Elkady Ehab F, Fouad Marwa A, Jaadan Bushra M
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini Street, Cairo 11562, Egypt.
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini Street, Cairo 11562, Egypt.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Feb 15;1076:61-69. doi: 10.1016/j.jchromb.2018.01.022. Epub 2018 Feb 2.
A new validated bio-analytical LC-MS/MS method was developed for the simultaneous extraction and determination of four proton pump inhibitors: esomeprazole, lansoprazole, pantoprazole and rabeprazole in human plasma using escitalopram as an internal standard. The proteins in plasma samples were precipitated using acetonitrile for the extraction of analytes which is a simple economic method. The separation was accomplished using a mobile phase composed of 10 mM ammonium formate: acetonitrile: methanol (20:40:40% v/v) at a flow rate of 0.8 mL/min in isocratic mode on a reversed phase C18 INERTSIL ODS-3 (5 μm, 150 × 4.6 mm) and column temperature of 40 °C. Positive mode electrospray ionization source was used prior to multiple reaction monitoring (MRM) detection using parent and daughter ions: m/z 346.2 → 198.1 for esomeprazole, m/z 370.1 → 252 for lansoprazole, m/z 384.2 → 200.2 for pantoprazole, m/z 360.1 → 242.1 for rabeprazole and m/z 325.2 → 109 for escitalopram. The calibration curves were constructed, and the method was linear in the range of 20-5000 ng/mL applying weighted (1/X) linear regression coefficient for all drugs. The method was fully validated following US-FDA and EMA guidelines.
建立了一种经过验证的新型生物分析液相色谱-串联质谱法，以艾司西酞普兰为内标，同时提取和测定人血浆中的四种质子泵抑制剂：埃索美拉唑、兰索拉唑、泮托拉唑和雷贝拉唑。使用乙腈沉淀血浆样品中的蛋白质以提取分析物，这是一种简单经济的方法。在反相C18 INERTSIL ODS-3（5μm，150×4.6mm）柱上，以等度模式，流动相由10mM甲酸铵：乙腈：甲醇（20:40:40% v/v）组成，流速为0.8mL/min，柱温为40°C，进行分离。在多反应监测（MRM）检测之前，使用正模式电喷雾电离源，监测母离子和子离子：埃索美拉唑为m/z 346.2→198.1，兰索拉唑为m/z 370.1→252，泮托拉唑为m/z 384.2→200.2，雷贝拉唑为m/z 360.1→242.1，艾司西酞普兰为m/z 325.2→109。构建了校准曲线，该方法在20-5000 ng/mL范围内呈线性，对所有药物应用加权（1/X）线性回归系数。该方法按照美国食品药品监督管理局（US-FDA）和欧洲药品管理局（EMA）的指南进行了全面验证。
