經確效之高效液相層析法同時測定長春胺及其潛在降解（代謝）物 Vincaminic Acid   全文下載

A Validated HPLC Method for the Simultaneous Determination of Vincamine and its Potential Degradant (Metabolite), Vincaminic Acid: Applications to Pharmaceutical Formulations and Pharmacokinetic Studies

開發並確效可同時測定長春胺及其潛在降解（代謝）物vincaminic acid之高效液相層析法。層析使用Spheri-5 RP-C8管柱（5 μm, 內徑220 × 4.6 mm），乙?及0.05 M醋酸鈉30：70（v / v）為移動相，pH值4.0，流速1 mL/min，檢測波長270 nm，依據波峰面積定量分析物。長春胺和vincamin-ic acid濃度範圍分別為0.1-50和0.4-50 μg/mL時，呈線性關係。長春胺和vincaminic acid之偵測極限分別為0.03和0.08 μg/mL。本研究目標有二，首先是長春胺於製劑中之穩定性試驗，此外，vincaminic acid的測定可低至同時存在的長春胺之0.07%。其次是研究口服60 mg長春胺之健康志願者血漿及尿液樣本，長春胺及其主要代謝物vincaminic acid之監測。本方法具令人滿意之準確性（回收率 > 97%），總體標準差介於1.4至2.3%。"

A sensitive and specific HPLC method was developed and validated for the simultaneous determination of vincamine and its potential degradant (metabolite), vincaminic acid. Chromatographic separation was achieved on a Spheri-5 RP-C8 (5 μm) (220 × 4.6 mm i.d.) column using a mobile phase composed of acetonitrile and 0.05 M sodium acetate, pH 4.0 (30 : 70, v/v) at a flow rate of 1 mL/min. The UV detector was set at 270 nm and the quantitation of the analytes was based on the peak areas. The method was proven to be accurate and precise with linearity ranges of 0.1 - 50 and 0.4 - 50 µg/mL for vincamine and vincaminic acid, respec-tively. The limits of detection were 0.03 and 0.08 µg/mL for vincamine and vincaminic acid, respectively. The method was applied to serve two goals. First; stability-indicating assay of vincamine in its pharmaceutical formulations, in addition, the determination of vincaminic acid down to a level of 0.07% in presence of excess of the parent drug. Second; drug monitoring of vincamine and its main metabolite, vincaminic acid in human plasma/urine samples taken from a healthy volunteer treated with 60 mg oral dose of vincamine. The accuracy of the method was satisfactory (recovery > 97%). The overall standard deviation ranged from 1.4 to 2.3%.