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1、HPLC法测定患者血浆中氯吡格雷羧酸代谢产物的血药浓度刘丽娜1*,夏泉2,3,黄燕2,许杜娟1#,2,3(1.安徽医科大学药学院,2.安徽医科大学第一附属医院药剂科,3.国家中医药管理局中药化学三级实验室,安徽合肥230032)摘要:目的建立一种简易快速的HPLC-UV法测定人血浆中氯吡格雷羧酸代谢产物(CCA)的浓度。方法以苯妥英钠为内标,血浆样品经6%高氯酸液-液萃取。使用HypersilODS2(4.6×250mm,5μm),流动相为(0.05M磷酸二氢钾,三乙胺调PH至5.7):乙腈(78:22)。紫外检测羧酸氯吡格雷(CCA)的波长为220nm,流速1.0ml/min,柱温50℃。
2、结果羧酸氯吡格雷(CCA)血药浓度范围在0.10-8.0μg/ml范围内线性关系良好(r=0.9995);平均回收率为100.75%;分析方法最低检测线0.05μg/ml。日内、日间RSD均<3%,冻融稳定性RSD均<10%(n=5)。结论本方法简便,准确,灵敏度高,专属性和稳定性较好,适用于氯吡格雷制剂的临床研究和药动学研究。关键词:氯吡格雷;氯吡格雷羧酸代谢产物;高效液相色谱法;血药浓度High-performanceliquidchromatographicdeterminationofinactivecarboxylicacidmetaboliteofclopidogrelinhum
3、anplasmaLIULina1*,XIAQuan2,3,HUANGYan2,XUDujuan1#,2,3,(1.SchoolofPharmacy,AnhuiMedicalUniversity,2.DepartmentofPharmacy,theFirstAffiliatedHosp-italofAnhuiMedicineUniversity,3.Third-GradePharmaceuticalChemistryLaboratoryofStateAdministrationofTraditionalChineseMedicine,AnhuiHefei230032,China)ABSTRAC
4、T:ObjectiveToestablishasimpleandrapidmethod(HPLC-UV)forthedeterminationofcarboxylicacidmetaboliteofclopidogrel(CCA)inhumanplasma.MethodTheanalyticalprocedureinvolvesliquid–liquidextractionoftheanalyteandaninternalstandard(phenytoinsodium)withchemicalreagent-6%perchloricacid.Theseparationwasachieved
5、usingHypersilODSC18(4.6×250mm,5μm)analyticalcolumnwithmobilephaseconsistingof0.05Mphosphatebuffercontainingtriethylamine(pH5.7)andacetonitrile(78:22v/v)atdetectorwavelengthof220nm.Theflowratewas1.0ml/minandthecolumntemperaturewassetat50℃.ResultAgoodlinearitywasshownintheconcentrationrangeof0.10–8.0
6、μg/mL(r=0.995);theaveragerecoverywas100.75%;theLOQwasfoundtobe0.05μg/ml.Boththeinter-dayandintra-dayRSDwerelowerthan3%;thefreeze-thawstabilityRSDwaslessthe10%(n=5).ConclusionThemethodwasconvenient,reliable,sensitivewhichcouldbeappliedintheclinicalinvestigationandpharmacokineticstudyofclopidogrel.KE
7、YWORDS:clopidogrel;carboxylicacidmetaboliteofclopidogrel;HPLC;concentration氯吡格雷(clopidogrel)是一种新型的噻吩并吡啶类衍生物,具有抗血小板聚集作用及抗血栓形成作用。其作用机制是通过选择性地与血小板表面ADP受体结合来抑制血小板的聚集,目前它已被广泛应用于冠脉支架植入术中术后预防急、慢性血栓形成[1]。氯吡格雷为前体药在体