicphase’sinitialcontentincreased，theoreticalplatenum

6、berandretentiontimedecreased，butpeakheightincreased．Whenthegradientsteepnessincreased，theoreticalplatenumberandpeakheightincreased，butretentiontimedecreased．Usingtheoptimizedmethod，goodlineafitywasachievedovertherangeof2~200gg／mL．Externalstandardworkin

7、gcurveY=1833．39X+5675．32．rz>0．9999．Limitofdetectionwas0．1~tg／mLundertheconditionofS／N>3．Theprecisionwasgoodwiththeintra—dayRSDslessthan1．26％andinter-dayRSDslessthan2．08％．Theaccuracywasalsosatisfied．Therecoveryrateswereintherangeof98．21％tO102．18％．withRS

8、Dsbetween0．35％and0．96％．Thetestsamplesshowedgoodstabilityunderroomtemperature，freezeconditionandthreecyclesoffreeze．thawcondition．TheRSDsofpeakareaof6samplesplacedatroomtemperaturefor3，6，12，24，48，96hourswerebetween0．35％and1．02％．TheRSDsof