Varghese Susheel John, Ravi Thengungal Kochupappy
Sri Ramakrishna Institute of Paramedical Sciences, College of Pharmacy, Department of Pharmaceutical Analysis, Coimbatore, 641 044, Tamil Nadu, India.
J AOAC Int. 2013 Mar-Apr;96(2):307-12. doi: 10.5740/jaoacint.11-117.
A simple, rapid, and sensitive LC/electrospray ionization (ESI)-MS method was developed and validated for the simultaneous determination of rosuvastatin (ROS) and ezetimibe (EZE) in human plasma. Following liquid-liquid extraction, the analytes and an internal standard, atorvastatin (ATO), were separated using an isocratic mobile phase comprising 0.1% (v/v) formic acid-methanol (20 + 80, v/v) on an RP-C18 column. Detection was performed on a mass spectrometer by selected ion monitoring using their respective [M-H]- ions, m/z 480 for ROS, m/z 408 for EZE, and m/z 557 for ATO. For both analytes, the method was linear in the range of 0.1 to 10 nglmL. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 4 min made it possible to determine many plasma samples/day. The validated LC/ESI-MS method can be used to study pharmacokinetics, bioavailability, and bioequivalence of combined dosage forms of ROS and EZE.
建立了一种简单、快速且灵敏的液相色谱/电喷雾电离（ESI）-质谱法，并对其进行了验证，用于同时测定人血浆中的瑞舒伐他汀（ROS）和依折麦布（EZE）。液-液萃取后，在RP-C18柱上使用由0.1%（v/v）甲酸-甲醇（20 + 80，v/v）组成的等度流动相分离分析物和内标阿托伐他汀（ATO）。通过质谱仪，使用各自的[M-H]-离子进行选择离子监测来进行检测，ROS的m/z为480，EZE的m/z为408，ATO的m/z为557。对于两种分析物，该方法在0.1至10 ng/mL范围内呈线性。在标准曲线范围内的浓度下获得了可接受的精密度和准确度。4分钟的运行时间使得每天能够测定许多血浆样品。经验证的液相色谱/电喷雾电离-质谱法可用于研究ROS和EZE联合剂型的药代动力学、生物利用度和生物等效性。
