高效液相色谱法测定吡罗西康含量的改进与验证

M. Abdulkarim, G. Z. Abdullah, M. Sakeena, Mallikarjun Chitneni, M. Yam, E. S. Mahdi, I. M. Salman, O. Ameer, M. Sattar, M. Basri, A. M. Noor
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引用次数: 3

摘要

吡罗昔康是一种非甾体抗炎药,广泛用于治疗关节疼痛和骨关节炎。本研究的目的是对HPLC法进行改进和验证,以便在不受制剂中其他成分干扰的情况下,获得一种准确、灵敏、精确的定量吡罗昔康浓度的方法。对Owen等人发表的方法进行了改编和修改,以适应上述要求。由于所使用的流动相不能从制剂辅料的干扰中分离出药物峰,因此对流动相进行了修饰。改性流动相为5 mM调至pH 3的磷酸氢二钠与浓邻磷酸、甲醇、乙腈和冰醋酸的比例分别为27:20:52:1。结果表明,即使在同一天的不同时间或不同天的不同时间运行,该方法也具有特异性、精密度、准确性和可重复性。检测限为0.035 μg/ml,定量限为0.0625 μg/ml。由此可见,该方法可用于体外研究大鼠皮肤和合成膜的渗透性样品中吡罗西康的浓度测定。关键词:吡罗昔康;高效液相色谱法;定量分析;
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Modification and Validation of an HPLC Method for Quantification of Piroxicam
Piroxicam is a NSAID that is widely used in the treatment of joint pain and osteoarthritis. The objectives of the study were to modify and validate HPLC method so as to obtain an accurate, sensitive and precise method to quantify piroxicam concentrations without interference from the other ingredients presence in the formulation. The method published by Owen et al. was adapted and modified to suit the above requirements. The modification was carried out on the mobile phase as the mobile phase used by the authors was not able to separate the drug peak from the interference of the formulation excipients. The modified mobile phase consisted of 5 mM of disodium hydrogen phosphate adjusted to pH 3 with concentrated ortho phosphoric acid, methanol, acetonitrile and glacial acetic acid at ratios of 27:20:52:1 respectively. The method was validated and found to be specific, precise, accurate and reproducible even when run at different times of the same day or on different times on different days. The limit of detection and quantification were determined to be 0.035 μg/ml and 0.0625 μg/ml respectively. It could be concluded that this method could be used to determine piroxicam concentration in the samples collected from in vitro study of permeability through the synthetic membrane and excised rat skin. Keywords: Piroxicam, HPLC, Quantification analysis, Modification.
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