Singh Sonu Sundd, Shah Hiten, Gupta Sapna, Jain Manish, Sharma Kuldeep, Thakkar Purav, Shah Ruchy
Biomedical and DMPK Department, Zydus Research Centre, Sarkhej-Bavla N.H. No. 8A, Moraiya, Ahmedabad 382213, India.
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Nov 25;811(2):209-15. doi: 10.1016/j.jchromb.2004.09.001.
A novel liquid chromatographic--electrospray ionisation mass spectrometric (LC--ESI-MS) method has been developed for the determination of escitalopram, an antidepressant in human plasma using paroxetine as internal standard. The method involved liquid--liquid extraction of the analyte from human plasma with a mixture of diethyl ether and dichloromethane (70:30, v/v). The chromatographic separation was achieved within 7.0 min by using 2.0 mM ammonium acetate (pH 5.0)--acetonitrile (54:46, v/v) as mobile phase and a ODS YMCAQ 150 mm x 4.6 mm analytical column; the flow-rate was 1.0 ml/min. Ion signals m/z 325.0 and 330.0 for escitalopram and internal standard, were measured in the positive mode. A detailed validation of the method was performed as per USFDA guidelines and the standard curves were found to be linear in the range of 1.0-200 ng/ml with a mean correlation coefficient more than 0.99. The absolute recovery was more than 75% for both escitalopram and internal standard. The method was simple, sensitive, precise, accurate and was successfully applied to the bioequivalence study of escitalopram in healthy, male, human subjects.
已开发出一种新型液相色谱 - 电喷雾电离质谱（LC - ESI - MS）方法，以帕罗西汀为内标物测定人血浆中的抗抑郁药艾司西酞普兰。该方法包括用乙醚和二氯甲烷的混合物（70:30，v/v）从人血浆中液 - 液萃取分析物。使用2.0 mM醋酸铵（pH 5.0） - 乙腈（54:46，v/v）作为流动相和ODS YMCAQ 150 mm×4.6 mm分析柱，在7.0分钟内实现色谱分离；流速为1.0 ml/min。在正模式下测量艾司西酞普兰和内标物的离子信号m/z 325.0和330.0。按照美国食品药品监督管理局（USFDA）指南对该方法进行了详细验证，发现标准曲线在1.0 - 200 ng/ml范围内呈线性，平均相关系数大于0.99。艾司西酞普兰和内标物的绝对回收率均超过75%。该方法简单、灵敏、精确、准确，并成功应用于健康男性受试者中艾司西酞普兰的生物等效性研究。
