CAJ | 학술논문

目的：建立液质联用色谱法（LC-MS-MS）测定人血浆中非布司他（febuxostate ）浓度。方法空白血浆加非布司他，用乙腈作为沉淀剂，取上清液用于LC-MS-MS分析。分析柱为Thermo Biobasic-8柱（5μm，50 mm ×2．1 mm），流动相为乙腈-10 mmol/L乙酸铵（含0．05％甲酸）（70：30），流速为0．2 ml/min；质谱条件：电喷雾离子化电离源ESI负离子检测，喷雾电压（SP）3500 kV，鞘气（SGP）流速10 Arb，辅助气（AGP）流速45 Arb，毛细管温度（TEM）270℃；非布司他和内标苯扎贝特的碰撞能量分别为10 eV、18 eV；选择反应监测（ SRM ）分别测定非布司他和内标苯扎贝特负离子m/z 315→271和m/z 360→274。结果非布司他在10～8000μg/L检测浓度范围内呈良好线性关系（r＞0．99），最低定量限（LLOQ）为10μg/L，绝对回收率在85％以上，高中低3种浓度的日内和日间RSD＜15％。结论该方法操作简便、灵敏、准确，适用于临床非布司他的血药浓度监测及其药动学研究。
목적：건립액질련용색보법（LC-MS-MS）측정인혈장중비포사타（febuxostate ）농도。방법공백혈장가비포사타，용을정작위침정제，취상청액용우LC-MS-MS분석。분석주위Thermo Biobasic-8주（5μm，50 mm ×2．1 mm），류동상위을정-10 mmol/L을산안（함0．05％갑산）（70：30），류속위0．2 ml/min；질보조건：전분무리자화전리원ESI부리자검측，분무전압（SP）3500 kV，초기（SGP）류속10 Arb，보조기（AGP）류속45 Arb，모세관온도（TEM）270℃；비포사타화내표분찰패특적팽당능량분별위10 eV、18 eV；선택반응감측（ SRM ）분별측정비포사타화내표분찰패특부리자m/z 315→271화m/z 360→274。결과비포사타재10～8000μg/L검측농도범위내정량호선성관계（r＞0．99），최저정량한（LLOQ）위10μg/L，절대회수솔재85％이상，고중저3충농도적일내화일간RSD＜15％。결론해방법조작간편、령민、준학，괄용우림상비포사타적혈약농도감측급기약동학연구。
Objective To establish a LC-MS-MS method for determining febuxostate in human plasma .Methods Febuxostate added into blank plasma was sedimented by acetonitrile , and the supernatant was determined by LC-MS-MS.Analytical column was Thermo Biobasic-8,5 μm,50 mm ×2.1 mm(ID).The mobile phase consisted of acetonitrile-10 mmol/L ammonium acetate (0.05%acid=70:30 at a flow rate of 0.2 ml/min.Mass spectrum conditions:ESI-was performed in the SRM mode using target ions m/z 315→271 (10 eV)(febuxostate), m/z 360→274 (18 eV)(bezafibrate), SP 3 500 kV, SGP 10 Arb, AGP45 Arb, TEM 270℃.Results The calibration curve was linear over the range of 10-8 000 μg/L.The LLOQ of Febuxostate in plasma was 10 μg/L.The extracted recovery was >85%.The intra-and inter-day RSD were <15%.Conclusion The method was sensitive , simple and accurate to deter-minate febuxostate plasma concentration and to study pharmacokinetics of febuxostate .