Lee Heon-Woo, Seo Ji-Hyung, Lee Hyun-Su, Jeong Seo-Young, Cho Young-Wuk, Lee Kyung-Tae
Department of Pharmacological Biochemistry, College of Pharmacy, Kyung Hee University, Hoegi-Dong, Dongdaemun-Ku, Seoul 130-701, Republic of Korea.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Feb 1;862(1-2):246-51. doi: 10.1016/j.jchromb.2007.11.016. Epub 2007 Nov 23.
A simple method using a one-step liquid-liquid extraction (LLE) with methyl-t-butyl ether (MTBE) followed by high-performance liquid chromatography (HPLC) with negative-ion electrospray ionization tandem mass spectrometric (ESI-MS/MS) detection was developed for the determination of cilnidipine in human plasma using benidipine as an internal standard (IS). Acquisition was performed in multiple reaction monitoring (MRM) mode, by monitoring the transitions: m/z 491.1>121.8 for cilnidipine and m/z 504.2>122.1 for IS, respectively. Analytes were chromatographed on a CN column by isocratic elution using 10mM ammonium acetate buffer-methanol (30:70, v/v; adjusted with acetic acid to pH 5.0). Results were linear (r2=0.99998) over the studied range (0.1-20ng/ml) with a total LC-MS/MS analysis time per run of 3min. The developed method was validated and successfully applied to a cilnidipine bioequivalence study in 24 healthy male volunteers.
建立了一种简单的方法，采用甲基叔丁基醚（MTBE）一步液液萃取（LLE），然后以贝尼地平作为内标（IS），通过负离子电喷雾电离串联质谱（ESI-MS/MS）检测的高效液相色谱（HPLC）法测定人血浆中的西尼地平。采用多反应监测（MRM）模式进行采集，分别监测西尼地平的m/z 491.1>121.8和内标的m/z 504.2>122.1的跃迁。分析物在CN柱上通过等度洗脱进行色谱分离，使用10mM醋酸铵缓冲液-甲醇（30:70，v/v；用醋酸调节至pH 5.0）。在所研究的范围（0.1 - 20ng/ml）内结果呈线性（r2 = 0.99998），每次运行的总LC-MS/MS分析时间为3分钟。所建立的方法经过验证，并成功应用于24名健康男性志愿者的西尼地平生物等效性研究。
