Monser Lotfi, Darghouth Frida
Chemistry Department, Institut National des Sciences Appliquées et de Technologie, Centre Urbain Nord, B.P.No. 676, 1080 Tunis Cedex, Tunis, Tunisia.
J Pharm Biomed Anal. 2003 Aug 8;32(4-5):1087-92. doi: 10.1016/s0731-7085(03)00213-9.
A simple, selective and sensitive high performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination of naproxen and its main degradation products such as 1-(6-methoxy-2-naphthyl) ethanol (MNE), 2-methoxy-6-ethyl naphthalene (MEN) and 2-acetyl-6-methoxy naphthalene (AMN). The separation of these compounds was achieved on porous graphitic carbon (PGC) column using tetrahydrofuran-methanol as the mobile phase, and the effluent from the column was monitored at 272 nm. At a flow rate of 1 ml min(-1), the retention time of the last eluting compound was less than 10 min. Correlation coefficient for calibration curves in the ranges 2-25 microg ml(-1) for all compounds studied were greater than 0.999. The sensitivity of detection is 0.05 microg l(-1) for naproxen, MNE and MEN and 0.20 microg ml(-1) for AMN. The reproducibility of the peak area of these compounds using isocratic elution were quite high, and the standard deviations (S.D.) were below 2% (n=5). The reproducibility of retention times of these compounds was within 1% (n=5). The proposed liquid chromatographic method was successfully applied to the analysis of commercially available naproxen sodium (NS) dosage forms with recoveries of 98.8-102%. A comparative study shows that the selectivity of these compounds on PGC column was different to that obtained with octadecyl silica (ODS) columns.
已开发出一种简单、选择性好且灵敏的高效液相色谱(HPLC)方法,用于同时测定萘普生及其主要降解产物,如1-(6-甲氧基-2-萘基)乙醇(MNE)、2-甲氧基-6-乙基萘(MEN)和2-乙酰基-6-甲氧基萘(AMN)。这些化合物在多孔石墨化碳(PGC)柱上以四氢呋喃-甲醇为流动相实现分离,柱流出物在272 nm处进行监测。在流速为1 ml min⁻¹时,最后洗脱化合物的保留时间小于10分钟。所研究的所有化合物在2 - 25 μg ml⁻¹范围内校准曲线的相关系数均大于0.999。萘普生、MNE和MEN的检测限为0.05 μg l⁻¹,AMN的检测限为0.20 μg ml⁻¹。这些化合物采用等度洗脱时峰面积的重现性相当高,标准偏差(S.D.)低于2%(n = 5)。这些化合物保留时间的重现性在1%以内(n = 5)。所提出的液相色谱方法成功应用于市售萘普生钠(NS)剂型的分析,回收率为98.8 - 102%。一项对比研究表明,这些化合物在PGC柱上的选择性与在十八烷基硅胶(ODS)柱上获得的选择性不同。