HPLC法同时测定人尿液中三苯双脒代谢物氨脒和乙酰氨脒的浓度

发布时间：2018-04-27 10:21

本文选题：三苯双脒 + 代谢物　；参考：《中国药房》2015年02期

【摘要】：目的:建立同时测定人尿液中三苯双脒代谢物氨脒和乙酰氨脒浓度的方法,并进行其排泄动力学研究。方法:8名健康男性受试者空腹口服三苯双脒肠溶片400 mg,收集服药前及服药后0~2、2~4、4~6、6~8、8~12、12~24、24~36、36~48 h的尿液。尿样经沉淀蛋白并稀释后,以比卡鲁胺为内标,采用高效液相色谱法进样测定,色谱柱为Agilent Zorbax Extend C18(250 mm×4.6 mm,5μm)流动相为乙腈-水-三乙胺(60∶40∶0.2,V/V/V),紫外检测波长为265 nm,流速为0.7 ml/min,进样量为10μl。结果:氨脒和乙酰氨脒尿药浓度分别在0.5~500μg/ml(r=0.996 2)和0.1~200μg/ml(r=0.995 8)范围内线性关系良好,最低定量限分别为0.5、0.1μg/ml,绝对回收率分别为94.78%~95.23%和91.26%~96.99%,相对回收率为98.37%~101.44%和99.26%~102.06%,日内、日间RSD7%;-20℃冷冻24 h及7 d和反复冻融均稳定,RSD7%。受试者口服400 mg三苯双脒肠溶片后,氨脒和乙酰氨脒48 h尿累积排泄率分别为(55.84±13.60)%和(14.98±7.65)%,采用DAS 2.0程序计算氨脒和乙酰氨脒半衰期分别为(3.46±0.73)h和(4.21±0.43)h,尿药排泄速率常数分别为(0.21±0.07)h-1和(0.17±0.02)h-1。结论:该方法简单、快速、灵敏、重复性好,可用于健康受试者口服三苯双脒肠溶片后氨脒和乙酰氨脒尿药浓度的测定。
[Abstract]:Objective: to establish a method for simultaneous determination of three benzamid metabolites of amamamid and Acetamiprid in human urine and to study its excretory kinetics. Methods: 8 healthy male subjects were taken orally Tribendimidine Enteric-coated Tablets 400 mg orally, and the urine of 0~2,2~4,4~6,6~8,8~ 12,12~24,24~36,36~48 h before and after taking the medicine was collected. The urine sample was precipitated protein. After dilution, using high performance liquid chromatography with biacaramine as internal standard, the chromatographic column was Agilent Zorbax Extend C18 (250 mm * 4.6 mm, 5 u m) with acetonitrile water three ethylamine (60: 40: 0.2, V/V/V), UV detection wavelength 265 nm, velocity of 0.7 mL /min, and 10 mu L. results: amamamid and acetamiprid urine concentration. The linear relationship between 0.5~500 mu g/ml (r=0.996 2) and 0.1~200 mu g/ml (r=0.995 8) is good, the minimum quantitative limit is 0.5,0.1 u g/ml, and the absolute recovery is 94.78%~95.23% and 91.26%~96.99% respectively. The relative recovery rate is 98.37%~101.44% and 99.26%~102.06%, day, day, 24, 7 and repeated freezing and thawing. After oral administration of 400 mg Tribendimidine Enteric-coated Tablets, the cumulative excretion rate of amamamid and acetamiprid 48 h urine was (55.84 + 13.60)% and (14.98 + 7.65)% respectively. The half-life of amamamid and acetamiprid was (3.46 + 0.73) H and (4.21 + 0.43) h respectively by DAS 2 program. The urinary excretion rate constant was (0.21 + 0.07) H-1 and (0.17 + 7.65) h-1. conclusion, respectively. The method is simple, rapid, sensitive and reproducible, and can be used for the determination of amamiprid and Acetamiprid in healthy volunteers after oral administration of Tribendimidine Enteric-coated Tablets.

【作者单位】：山东医学高等专科学校;山东大学齐鲁医院临床药理研究所;德州市食品药品监督管理局德城区分局;
【分类号】：R927;O657.72

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