液相色譜-質(zhì)譜聯(lián)用法測定人血漿中氯吡格雷的濃度
發(fā)布時間:2018-05-19 14:09
本文選題:氯吡格雷 + 液相色譜-質(zhì)譜法。 參考:《中國臨床藥理學(xué)雜志》2016年18期
【摘要】:目的建立液相色譜-質(zhì)譜聯(lián)用法(HPLC-MS/MS)測定人血漿中氯吡格雷的血藥濃度。方法以硫酸氫氯吡格雷-d4作為內(nèi)標(biāo),色譜柱為Xterra~汶RP_(18)(4.6 mm×100 mm,3.5μm),流動相為乙腈∶水相(0.1%甲酸水溶液)=66∶34,流速為1.0 m L·min~(-1)。三重四極桿質(zhì)譜儀進(jìn)行多反應(yīng)監(jiān)測模式,電噴霧離子源正離子檢測。生物樣品預(yù)處理用乙腈直接沉淀蛋白?疾煸摲椒ǖ膶傩浴(biāo)準(zhǔn)曲線和定量下限、精密度與回收率、穩(wěn)定性、溶血實驗及試驗樣品再分析實驗。結(jié)果線性范圍為5.00~5000.00 ng·L~(-1),最低定量下限為5.00ng·L~(-1);批內(nèi)、批間精密度均在1.28%~9.86%,相對偏差(RE)在-6.19%~14.27%;低、中、高3種濃度氯吡格雷質(zhì)控樣本內(nèi)標(biāo)歸一化的基質(zhì)效應(yīng)分別為(113.69±10.62)%,(104.96±5.23)%,(105.12±4.01)%;提取回收率分別為(103.07±5.75)%,(102.87±14.34)%,(97.76±2.04)%。采血時溶血不影響測定準(zhǔn)確度;試驗樣品再分析實驗準(zhǔn)確度符合要求。結(jié)論本方法是一種特異、快速、靈敏、穩(wěn)定的HPLC-MS/MS,適用于人血漿中氯吡格雷的檢測和藥代動力學(xué)研究。
[Abstract]:Objective to establish a liquid chromatography-mass spectrometry (LC-MS) method for the determination of clopidogrel in human plasma. Methods Clopidogrel d4 sulfate was used as the internal standard. The chromatographic column was Xterra-1 RP_(18)(4.6 脳 100mm ~ (3. 5 渭 m), the mobile phase was acetonitrile (acetonitrile): water phase (0.1% formic acid solution) was 66: 34, the flow rate was 1.0 mL 路min ~ (-1). The triple quadrupole mass spectrometer is used to monitor the multi-reaction and the electrospray ion source is used to detect the positive ion. The protein was precipitated directly by acetonitrile in biological sample pretreatment. The specificity, standard curve and quantitative limit, precision and recovery, stability, hemolysis and sample reanalysis of the method were investigated. 緇撴灉綰挎,
本文編號:1910404
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