LC-MS/MS法测定人尿液中他唑巴坦钠浓度及其尿药排泄动力学研究 点击下载
论文标题: LC-MS/MS法测定人尿液中他唑巴坦钠浓度及其尿药排泄动力学研究
英文标题:
中文摘要: 目的:建立测定人尿液中他唑巴坦钠浓度的方法,并进行尿药排泄动力学研究。方法:尿液样品经10%高氯酸沉淀后,采用高效液相色谱-串联质谱(LC-MS/MS)法测定尿液中他唑巴坦钠的浓度。色谱柱为Hypersil GOLD C18,流动相为甲醇-水(30 ∶ 70,V/V),流速为0.2 ml/min,柱温为30 ℃,进样量为5 μl;采用电喷雾离子源,以多反应监测方式进行正离子扫描,用于定量分析的离子对为m/z 301→168。入组8名健康受试者,静脉滴注注射用头孢噻肟钠他唑巴坦钠(6 ∶ 1,m/m)2.34 g,收集其给药前和给药后0~2、2~5、5~8、8~12和12~16 h的尿液研究其尿液排泄动力学。结果:他唑巴坦钠尿药浓度在0.25~500 μg/ml范围内线性关系良好(r=0.999 9),定量下限为0.25 μg/ml,批内、批间RSD<10%,方法回收率为93.8%~111.8%,提取回收率为93.9%~99.7%,介质效应为87.6%~107.2%。受试者用药16 h后,他唑巴坦钠的尿累积排泄量为(209.70±39.24)mg,累积排泄率为(61.7±11.5)%。结论:LC-MS/MS法用于人尿液中他唑巴坦钠浓度的测定和排泄动力学的研究简便、快捷、灵敏度高;他唑巴坦钠主要经肾脏排泻。
英文摘要: OBJECTIVE: To establish a method for the concentration determination of tazobactam sodium in human urine, and to study urinary excretion pharmacokinetics. METHODS: The urine samples were extracted by 10% perchloric acid, and then determined by LC-MS/MS. The separation was performed on a Hypersil GOLD C18 column with mobile phase consisted of ethanol-water (30 ∶ 70,V/V) at flow rate of 0.2 ml/min; the column temperature was set at 30 ℃, and sample size was 5 μl. ESI was used, and positive ion scanning was conducted in MRM mode; ion pair for quantitative analysis was m/z 301→168. 8 healthy volunteers were given Cefotaxime sodium and tazobactam sodium for injection (6 ∶ 1,m/m) 2.34 g intravenously, and then urine samples were collected before medication, 0-2, 2-5, 5-8, 8-12 and 12-16 h after medication.  RESULTS: The linear range of tazobactam sodium was 0.25-500 μg/ml (r=0.999 9). The limit of quantitation was 0.25 μg/ml; RSDs of inter-batch and intra-batch were all lower than 10%; method recoveries were 93.8%-111.8%; extraction recoveries were 93.9%-99.7%; medium effect ranged 87.6%-107.2%. 16 h after medication, accumulative excretion amount of tazobactam sodium in urine was (209.70±39.24) mg and accumulative excretion rate was (61.7±11.5)%. CONCLUSIONS: LC-MS/MS method can be used for the concentration determination of tazobactam sodium in human urine and excretion kinetics study. It is simple, rapid and sensitivity; tazobactam sodium mainly excrete viareral tissue.
期刊: 2016年第27卷第32期
作者: 任立玲,王源园,孙鲁宁,张宏文,谢利军,刘云,王永庆
英文作者: REN Liling,WANG Yuanyuan,SUN Luning,ZHANG Hongwen,XIE Lijun,LIU Yun,WANG Yongqing
关键字: 高相液相色谱-串联质谱法;他唑巴坦钠;尿液;尿药浓度;排泄动力学
KEYWORDS: LC-MS/MS; Tazobactam sodium; Urine; Urine concentration; Excretion pharmacokinetics
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