海峡药学
海峽藥學
해협약학
STRAIT PHARMACEUTICAL JOURNAL
2014年
8期
147-150
,共4页
吲达帕胺%高效液相色谱串联质谱法%血药浓度
吲達帕胺%高效液相色譜串聯質譜法%血藥濃度
신체파알%고효액상색보천련질보법%혈약농도
Indapamide%Liquid chromatography tandem mass spectrometry%Plasma concentration of drug
目的：建立高效液相色谱-质谱联用法测定人血浆中吲达帕胺浓度。方法以非那西丁为内标，血浆样品经乙腈沉淀后，经 HPLC-MSMS分离-分析。采用Venusil MP-C18柱（2.1mm ×150mm，5μm，Agela），以甲醇∶水（10mM 甲酸铵含0.1％甲酸）＝（75∶25，V/V）为流动相；流速：0.3mL· min -1，采用电喷雾离子源（ESI），以多离子反应监测方式（MRM）进行正离子监测，吲达帕胺和内标非那西丁的定量分析离子对分别为m/z 366.1→132.0和 m/z 180.1→138.0。结果吲达帕胺的线性范围为0.359～46.0μg · L -1，定量下限为0.359μg · L -1。方法回收率在85.8％～100.3％，日内和日间精密度均小于10％。结论该方法操作简便、灵敏、准确，适用于吲达帕胺的人体药代动力学研究。
目的：建立高效液相色譜-質譜聯用法測定人血漿中吲達帕胺濃度。方法以非那西丁為內標，血漿樣品經乙腈沉澱後，經 HPLC-MSMS分離-分析。採用Venusil MP-C18柱（2.1mm ×150mm，5μm，Agela），以甲醇∶水（10mM 甲痠銨含0.1％甲痠）＝（75∶25，V/V）為流動相；流速：0.3mL· min -1，採用電噴霧離子源（ESI），以多離子反應鑑測方式（MRM）進行正離子鑑測，吲達帕胺和內標非那西丁的定量分析離子對分彆為m/z 366.1→132.0和 m/z 180.1→138.0。結果吲達帕胺的線性範圍為0.359～46.0μg · L -1，定量下限為0.359μg · L -1。方法迴收率在85.8％～100.3％，日內和日間精密度均小于10％。結論該方法操作簡便、靈敏、準確，適用于吲達帕胺的人體藥代動力學研究。
목적：건립고효액상색보-질보련용법측정인혈장중신체파알농도。방법이비나서정위내표，혈장양품경을정침정후，경 HPLC-MSMS분리-분석。채용Venusil MP-C18주（2.1mm ×150mm，5μm，Agela），이갑순∶수（10mM 갑산안함0.1％갑산）＝（75∶25，V/V）위류동상；류속：0.3mL· min -1，채용전분무리자원（ESI），이다리자반응감측방식（MRM）진행정리자감측，신체파알화내표비나서정적정량분석리자대분별위m/z 366.1→132.0화 m/z 180.1→138.0。결과신체파알적선성범위위0.359～46.0μg · L -1，정량하한위0.359μg · L -1。방법회수솔재85.8％～100.3％，일내화일간정밀도균소우10％。결론해방법조작간편、령민、준학，괄용우신체파알적인체약대동역학연구。
OBJECITIVE To establish a high performance liquid chromatography tandem mass spectrometry ( HPLC-MSMS) method for the determination of indapamide in human plasma.METHODS Plasma samples were precipitated with acetonitrile and determined by HPLC-MSMS using phenacetin as the internal standard.The separa-tion was carried out on a Venusil MP-C18 column(2.1mm ×150mm,5μm) with a mobile phase of methanol-water (including 10mM ammonium formate and 0.1%formic acid) (75∶25) and the flow rate was 0.3mL· min -1.ESI was performed in the MRM positive mode with using target ions at m /z 366.1→132.0 ( indapamide ) and m/z 180.1→138.0 ( phenacetin ) .RESULTS The calibration curve of indapamide was obtained in the range of 0.359 ~46.0μg· L-1 with good linearity ( r>0.99 ).The LLOQ of indapamide was 0.359μg · L-1.The method recovery was more than 85%,the relative recovery was 85%~115%,and the intra and inter day RSDs were less than 10%.CONCLUSION This method is simple ,of good sensitivity and precision ,which is suitable for human pharmacoki-netic studies of indapamide.
