四种分光光度法同时测定氯唑恶酮双氯芬酸钾二元混合物的比较研究

Rady F. Abdul-Kareem
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Method A, is a dual wavelength spectrophotometric method in which the wavelengths selected for determination of chlorzoxazone were 259 nm and 294 nm, whereas the wavelengths selected for determination of diclofenac potassium were 294 nm and 242 nm. while method B, is a ratio difference spectrophotometric method in which the wavelengths selected for determination of chlorzoxazone were 280 nm and 230 nm, whereas the wavelengths selected for determination of diclofenac potassium were 246 nm and 284 nm. while method C, is the first derivative of the ratio spectra measured at 290 nm and 301 nm for chlorzoxazone and diclofenac potassium, respectively. While method D, is the constant center spectrophotometric method in which more measured at 280 nm and 277 nm for chlorzoxazone and diclofenac potassium, respectively. 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引用次数: 0

摘要

建立了四种简单、快速、准确、重复性好、简便易行的分光光度法,可同时测定氯唑唑酮和双氯芬酸钾的含量,无需预先分离。方法A采用双波长分光光度法,测定氯唑唑酮的波长分别为259 nm和294 nm,测定双氯芬酸钾的波长分别为294 nm和242 nm。方法B为比值差分光光度法,测定氯唑唑酮的波长分别为280 nm和230 nm,测定双氯芬酸钾的波长分别为246 nm和284 nm。方法C为氯唑唑酮和双氯芬酸钾分别在290 nm和301 nm测得的比值光谱的一阶导数。方法D为恒中心分光光度法,分别在280 nm和277 nm处测定氯唑唑酮和双氯芬酸钾。beerlambert图回归分析表明,两种药物的浓度在2.5 ~ 20 μg/mL范围内相关性良好,方法a中氯唑唑酮和双氯芬酸钾的LOD分别为0.308 μg/mL和0.932 μg/mL, LOQ分别为0.458 μg/mL和1.388 μg/mL, RSD分别为1.325和1.666,回收率分别为98.99和101.23。方法a中氯唑唑酮和双氯芬酸钾的LOD分别为0.307 μg/mL和0.373 μg/mL, LOQ分别为0.929 μg/mL和1.123 μg/mL, RSD分别为1.065和1.371,回收率分别为99.94和101.53;氯唑唑酮和双氯芬酸钾的检出限分别为0.287和0.301 μg/mL,检出限分别为0.871和0.911 μg/mL, RSD分别为1.214和1.596,回收率分别为99.73和100.26。氯唑唑酮和双氯芬酸钾的检出限分别为0.221和0.331 μg/mL,检出限分别为0.521和0.825 μg/mL, RSD分别为0.914和1.412,回收率分别为101.22和98.59;方法d根据ICH指南进行了验证,并成功地应用于氯唑唑酮和双氯芬酸钾在实验室制剂和商业胶囊制剂中的含量测定。
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COMPARATIVE STUDY AMONG FOUR SPECTROPHOTOMETRIC METHODS FOR THE SIMULTANEOUS DETERMINATION OF BINARY MIXTURE OF CHLORZOXAZONE AND DICLOFENAC POTASSIUM
Four simple, fast, accurate, reproducible, and non-sophisticated spectrophotometric methods were developed and validated for the simultaneous determination of chlorzoxazone and diclofenac potassium without preliminary separation in pure powder form and in their capsule formulation. Method A, is a dual wavelength spectrophotometric method in which the wavelengths selected for determination of chlorzoxazone were 259 nm and 294 nm, whereas the wavelengths selected for determination of diclofenac potassium were 294 nm and 242 nm. while method B, is a ratio difference spectrophotometric method in which the wavelengths selected for determination of chlorzoxazone were 280 nm and 230 nm, whereas the wavelengths selected for determination of diclofenac potassium were 246 nm and 284 nm. while method C, is the first derivative of the ratio spectra measured at 290 nm and 301 nm for chlorzoxazone and diclofenac potassium, respectively. While method D, is the constant center spectrophotometric method in which more measured at 280 nm and 277 nm for chlorzoxazone and diclofenac potassium, respectively. Regression analysis of Beer-Lambert’s plots showed good correlation in concentration range of 2.5 – 20 μg/mL for both drugs with LOD 0.308 μg/mL and 0.932 μg/mL, LOQ 0.458 μg/mL and 1.388 μg/mL, RSD 1.325 and 1.666 and % recovery 98.99 and 101.23 for chlorzoxazone and diclofenac potassium, respectively in method A. Furthermore, LOD 0.307 μg/mL and 0.373 μg/mL, LOQ 0.929 μg/mL and 1.123 μg/mL, RSD 1.065 and 1.371 and % recovery 99.94 and 101.53 for chlorzoxazone and diclofenac potassium, respectively in method B. Furthermore, LOD 0.287 μg/mL and 0.301 μg/mL, LOQ 0.871 μg/mL and 0.911 μg/mL, RSD 1.214 and 1.596 and % recovery 99.73 and 100.26 for chlorzoxazone and diclofenac potassium, respectively in method C. Furthermore, LOD 0.221 μg/mL and 0.331 μg/mL, LOQ 0.521 μg/mL and 0.825 μg/mL, RSD 0.914 and 1.412 and % recovery 101.22 and 98.59 for chlorzoxazone and diclofenac potassium, respectively in method D. The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of chlorzoxazone and diclofenac potassium in their laboratory prepared mixtures and commercial capsule formulation.
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