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液相色谱-电喷雾电离-质谱法测定人血浆中莫索尼定的含量

Determination of moxonidine in human plasma by liquid chromatography-electrospray ionisation-mass spectrometry.

作者信息

Zhao Luhua, Ding Li, Wei Xin

机构信息

Center for Instrumental Analysis, China Pharmaceutical University, 24th Tongjiaxiang Road, Nanjing 210009, PR China.

出版信息

J Pharm Biomed Anal. 2006 Jan 23;40(1):95-9. doi: 10.1016/j.jpba.2005.06.002. Epub 2005 Jul 11.

Abstract

A sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and quantification of moxonidine in human plasma. After the addition of clonidine-HCl, the internal standard (IS) and sodium hydrogen carbonate, plasma samples were extracted using 5 mL ethyl acetate. The compounds were separated on a Lichrospher ODS (5 microm, 250 mm x 4.6 mm) column using an elution system of 10 mmol/L ammonium acetate buffer-methanol (20:80 v/v) as the mobile phase. Analytes were determined using electrospary ionization in a single quadrupole mass spectrometer. LC-ESI-MS was performed in the selected-ion monitoring (SIM) mode using target ions at m/z: 242.2 for moxonidine and m/z: 230.1 for the IS. The method has shown to be sensitive and specific by testing six different blank plasma batches. Linearity was established for the range of concentrations 0.01976-9.88 ng/mL with a coefficient of correlation (r) of 0.9999. The lower limit of quantification (LOQ) was identifiable and reproducible at 0.01976 ng/mL. The method has been successfully applied to study the pharmacokinetics of moxonidine in healthy male Chinese volunteers.

摘要

已开发并验证了一种灵敏且特异的液相色谱 - 电喷雾电离 - 质谱(LC - ESI - MS)方法,用于鉴定和定量人血浆中的莫索尼定。加入盐酸可乐定、内标(IS)和碳酸氢钠后,用5 mL乙酸乙酯萃取血浆样品。化合物在Lichrospher ODS(5微米,250 mm×4.6 mm)柱上分离,以10 mmol/L乙酸铵缓冲液 - 甲醇(20:80 v/v)作为流动相的洗脱系统。在单四极杆质谱仪中使用电喷雾电离测定分析物。LC - ESI - MS在选择离子监测(SIM)模式下进行,莫索尼定的目标离子为m/z: 242.2,内标的目标离子为m/z: 230.1。通过检测六个不同的空白血浆批次,该方法已显示出灵敏性和特异性。在0.01976 - 9.88 ng/mL的浓度范围内建立了线性关系,相关系数(r)为0.9999。定量下限(LOQ)在0.01976 ng/mL时可识别且可重现。该方法已成功应用于研究健康中国男性志愿者中莫索尼定的药代动力学。

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