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1、柱前衍生-固相萃取高效液相色谱法快速测定丙戊酸血药浓度药物分析杂志ChinJPharmAnal2005,25(12)--——1469--——柱前衍生一固相萃取高效液相色谱法快速测定丙戊酸血药浓度孙增先,周金玉,张骞峰(连云港市第一人民医院临床药学研究中心连云港222002)摘要目的:建立柱前衍生一固相萃取高效液相色谱法测定丙戊酸血药浓度分析方法,去除过量未反应的衍生试剂.方法:选择2一溴一对硝基苯乙酮为衍生试剂,环己烷羧酸为内标,采用AccubondSPEC,.小柱处理反应液,Nova—pakC..柱(4m,3.9i
2、nln×150mm)为分析柱;甲醇一水(77:23)为流动相,检测波长为262nnl,流速1mL?min～,柱温25℃.结果:反应液中9o%以上未反应的衍生试剂被去除,内标及丙戊酸衍生物被保留和纯化.内标环己烷羧酸和丙戊酸的保留时间分别为3.0和4.5min,线性范围为16.6～265g?mL～,相关系数为0.9998.平均回收率为99.85%,日内日间误差RSD均小于5.16%.结论:本法快速简便,结果准确,非常适合临床常规监测需要.关键词:柱前衍生;固相萃取;高效液相色谱法;丙戊酸;血药浓度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
