目的 建立超快速液相色谱-串联质谱(UPLC-MS/MS)法检测胎盘灌流液中拉米夫定的浓度。方法 以法莫替丁为内标，胎盘灌流液样本用乙腈沉淀蛋白处理，采用Shim-pack XR-ODS II C18柱(2.0 mm×75 mm，2.2 μm)为分析柱，以甲醇和10 mmol·L-1醋酸铵溶液为流动相进行梯度洗脱，流速为0.4 mL·min-1，采用离子选择性电极离子源正离子模式，多反应监测进行定量分析。结果 本法在1~2 500 ng·mL-1间线性良好，日内日间精密度＜10%，绝对回收率≥72%。结论 本方法快速可靠，结果准确，适用于生物样本中拉米夫定浓度的测定。
Abstract
OBJECTIVE To develop a method for determining the concentration of lamivudine in placental perfusate by employing ultra fast liquid chromatography with tandem mass spectrometry (UFLC-MS/MS). METHODS Famotidine was used as the internal standard. After protein precipitation with acetonitrile, the chromatography was performed on a Shim-pack XR-ODS II C18 column (2.0 mm×75 mm,2.2 μm) with mobile phase consisting of methanol and 10 mmol·L-1 ammonium acetate, gradient elution was used, and the flow rate was 0.4 mL·min-1. Tandem mass spectrometric detection was conducted by using multiple reaction monitoring (MRM) in positive ionization mode with an electrospray ionization interface. RESULTS The calibration curve of lamivudine was linear in the range of 1-2 500 ng·mL-1. The intra- and inter-batch RSDs were less than 10%. The method recovery was more than 72%. CONCLUSION The method is rapid and accurate, which is suitable for the determination of lamivudine in placental perfusate.
关键词
拉米夫定 /
超快速液相色谱-串联质谱法 /
胎盘灌流液
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Key words
lamivudine /
UFLC-MS/MS /
placental perfusate
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中图分类号：
R969.1
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参考文献
HUTSON J R, GARCIA-BOURNISSEN F,DAVIS A,et al.The human placental perfusion model:A systematic review and development of a model to predict in vivo transfer of therapeutic drugs.Clin Pharmacol Ther,2011,90(1):67-76. NANOVSKAYA T N,PATRIKEEVA S,HEMAUER S,et al.Effect of albumin on transplacental transfer and distribution of rosiglitazone and glyburide.J Matern-Fetal Neo M,2008,21(3):197-207. SHAN X Q. Determination the content of lamivudine in human plasma by RP-HPLC. China Pharm(中国药师), 2006, 9 (5): 447-449. ZHANG L J, YAO Y M, SUN J J, et al. Determination the concentration of nevirapine, lamivudine, stavudine, zidovudine, efavirenz in human plasma for simultaneous quantification by HPLC-MS/MS. Chin J Clin Pharmacol(中国临床药理学杂志), 2010, 26(2):133-136. LI Z, DING C G, GE Q H, et al. Determination of lamivudine, zidovudine and nevirrapine in human plasma by LC-MS/MS. Chin J Pharm(中国医药工业杂志), 2010, 41(3):200-204. VALLURU R K, PHANI B R, RAVI K, et al. High throughput LC-MS/MS method for simultaneous determination of zidovudine, lamivudine and nevirapine in human plasma. J Chromatog B, 2013, 23(921):9-14. HIREN N M, ARVIND G, ASHUTOSH P, et al. High throughput LC-MS/MS method for simultaneous quantification of lamivudine, stavudine and nevirapine in human plasma. J Chromatog B, 2007, 853 (2): 320-332. MANISH Y, PURAN S, SAILENDRA G, et al. Selective determination of antiretroviral agents tenofovir, emtricitabine, and lamivudine in human plasma by a LC-MS/MS method for a bioequivalence study in healthy Indian subjects. J Chromatog Sci, 2010, 48(2): 704-713. JOSEPH E R, BRANDON K, LANE R B, et al. Validation of a sensitive LC-MS/MS method for the determination of zidovudine and lamivudine in human plasma. Biomed Chromatogr, 2012, 26(1): 12-20.
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脚注
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基金
国家自然科学基金资助项目(81360108)
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