HPLC法同时测定人血浆中拉米夫定、齐多夫定和奈韦拉平的浓度
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摘要
目的:建立能同时测定人血浆中拉米夫定(3TC)、齐多夫定(AZT)和奈韦拉平(NVP)浓度的方法。方法:血浆用乙腈沉淀处理后,以乙酸乙酯提取后进行高效液相色谱法测定。色谱柱为Agilent XDB-C18,流动相为乙腈-水溶液(梯度洗脱),流速为0.8 ml/min,检测波长为268 nm,柱温为30℃,内标为甲硝唑。结果:3TC、AZT、NVP血药浓度分别在0.05~10μg/ml(r=0.9981)、0.05~10μg/ml(r=0.999 0)、0.1~20μg/ml(r=0.999 3)范围内线性关系良好,定量限分别为0.05、0.05、0.1μg/ml;平均方法回收率分别为96.36%~105.84%、98.73%~101.93%、98.78%~108.07%,日内、日间RSD<8%。结论:本方法简便、快速、准确、灵敏,可用于同时使用3TC、AZT和NVP的艾滋病患者的临床治疗药物监测及药动学研究。
OBJECTIVE: To establish a sensitive and rapid method for the simultaneous determination of lamivudine(3TC),zidovudine(AZT)and nevirapine(NVP)in human plasma. METHODS: The plasma were extracted with ethyl acetate after precipitated by acetonitrile. The determination was performed on Agilent XDB-C18 with mobile phase consisted of acetonitrile-water(gradient elution)at the flow rate of 0.8 ml/min. The detection wavelength was 268 nm,and column temperature was 30 ℃. Metronidazole was used as the internal standard. RESULTS: The linear range of 3TC,AZP,NVP were 0.05-10 μg/ml(r=0.998 1),0.05-10 μg/ml(r=0.999 0),0.1-20 μg/ml(r=0.999 3),respectively;and the limits of quantitation was 0.05,0.05,0.1 μg/ml respectively. the average method recovery were 96.36%-105.84%,98.73%-101.93%,98.78%-108.07%,respectively. The intra-day and inter-day RSD were all <8%。CONCLUSIONS: The method is simple and rapid,accurate,sensitive,and can be used for therapy drug monitoring and pharmacokinetic study of AIDS patients receiving 3TC,AZT and NVP simultaneously.
OBJECTIVE: To establish a sensitive and rapid method for the simultaneous determination of lamivudine(3TC),zidovudine(AZT)and nevirapine(NVP)in human plasma. METHODS: The plasma were extracted with ethyl acetate after precipitated by acetonitrile. The determination was performed on Agilent XDB-C18 with mobile phase consisted of acetonitrile-water(gradient elution)at the flow rate of 0.8 ml/min. The detection wavelength was 268 nm,and column temperature was 30 ℃. Metronidazole was used as the internal standard. RESULTS: The linear range of 3TC,AZP,NVP were 0.05-10 μg/ml(r=0.998 1),0.05-10 μg/ml(r=0.999 0),0.1-20 μg/ml(r=0.999 3),respectively;and the limits of quantitation was 0.05,0.05,0.1 μg/ml respectively. the average method recovery were 96.36%-105.84%,98.73%-101.93%,98.78%-108.07%,respectively. The intra-day and inter-day RSD were all <8%。CONCLUSIONS: The method is simple and rapid,accurate,sensitive,and can be used for therapy drug monitoring and pharmacokinetic study of AIDS patients receiving 3TC,AZT and NVP simultaneously.
引文
[1]中华医学会感染病学分会艾滋病学组.中华医学会第五次全国艾滋病、病毒性丙型肝炎暨全国热带病学术会议论文汇编[C].2011:44.
[2]Nandi U,Das A,Roy B,et al.Development and validation of an HPLC-UV method for simultaneous determination of zidovudine,lamivudine,and nevirapine in human plasma and its application to pharmacokinetic study in human volunteers[J].Drug Test Anal,2013,5(6):485.
[3]Kumar VR,Reddy BR,Sreekanth K,et al.High throughput LC-MS/MS method for simultaneous determination of zidovudine,lamivudine and nevirapine in human plasma[J].J Chromatogr B Analyt Technol Biomed Life Sci,2013(921/922):9.
[4]李周,丁存刚,葛庆华,等.人血浆中拉米夫定、齐多夫定、奈韦拉平的LC-MS/MS法测定[J].中国医药工业杂志,2010,41(3):200.
[5]Herve R,Bernard M,Corinne C,et al.Determination of 19antiretroviral agents in pharmaceuticals or suspected products with two methods using high-performance liquid chromatography[J].J Chromatogr B,2007,850:376.
[2]Nandi U,Das A,Roy B,et al.Development and validation of an HPLC-UV method for simultaneous determination of zidovudine,lamivudine,and nevirapine in human plasma and its application to pharmacokinetic study in human volunteers[J].Drug Test Anal,2013,5(6):485.
[3]Kumar VR,Reddy BR,Sreekanth K,et al.High throughput LC-MS/MS method for simultaneous determination of zidovudine,lamivudine and nevirapine in human plasma[J].J Chromatogr B Analyt Technol Biomed Life Sci,2013(921/922):9.
[4]李周,丁存刚,葛庆华,等.人血浆中拉米夫定、齐多夫定、奈韦拉平的LC-MS/MS法测定[J].中国医药工业杂志,2010,41(3):200.
[5]Herve R,Bernard M,Corinne C,et al.Determination of 19antiretroviral agents in pharmaceuticals or suspected products with two methods using high-performance liquid chromatography[J].J Chromatogr B,2007,850:376.