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1、柱前衍生-固相萃取高效液相色譜法快速測定丙戊酸血藥濃度藥物分析雜志ChinJPharmAnal2005,25(12)--——1469--——柱前衍生一固相萃取高效液相色譜法快速測定丙戊酸血藥濃度孫增先,周金玉,張騫峰(連云港市第一人民醫(yī)院臨床藥學(xué)研究中心連云港222002)摘要目的:建立柱前衍生一固相萃取高效液相色譜法測定丙戊酸血藥濃度分析方法,去除過量未反應(yīng)的衍生試劑.方法:選擇2一溴一對硝基苯乙酮為衍生試劑,環(huán)己烷羧酸為內(nèi)標(biāo),采用AccubondSPEC,.小柱處理反應(yīng)液,Nova—pakC..柱(4m,3.9i
2、nln×150mm)為分析柱;甲醇一水(77:23)為流動相,檢測波長為262nnl,流速1mL?min~,柱溫25℃.結(jié)果:反應(yīng)液中9o%以上未反應(yīng)的衍生試劑被去除,內(nèi)標(biāo)及丙戊酸衍生物被保留和純化.內(nèi)標(biāo)環(huán)己烷羧酸和丙戊酸的保留時間分別為3.0和4.5min,線性范圍為16.6~265g?mL~,相關(guān)系數(shù)為0.9998.平均回收率為99.85%,日內(nèi)日間誤差RSD均小于5.16%.結(jié)論:本法快速簡便,結(jié)果準(zhǔn)確,非常適合臨床常規(guī)監(jiān)測需要.關(guān)鍵詞:柱前衍生;固相萃取;高效液相色譜法;丙戊酸;血藥濃度RapidDeterm
3、inationofValproicAcidinSerumbyPrecolumnDerivationHighPerformanceLiquidChromatography,thSolidPhaseExtractionSUNZeng—xian,ZHOUJing—yu,ZHONGQian—fen(No.1hospitalofIAanyungang,JiangsuLianyungang222002,China)Abstractobjective:Toestablisharapidanalysismethodforthedet
4、erminationofvalproicacidinserumbyprecol?umnderivationhighperformanceliquidchromatographywithsolidphaseextraction.Superfluousunreactedderivativereagentwasremovedfromreactionsolution.Methods:2一Bromo一4一nitroacetophenonewasselectedasderivativereagent.Cyclohexanecar
5、boxylicacidwasusedasaninternalstandard.InternalstandardandvalproicacidderivationwereextractedfromreactionsolutionwithaccubondSPECl8column.rnleanalyticalcolumnwasNova—pakCl8col—umn(3.9mm×150mm,4Ixm).rnlemobilephaseconsistedofmethanol—water(77:23).rnledetectionwa
6、ve—lengthwas262nmandtheflowratewas1mL?min~.columntemperaturewas25℃.Results:Morethan90%unreactedderivationreagentwasremovedfromreactionsolution.internalstandardandvalproicacidderivationwereretainedandpurified.rnleretainfiontimeofcyclohexanecarboxylicacidandvalpr
7、oicacidwas3.0and4.5min.re.spectively.rnlelinearrangeofvalproicacidwas16.6—265g?mL_.andcorrelationcoefficientwas0.9998.rnlerelativerecoveriesofvalproicacidwas99.85%.Therelativestandarddeviation(RSD)ofwithindayandbetweendaywerealllessthan5.16%.Conclusion::rnlisme
8、thodisfoundtoberapid,accurate,sensitiveandmoresuitableforclinicalpracticeapplication.Keywords:precolumnderivation,solidphaseextraction,highperformanceliquidchromatography;va