Oliveira Celso H, Barrientos-Astigarraga Rafael E, Abib Eduardo, Mendes Gustavo D, da Silva Débora R, de Nucci Gilberto
Department of Pharmacology, State University of Campinas, SP, Campinas, Brazil.
J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Jan 15;783(2):453-9. doi: 10.1016/s1570-0232(02)00711-0.
An analytical method based on liquid chromatography with positive ion electrospray ionization (ESI) coupled to tandem mass spectrometry detection was developed for the determination of lansoprazole in human plasma using omeprazole as the internal standard. The analyte and internal standard were extracted from the plasma samples by liquid-liquid extraction using diethyl-ether-dichloromethane (70:30; v/v) and chromatographed on a C(18) analytical column. The mobile phase consisted of acetonitrile-water (90:10; v/v)+10 mM formic acid. The method has a chromatographic total run time of 5 min and was linear within the range 2.5-2000 ng/ml. Detection was carried out on a Micromass triple quadrupole tandem mass spectrometer by Multiple Reaction Monitoring (MRM). The intra- and inter-run precision, calculated from quality control (QC) samples, was less than 3.4%. The accuracy as determined from QC samples was less than 9%. The method herein described was employed in a bioequivalence study of two capsule formulations of lansoprazole.
建立了一种基于液相色谱-正离子电喷雾电离(ESI)串联质谱检测的分析方法,以奥美拉唑为内标物测定人血浆中的兰索拉唑。采用乙醚-二氯甲烷(70:30;v/v)液-液萃取法从血浆样品中提取分析物和内标物,并在C(18)分析柱上进行色谱分离。流动相由乙腈-水(90:10;v/v)+10 mM甲酸组成。该方法的色谱总运行时间为5分钟,在2.5-2000 ng/ml范围内呈线性。通过多反应监测(MRM)在Micromass三重四极杆串联质谱仪上进行检测。根据质量控制(QC)样品计算的批内和批间精密度小于3.4%。由QC样品测定的准确度小于9%。本文所述方法用于兰索拉唑两种胶囊制剂的生物等效性研究。