摘要
目的:以往测定人血浆中瑞格列奈多采用LC-MS法和LC-MS/MS法,方法灵敏度高,但是由于试验成本较高无法普及,故研究建立人血浆中瑞格列奈浓度测定的HPLC方法。方法:采用高效液相色谱法,色谱柱为Agilent Zorbax C18柱(150mm×4.6mm,5μm),流动相为乙腈-醋酸铵缓冲液(10mmol/mL,pH4.0)(78:22,V/V);流速1mL/min,检测波长245nm,柱温34℃,进样量20μL。结果:血浆中杂质不干扰样品的测定;瑞格列奈血药浓度在2.0~100ng/mL范围内线性关系良好,定量下限为2.0ng/mL;高、中、低3种浓度的日内、日间RSD均〈10%;绝对回收率为83.8%~93.2%,相对回收率92.7%~105.3%。结论:本方法快速、简便、重现性好,可用于瑞格列奈的临床药动学和药效学研究。
Objective: Separation of repaglinide by LC-MS or LC-MS/MS has the advantage of high sensitivity, but its utility is limited for its expensive cost. The method for determination of repaglinide concentration in human plasma by HPLC was established. Method: Separation was performed on Agilent Zorbax C 18(150mm × 4.6 mm, 5mm) column with a mobile phase consisted of acetonitrile and ammonium acetate buffer (10mmol/L, pH4.0) (78:22, V/V) at the conditions of below: flow rate 1 mL/min, column temperature 34℃, detection wavelength 245 nm and injection volume 20 μ L. Results: The linear range of repaglinide was 2.0-100.0ng/mL, and the lower determination limit was 2.0ng/mL. RSDs of intra-day and inter-day were all less than 10%. Absolute recovery was 83.8%-93.2% and relative recovery was 92.7%-105.3%. Conclusion: Our method is rapid, convenient, sensitive and reproducible for clinical pharmacokinetic and pharmacodynamic study of repaglinide.
出处
《药品评价》
CAS
2013年第12期31-33,共3页
Drug Evaluation
基金
"瑞格列奈治疗的Ⅱ型糖尿病患者血药浓度与药效学相关性研究"
2011紫禁城国际药师论坛科研基金资助项目
编号:zjc2011005
"单独应用瑞格列奈治疗的2型糖尿病患者体内血药浓度与药效学相关性研究"
2011南京医科大学科技发展基金面上项目
编号:2011NJMU022