Iqbal Muzaffar, Ezzeldin Essam, Rezk Naser L, Bajrai Amal A, Al-Rashood Khalid A
Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, PO Box No 2457 Riyadh, Saudi Arabia.
Bioavailability Laboratory, College of Pharmacy, King Saud University, PO Box No 2457 Riyadh, Saudi Arabia.
Bioanalysis. 2018 Jul;10(14):1087-1097. doi: 10.4155/bio-2018-0065. Epub 2018 Apr 25.
The purpose of this study was development, validation and application of ultra-performance liquid chromatography (UPLC)-ESI-MS/MS method for quantitation of flibanserin in plasma samples.
METHOD & RESULTS: After extraction of analyte from plasma by diethyl ether, separation was performed on UPLC C column using mobile phase composition of 10 mM ammonium formate-acetonitrile (30:70, v/v) by isocratic elution of 0.3 ml/min. The multiple reaction monitoring transitions of m/z 391.13 → 161.04 and 384.20 → 253.06 were used for detection of analyte and internal standard (quetiapine), respectively. The calibration curves were linear (r ≥ 0.995) between 0.22 and 555 ng/ml concentration and all validation results were within the acceptable range as per US FDA guidelines.
The assay procedure was fully validated and successfully applied in pharmacokinetic interaction study of flibanserin with bosentan in rats.
本研究旨在开发、验证并应用超高效液相色谱（UPLC）-电喷雾串联质谱（ESI-MS/MS）法对血浆样本中的氟立班丝氨进行定量分析。
通过乙醚从血浆中提取分析物后，采用10 mM甲酸铵-乙腈（30:70，v/v）的流动相组成，以0.3 ml/min的等度洗脱在UPLC C柱上进行分离。分别采用m/z 391.13 → 161.04和384.20 → 253.06的多反应监测转换对分析物和内标（喹硫平）进行检测。校准曲线在0.22至555 ng/ml浓度之间呈线性（r≥0.995），所有验证结果均在美国食品药品监督管理局（US FDA）指南规定的可接受范围内。
该分析方法已得到充分验证，并成功应用于大鼠体内氟立班丝氨与波生坦的药代动力学相互作用研究。
