scholarly journals Quantitative Analysis of Sulpiride and Impurities of 2-Aminomethyl-1-Ethylpyrrolidine and Methyl-5-Sulphamoyl-2-Methoxybenzoate in Pharmaceuticals by High-Performance Thin-Layer Chromatography and Scanning Densitometry

1999 ◽  
Vol 82 (4) ◽  
pp. 825-829 ◽  
Author(s):  
Danica Agbaba ◽  
Tatjana Miljkovic ◽  
Valentina Marinkovic ◽  
Dobrila Zivanov-Stakic ◽  
Sote Vladimirov

Abstract A simple and reliable thin-layer chromatographic method for determining sulpiride and impurities of 2-aminomethyl-1-ethylpyrrolidine and methyl-5-sulphamoyl-2-methoxybenzoate was developed and validated. A methylene chloride–methanol–ammonia solution (25%; 18 + 2.8 + 0.4, v/v) solvent system is used for separation and quantitative evaluation of chromatograms. The chromatographic plate is first scanned at 240 nm to locate chromatographic zones corresponding to sulpiride and methyl-5-sulphamoyl-2-methoxybenzoate. Then 2-aminomethyl-1-ethylpyrrolidine is derivatized in situ with ninhydrin, and resulting colored spots are measured at 500 nm. The method is reproducible and convenient for quantitative analysis and purity control of sulpiride in its raw material and in its dosage forms.

2014 ◽  
Vol 21 (1) ◽  
pp. 11-15
Author(s):  
Daiva Kazlauskienė ◽  
Guoda Kiliuvienė ◽  
Palma Nenortienė ◽  
Giedrė Kasparavičienė ◽  
Ieva Matukaitytė

By conducting the toxicological analysis it is meaningful to determine the analytical system that could identify simultaneously several medicinal preparations quickly and precisely. The purpose of this work was to create and validate the method of thin-layer chromatography that would be suitable to separate the components of antidepressant mixture (amitriptyline hydrochloride, paroxetine hydrochloride, sertraline hydrochloride, fluvoxamine maleate and buspirone hydrochloride) and to identify them. The system was validated with regard to the sensitivity, repetition of data, resistance and particularity. The solvent systems with potential of high separation of components in their mixture were created: acetonitrile, methanol, ammonia solution 25 percent (85:10:5); acetonitrile, methanol, ammonia solution 25 percent (75:20:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (50:45:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (42:55:3); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (25:70:5); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (60:36:4). One of the most suitable solvent systems for separation of the analyzed mixture (sertraline, amitriptyline, paroxetine, buspirone, fluvoxamine) was determined – acetonitrile, methanol, ammonia solution 25 percent (85:10:5). When this solvent system was used, the average Rf values of the analyzed compounds differed the most. Validation was conducted – the relative standard deviation (RSD, percent) of the average Rf value of the analyzed compounds varied from 0,6 to 1,8 percent and did not exceed the permissible error of 5 percent. The sensitivity of methodology was determined by assessing the intensity of the mixture’s spots on the chromatographic plate. The detection limit of buspirone was 0,0012 µg; sertraline – 0,0008 µg; amitriptyline – 0,0004 µg; fluvoxamine – 0,0004 µg; paroxetine – 0,0008 µg. The resistance of results to the changed conditions – it was determined that when the amounts of the solvents acetonitrile and methanol were increased or decreased to two milliliters, the average Rf values of the analyzed compounds did not change statistically significantly


INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 42-48
Author(s):  
P. J. Patel ◽  
◽  
D. A Shah ◽  
F. A. Mehta ◽  
U. K. Chhalotiya

A simple, sensitive and precise high performance thin layer chromatographic (HPTLC)method has been developed for the estimation of ondansetron (OND) and ranitidine (RAN) in combination. The method was employed on thin layer chromatography (TLC) and aluminium plates were precoated with silica gel 60 F254 as the stationary phase, while the solvent system was methanol. The Rf values were observed to be 0.5 ± 0.02, and 0.3 ± 0.02 for OND and RAN, respectively. The separated spots were densitometrically analyzed in absorbance mode at 299 nm. This method was linear in the range of 25-300 ng/band for OND and 50-600 ng/band for RAN. The limits of detection for OND and RAN were found to be 3.47 and 1.83 ng/band, respectively. The limits of quantification for OND and RAN were found to be 10.53 and 5.55 ng/band, respectively. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of OND and RAN in combined dosage form.


2006 ◽  
Vol 89 (3) ◽  
pp. 619-623 ◽  
Author(s):  
Kamlesh Dhalwal ◽  
Yogesh S Biradar ◽  
Mandapati Rajani

Abstract Whole plant of Phyllanthus amarus Linn. is a reputed drug of the Indian systems of medicine that is used as hepatoprotective agent. A simple high-performance thin-layer chromatography (HPTLC) densitometric method has been developed for the simultaneous quantitation of phyllanthin, hypophyllanthin, gallic acid, and ellagic acid in the whole plant of P. amarus. They were found at levels of 0.37, 1.16, 0.36, and 0.17% (w/w), respectively. The method was validated for precision, repeatability, and accuracy. Instrumental precision was found to be 0.54, 0.93, 0.08, and 0.78% (coefficient of variation, CV); repeatability of the method was 1.01, 0.79, 0.98, and 1.06% (CV) for phyllanthin, hypophyllanthin, gallic acid, and ellagic acid, respectively. Accuracy of the method was determined by a recovery study conducted at 3 different levels, and the average recovery was found to be 99.09% for phyllanthin, 99.27% for hypophyllanthin, 98.69% for gallic acid, and 100.49% for ellagic acid. The proposed HPTLC method was found to be simple, precise, specific, sensitive, and accurate and can be used for routine quality control of raw material of P. amarus and formulations containing P. amarus. It also has the applicability in quantitating any of these marker compounds in other drugs.


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