Department of pharmacology, Institute of Dermatology, Chinese Academy of Medical Sciences & Peking Union Medical College, Nanjing 210042, China.
J Pharm Biomed Anal. 2011 Sep 10;56(2):324-9. doi: 10.1016/j.jpba.2011.05.012. Epub 2011 May 20.
A rapid, sensitive and specific high performance liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method for the quantification of 13-cis-retinoic acid (isotretinoin) in human plasma has been developed. Acitretin was employed as the internal standard (IS). The analytes were chromatographically separated on a Shimadzu Shim-pack VP-ODS C18 column (150 mm × 2.0 mm I.D.) with a mobile phase consisting of acetonitrile and water (90:10, v/v). Detection was performed on a single quadrupole mass spectrometer using an electrospray ionization interface with the selected-ion monitoring (SIM) mode. The method showed excellent linearity (r=0.9989) over the concentration range of 10-1500 ng/mL with good accuracy and precision. The intra- and inter-batch precisions were within 10% relative standard deviation. The recoveries were more than 80%. The validated method was successfully applied to a preliminary bioequivalence study of isotretinoin in 20 Chinese healthy male volunteers.
建立了一种灵敏、特异、快速的高效液相色谱-电喷雾电离质谱（LC-ESI-MS）法，用于人血浆中 13-顺式维甲酸（异维 A 酸）的定量分析。阿维 A 酯作为内标（IS）。分析物在 Shimadzu Shim-pack VP-ODS C18 柱（150mm×2.0mm ID）上进行色谱分离，流动相由乙腈和水（90:10，v/v）组成。采用电喷雾电离接口和选择离子监测（SIM）模式的单四极杆质谱仪进行检测。该方法在 10-1500ng/mL 的浓度范围内表现出良好的线性（r=0.9989），具有良好的准确性和精密度。批内和批间精密度均在 10%相对标准偏差以内。回收率大于 80%。该验证方法成功应用于 20 名中国健康男性志愿者中异维 A 酸的初步生物等效性研究。
