节点文献
大鼠胆汁中酮洛芬Ⅱ相代谢物酮洛芬葡萄糖醛酸的测定方法
RP-HPLC determination of ketoprofen glucuronides in rat bile liquid
【摘要】 目的:建立 RP-HPLC 法测定胆汁中酮洛芬Ⅱ相代谢物酮洛芬葡萄糖醛酸(S-KPG、R-KPG)。方法:采用 ODS 柱(5μm,4.6 mm×250 mm);流动相为乙腈-水(35:65),内含0.05 mol·L-1磷酸二氢钾和0.005 mol·L-1的四丁基溴化胺,pH5.6;流速为1 mL·min-1;检测波长232 nm;柱温30℃;进样是20μL。内标为10 mg·L-1的萘普生甲醇溶液。结果:在2~1000μmol·L-1浓度范围内,胆汁中 S-KPG、R-KPG 回归方程分别为 Y=0.0039X-0.0256,r=0.9998和 Y=0.0039X-0.0229,r=0.9998;最低检测限分别为0.5 μmol·L-1和1 μmol·L-1。S-KPG 和 R-KPG 在室温和胆汁生理 pH 时不稳定,在 pH4时最稳定。结论:本文应用 RP-HPLC 检测胆汁 S-KPG、R-KPG,方法简便、易行、实用,可以作为肝脏葡萄糖醛酸转移酶活性和胆排泄实验研究的分析手段。
【Abstract】 Objective:To establish an RP-HPLC method to determine ketoprofen glucuronides(S-KPG and R- KPG)in bile liquid.Methods:The chromatographic separation was performed using an ODS analytical column.The mobile phase consisted of acetonitrile and 0.05 mol·L-1phosphate buffer(pH 5.6)including 5 mmol·L-1tetra- butylammonium bromide(35:65).The detector wavelength was 232 nm,the flow rate was 1 mL·min-1,the volume of injection was 20 μL,and the oven temperature was 30℃.The internal standard was naproxen dissolved by meth- anol.Results:For both kinds of KPGs,the linear range was 2~1000 μmol·L-1.The linear equation of S-KPG was Y=0.0039X-0.0256,r=0.9998;the linear equation of R-KPG was Y=0.0039X-0.0229,r=0.9998. KPGs were easy to be hydrolyzed in the condition of room temperature and bile physiological pH.However,KPGs were stable in the condition of pH adjusted to 4.Conclusion:The method is simple and utility.And it can be used for the empirical study of the glucuronyltransferase activity and bile excretion function.
- 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2007年06期
- 【分类号】R96
- 【被引频次】2
- 【下载频次】147