用于测定人血浆中噻托溴铵的灵敏高效液相色谱-电喷雾电离质谱法。
Sensitive HPLC-ESI-MS method for the determination of tiotropium in human plasma.
作者信息
Ding Li, Tan Wenming, Zhang Yindi, Shen Jianping, Zhang Zhengxing
机构信息
Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.
出版信息
J Chromatogr Sci. 2008 May-Jun;46(5):445-9. doi: 10.1093/chromsci/46.5.445.
A sensitive high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) assay is established for the determination of tiotropium in human plasma using benzyltriethylammonium chloride as the internal standard (IS). After being treated with C(18) cartridges, plasma samples are separated by HPLC on a reversed-phase C(18) column with a mobile phase of 40mM ammonium acetate buffer-methanol (56:44, v/v). Tiotropium is determined in a single-quadrupole MS. HPLC-ESI-MS is performed in the selected ion monitoring mode using target ions at m/z 392.0 for tiotropium and m/z 192.3 for the IS. The calibration curve is linear over the range 1.5-30 pg/mL. The intra- and inter-assay variability values are less than 10.1% and 13.6%, respectively. The mean plasma extraction recovery of tiotropium is 92.3 +/- 5.0%. The method has been successfully applied to studying the pharmacokinetics of tiotropium in healthy Chinese volunteers.
建立了一种灵敏的高效液相色谱-电喷雾电离-质谱（HPLC-ESI-MS）分析法，以苄基三乙氯化铵作为内标（IS）来测定人血浆中的噻托溴铵。血浆样品经C(18)柱处理后，在反相C(18)柱上通过HPLC进行分离，流动相为40mM醋酸铵缓冲液-甲醇（56:44，v/v）。噻托溴铵在单四极杆质谱中进行测定。HPLC-ESI-MS在选择离子监测模式下进行，噻托溴铵的目标离子为m/z 392.0，内标的目标离子为m/z 192.3。校准曲线在1.5 - 30 pg/mL范围内呈线性。批内和批间变异值分别小于10.1%和13.6%。噻托溴铵的平均血浆提取回收率为92.3±5.0%。该方法已成功应用于研究健康中国志愿者体内噻托溴铵的药代动力学。
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