茚三酮试剂凝聚分光光度指纹图谱及硫酸庆大霉素、链霉素、阿米卡星、新霉素和硫酸庆大霉素的测定

Edebi N Vaikosen, Samuel J. Bunu, E. Dode, Ruth B. Efidi
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The final working concentrations ranged between 1600 and 2000 ug/ml.\nResults: The average weight of a neomycin sulphate tablet was 0.747g, with a standard deviation of 0.667%. After complexing with ninhydrin reagent at pH 6.0 for 10 to 15 min, all aminoglycosides developed purple coloration that lasted beyond 24 h, compared to the initial white, pale yellow, and colorless appearance of streptomycin, amikacin, neomycin, and gentamycin, respectively. The scanned spectra of the purple complex of ninhydrin formed after reaction with aminoglycosides in the visible region (350-900 nm) were similar, indicating the presence of a common parent structural moiety. At 550 nm, 650 nm, 750 nm, and 850 nm, distinct absorptions were observed. Amikacin, Streptomycin, and Gentamicin had the highest absorbance between 800 and 900 nm. After the reaction with ninhydrin, three distinct absorbances were observed in the Neomycin spectrum: between 380 and 400 nm, 580 and 600 nm, and around 800 nm. 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引用次数: 1

摘要

目的:建立一种简单、高效、廉价、快速、重现性好的氨基糖苷分光光度分析方法。方法:在pH为8.0的条件下,用茚三酮试剂对阿米卡星、庆大霉素、新霉素、链霉素等氨基糖苷类进行脱胺。将每种成分的工作标准溶液精确地放入一系列10 ml校准的容积瓶中,然后加入1 ml茚三酮试剂,在水浴中加热15分钟。将所得紫色配合物从350 nm扫描到930 nm,记录最大吸收波长(s)。最终工作浓度在1600 ~ 2000 ug/ml之间。结果:硫酸新霉素片平均质量为0.747g,标准偏差为0.667%。与茚三酮试剂在pH 6.0下络合10 ~ 15 min后,所有氨基糖苷均呈现紫色,并持续24 h以上,而链霉素、阿米卡星、新霉素和庆大霉素最初分别呈现白色、淡黄色和无色。与氨基糖苷反应后形成的紫色茚三酮配合物在可见光区(350 ~ 900 nm)扫描光谱相似,表明存在共同的亲本结构片段。在550 nm、650 nm、750 nm和850 nm处观察到不同的吸收。阿米卡星、链霉素和庆大霉素在800 ~ 900 nm吸光度最高。与茚三酮反应后,在新霉素光谱中观察到三个不同的吸光度:380 ~ 400 nm, 580 ~ 600 nm和800 nm左右。四种氨基糖苷类化合物与空白茚三酮试剂的比较光谱显示出其独特的特征。回归系数分别为0.996和0.995。结论:所建立的方法可用于链霉素注射液中链霉素的分析。在650和850 nm处,纯度范围为017 ~ 110%,符合英国药典(BP)对硫酸链霉素片纯度要求97.00 ~ 110%。
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SPECTROPHOTOMETRIC FINGERPRINTING AND CHEMICAL DETERMINATION OF STREPTOMYCIN, AMIKACIN, NEOMYCIN, AND GENTAMYCIN SULPHATE BY CONDENSING WITH NINHYDRIN REAGENT
Objective: The study aimed to develop a simple, efficient, inexpensive, rapid, and reproducible spectrophotometric analytical technique for aminoglycosides analysis by condensing with ninhydrin reagent. Methods: At a pH of 8.0, different aminoglycosides, including amikacin, gentamycin, neomycin, and streptomycin, were deaminated by the ninhydrin reagent. The working standard solution for each component was accurately placed into a series of 10 ml calibrated volumetric flasks, then 1 ml of the ninhydrin reagent was added and heated in a water bath for 15 min. The wavelength(s) of maximum absorption(s) was recorded after scanning the resultant purple complex from 350 nm to 930 nm. The final working concentrations ranged between 1600 and 2000 ug/ml. Results: The average weight of a neomycin sulphate tablet was 0.747g, with a standard deviation of 0.667%. After complexing with ninhydrin reagent at pH 6.0 for 10 to 15 min, all aminoglycosides developed purple coloration that lasted beyond 24 h, compared to the initial white, pale yellow, and colorless appearance of streptomycin, amikacin, neomycin, and gentamycin, respectively. The scanned spectra of the purple complex of ninhydrin formed after reaction with aminoglycosides in the visible region (350-900 nm) were similar, indicating the presence of a common parent structural moiety. At 550 nm, 650 nm, 750 nm, and 850 nm, distinct absorptions were observed. Amikacin, Streptomycin, and Gentamicin had the highest absorbance between 800 and 900 nm. After the reaction with ninhydrin, three distinct absorbances were observed in the Neomycin spectrum: between 380 and 400 nm, 580 and 600 nm, and around 800 nm. The comparative spectra for the four aminoglycosides and ninhydrin reagent with blank show a unique feature for the compounds. The coefficients of regression were 0.996 and 0.995, respectively. Conclusion: The proposed methods for analyzing streptomycin in streptomycin injections were successful. The percentage purity ranged from 017–110 % at 650 and 850 nm, which corresponds to the British Pharmacopoeia (BP) limit that streptomycin sulphate tablets should be between 97.00 and 110%.
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