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作 者:马萍[1] 李鹏飞[1] 刘丽宏[1] 王淑民[2] 丁春雷[1]
机构地区:[1]第二炮兵总医院药学部,北京100088 [2]首都医科大学附属北京同仁医院,北京100730
出 处:《质谱学报》2011年第1期43-49,共7页Journal of Chinese Mass Spectrometry Society
摘 要:建立高效液相色谱-串联质谱(HPLC—MS/MS)法同时测定人血浆中替米沙坦和氢氯噻嗪的浓度。选用Zorbax Eclipse XDB-C 18色谱柱,以乙腈-5mmol/L乙酸铵为流动相,采用梯度洗脱进行分离,样品用V(乙醚):V(二氯甲烷)=60:40的溶液,液-液萃取后进样,选用3200Q-Trap型质谱仪的多重反应监测(MRM)扫描方式进行检测。替米沙坦线性范围为1.0~1000.0μg/L,氢氯噻嗪线性范围为0.6~200.0μg/L,定量下限分别为1.0和0.6μg/L。准确度与精密度结果显示,方法日间、日内变异均小于15%,相对偏差分别为替米沙坦-5.6%~4.3%、氢氯噻嗪-6.3%~2.7%。替米沙坦和氢氯噻嗪的低、中、高3个浓度提取回收率均大于50%,稳定性较好。该方法可用于人体替米沙坦和氢氯噻嗪血药浓度的同时监测,以及复方制剂的人体药代动力学研究。Telmisartan and hydrochlorothiazide in human plasma were determined by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Telmisartan, hydrochlorothiazide and the internal standard were extracted from plasma using V (diethyl ether) : V (dichloromethane)=60:40, and separated on a Zorbax Eclipse XDB- C 18 column using acetonitrile-5 mmol/L ammonium acetate as mobile phase by gradient elution. Detection was carried out by multiple reaction monitoring (MRM) on a 3200Q-Trap LC-MS/MS system. The assay is linear over the range 1.0-1 000.0 μg/L with a lower limit of quantitation of 5.0 μg/L for telmisartan, and linear over the range 0. 6-200. 0 μg/L with a lower limit of quantitation of 0. 6 μg/L for hydrochlorothiazide. Intra- and inter-day precision are less than 15%. The relative deviations are in the range of -5.6%-4.3% for telmisartan, and --6. 3%--2. 7% for hydrochlorothiazide. The recoveries of telmisartan and hydrochlorothiazide are more than 50%, and stabilities are good.
关 键 词:高效液相色谱-串联质谱(HPLC—MS/MS) 替米沙坦 氢氯噻嗪 药代动力学
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