HPLC-MS/MS法测定人尿液中西他沙星的浓度

摘要

Objective: To establish a rapid and accurate method for the determination of sitafloxacin in hu-man urine by means of HPLC-MS/MS. Methods: The urine was treated with methanol, and the supernatant was analyzed by an HPLC-MS/MS method. Ten subjects were recruited in a randomized crossover test. Each one had single oral sitafloxacin granule 50 mg when fasting and postprandial, with a cleaning period of 5 days. All urine samples of the subjects were collected on the two periods, before administration (0 h) and after ad-ministration of 0-3, 3-6, 6-12, 12-24, 24-36, 36-48, 48-60 h, sitafloxacin contents were analyzed and the cu-mulative excretion and cumulative excretion rates were calculated. Results: The linear range for the detection of urine sitafloxacin was 0.250-200μg·mL-1, and the limit of quantification was 0.250μg·mL-1. Prototype drug was detected 3 h after oral administration in subjects' urine, the urine excretion was almost complete in 36 h, the cumulative excretion was about 35 mg and the cumulative excretion rate was about 70%. Conclusion: The established method is simple, reliable. It can be used for the determination of urine sitafloxacin and its urinary excretion in population.%目的：建立灵敏、快速、准确的人尿液中西他沙星浓度的HPLC-MS/MS检测方法，并将其用于测定健康受试者口服西他沙星颗粒剂后的尿药排泄。方法：尿液经甲醇处理后，取上清液进行HPLC-MS/MS法分析。10例受试者，每例空腹和餐后（随机交叉）单次口服西他沙星颗粒剂50 mg，经5天的清洗期后将两式受试者对调，两周期分别收集给药前（0 h）及给药后0~3、3~6、6~12、12~24、24~36、36~48、48~60 h各时间段的所有尿液并分析，计算西他沙星在尿液中的累计排泄量和累积排泄率。结果：西他沙星尿液的线性范围为0.250~200μg·mL-1，定量限为0.250μg· mL-1。健康受试者口服西他沙星颗粒剂后3 h即能检测到原型药物，36小时内经尿液排泄基本完全，累积排泄量约为35 mg，累积排泄率约为70%。结论：所建立的方法简便、可靠，可用于人口服西他沙星颗粒剂后药物尿液浓度的测定及其尿药排泄研究。