高效液相色谱法测定尿液中阿仑膦酸钠的浓度  

Determination of Alendronate Sodium in Human Urine by HPLC with Fluorescence Detector

作　　者：门磊[1] 赵云丽[1] 郝杰[1] 潘雪妍[1] 于治国[1] 

机构地区：[1]沈阳药科大学药学院,沈阳110016

出　　处：《中国药学杂志》2010年第19期1492-1495,共4页Chinese Pharmaceutical Journal

摘　　要：目的建立阿仑膦酸钠在人体内尿药浓度的高效液相色谱-荧光检测法,并应用于药动学研究。方法采用Shisheido Capcell Pak C18(4.6mm×150mm,5μm)色谱柱,洗脱方式:梯度洗脱,流动相A:25mmol·L-1柠檬酸-25mmol.L-1焦磷酸钠;流动相B:水;流动相C:乙腈-甲醇(1∶1),流速为1.0mL.min-1,柱温40℃;内标物:帕米膦酸钠;荧光检测:激发波长为260nm;发射波长为310nm。28名健康受试者服用阿仑膦酸钠片70mg后,测定阿仑膦酸钠的尿药浓度,并计算药动学参数。结果在25～5000μg·L-1内,阿仑膦酸钠与内标峰面积的比值与浓度呈良好的线性关系(r=0.9987)。日内及日间精密度(RSD)和准确度(RE)均符合要求。阿仑膦酸钠片在体内的累积排泄量Aet为(253830±267241)ng,最大排泄速率Umax为(58508±55394)ng.h-1。结论本试验提供了阿仑膦酸钠体内尿药浓度的HPLC测定方法及药动学参数,为临床应用提供了依据。OBJECTIVE To develop and validate a reliable analytical method for the pharmacokinetic study of alendronate sodium in human urine by a high performance liquid chromatography （HPLC） system with fluorescence detector.METHODS Liquid chromatography was performed on a Capcell Pak C18 column （4.6 mm×150 mm,5 μm particles）,using a gradient method starting with mobile phase acetonitrile/methanol-citrate/pyrophosphate buffer （35：65） at 1.0 mL· min^-1 and 40 ℃.The total run time was 25 min. The fluorometric detector was operated at 260 nm （excitation） and 310 nm （emission）. Pamidronate sodium was used as the internal standard. RESULTS The linearity of calibrated curves of urine samples was in the range of 25-5 000 μg·L^-1 （r=0.998 7）. The intra-and inter-day precision expressed as the relative standard deviation（RSD） was less than 15%. The limit of quantitation was 25 μg·L^-1of alendronate sodium in 5 mL urine. Following the oral administration of 70 mg alendronate sodium tablet to volunteers,the cumulative amount of alendronate sodium was excreted （Aet） and peak excretion rate （Umax） were （253 830±267 241 ）ng and （58 508± 55 394.5） ng·h-1 respectively. CONCLUSION The method was demonstrated to be highly feasible and reproducible and offered a satisfactory tool for the pharmacokinetics and relative bioavailability of alendronate sodium in urine samples.

关 键 词：阿仑膦酸钠 高效液相色谱法 尿样 药动学 

分 类 号：R969.11[医药卫生—药理学]