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高效液相色譜質(zhì)譜聯(lián)用法同時(shí)測(cè)定人血漿中5種核苷類抗病毒藥物濃度

發(fā)布時(shí)間:2018-08-15 18:59
【摘要】:目的建立LC-MS/MS法同時(shí)測(cè)定人血漿中阿昔洛韋、更昔洛韋、拉米夫定、阿德福韋和恩替卡韋的濃度。方法血漿樣品用乙腈沉淀蛋白后,以噴昔洛韋為內(nèi)標(biāo),用Poreshell C18色譜柱(3.0 mm×50 mm,2.7μm),以甲醇-10mmol·L-1醋酸銨溶液(均含0.2%甲酸)為流動(dòng)相進(jìn)行梯度洗脫,流速為0.3mL·min-1,柱溫為30℃,進(jìn)樣量為10μL,總分析時(shí)間為5 min,用電噴霧離子化源,正離子方式,多反應(yīng)監(jiān)測(cè)(MRM)掃描方式進(jìn)行監(jiān)測(cè),檢測(cè)專屬性、標(biāo)準(zhǔn)曲線與定量下限、精密度與回收率、基質(zhì)效應(yīng)和穩(wěn)定性。結(jié)果血漿中阿昔洛韋、更昔洛韋、拉米夫定的線性范圍為10.0~5 000.0μg·L-1(r0.99),定量下限為10.0μg·L-1;阿德福韋線性范圍為0.50~100.00μg·L-1(r0.996 8),定量下限為0.50μg·L-1;恩替卡韋的線性范圍為0.02~20.00μg·L-1,定量下限為0.02μg·L-1(r0.998 0)。低、中、高3個(gè)質(zhì)量濃度樣本的平均回收率在93.3%~109.8%,日內(nèi)、日間RSD均小于15%,提取回收率在85.6%~92.9%。結(jié)論該方法快速、靈敏、準(zhǔn)確,且專屬性強(qiáng)、重復(fù)性好,適用于同時(shí)測(cè)定人血漿中阿昔洛韋、更昔洛韋、拉米夫定、阿德福韋和恩替卡韋的濃度。
[Abstract]:Objective to establish a LC-MS/MS method for simultaneous determination of acyclovir, ganciclovir, lamivudine, adefovir and entecavir in human plasma. Methods after plasma samples were precipitated with acetonitrile, penciclovir was used as internal standard. Gradient elution was carried out on a Poreshell C18 column (3.0 mm 脳 50 mm ~ (2.7) 渭 m),) with methanol-10 mmol 路L ~ (-1) ammonium acetate solution (both containing 0.2% formic acid) as mobile phase. The flow rate was 0.3mL min-1 and the column temperature was 30 鈩,

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