Comparison of UV- and Derivative-Spectrophotometric and HPTLC UVDensitometric Methods for the Determination of Amrinone and Milrinone in Bulk Drugs

2020 ◽  
Vol 16 (3) ◽  
pp. 246-253
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Stefan Kruszewski

Background: Spectrophotometry and thin layer chromatography have been commonly applied in pharmaceutical analysis for many years due to low cost, simplicity and short time of execution. Moreover, the latest modifications including automation of those methods have made them very effective and easy to perform, therefore, the new UV- and derivative spectrophotometry as well as high performance thin layer chromatography UV-densitometric (HPTLC) methods for the routine estimation of amrinone and milrinone in pharmaceutical formulation have been developed and compared in this work since European Pharmacopoeia 9.0 has yet incorporated in an analytical monograph a method for quantification of those compounds. Methods: For the first method the best conditions for quantification were achieved by measuring the lengths between two extrema (peak-to-peak amplitudes) 252 and 277 nm in UV spectra of standard solutions of amrinone and a signal at 288 nm of the first derivative spectra of standard solutions of milrinone. The linearity between D252-277 signal and concentration of amironone and 1D288 signal of milrinone in the same range of 5.0-25.0 μg ml/ml in DMSO:methanol (1:3 v/v) solutions presents the square correlation coefficient (r2) of 0,9997 and 0.9991, respectively. The second method was founded on HPTLC on silica plates, 1,4-dioxane:hexane (100:1.5) as a mobile phase and densitometric scanning at 252 nm for amrinone and at 271 nm for milrinone. Results: The assays were linear over the concentration range of 0,25-5.0 μg per spot (r2=0,9959) and 0,25-10.0 μg per spot (r2=0,9970) for amrinone and milrinone, respectively. The mean recoveries percentage were 99.81 and 100,34 for amrinone as well as 99,58 and 99.46 for milrinone, obtained with spectrophotometry and HPTLC, respectively. Conclusion: The comparison between two elaborated methods leads to the conclusion that UV and derivative spectrophotometry is more precise and gives better recovery, and that is why it should be applied for routine estimation of amrinone and milrinone in bulk drug, pharmaceutical forms and for therapeutic monitoring of the drug.

2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.


2010 ◽  
Vol 93 (5) ◽  
pp. 1349-1354 ◽  
Author(s):  
Roy T Upton

Abstract TLC characterizations are among the key identity tests in most pharmacopoeial monographs. Pharmacopoeial standards are typically used by industry as a basis for meeting QC requirements and current good manufacturing practices (cGMPs). TLC is a relatively low-cost, highly versatile tool for developing specifications for raw materials, as well as for the various preparations for which pharmacopoeial standards are created. In addition to its use in the development of identity tests, TLC is a valuable tool for screening plant samples that pharmacopoeias must review in the development of monographs and botanical reference materials (BRMs). Specifically, HPTLC is the ideal TLC technique for these purposes because of its increased accuracy, reproducibility, and ability to document the results, compared with standard TLC. Because of this, HPTLC technologies are also the most appropriate TLC technique for conformity with GMPs. This article highlights the manner in which HPTLC is used by the American Herbal Pharmacopoeia (AHP) in the development of AHP monograph identity standards, the identification of adulterating species, and the development of AHP-verified BRMs.


2006 ◽  
Vol 89 (4) ◽  
pp. 995-998 ◽  
Author(s):  
Magdalena Wójciak-Kosior ◽  
Agnieszka Skalska ◽  
Grażyna Matysik ◽  
Magdalena Kryska

Abstract In this paper, a high-performance thin-layer chromatography (HPTLC) method combined with densitometry has been described. Chromatography was performed on silica gel Si 60F254 plates using dichloromethaneethyl acetateformic acid (9.5 + 0.5 + 0.1, v/v) mobile phase. This method has been successfully applied for the determination of phenobarbital in pharmaceuticals. Obtained results were comparable with traditionally used column high-performance liquid chromatography (HPLC) methods. For the proposed procedure, linearity (r > 0.999), sensitivity (limit of detection 0.4 g/spot), recovery (97.8102.1%), and repeatability were found to be satisfactory. The HPTLC-densitometry method has many advantages, such as simplicity, reasonable sensitivity, rapidity, and low cost, and it can be successfully used in routine quality control of multidrug preparations containing barbiturates.


Author(s):  
Adham Raeisi ◽  
Mostafa Ramezani ◽  
Hossein Ravazadeh ◽  
Mahdi A. Taher

Introduction: Antibiotics analysis is performed by many methods such as spectrophotometry, fluorimetry, polarography, and high-performance liquid chromatography. This analysis doesn't require derivatization but requires expensive equipment and extensive preparation. When more than one antibiotic is present in a formulation, interactions may occur between the drugs that must be separated before measurement. Thin-layer chromatography is a useful technique for identifying antibiotics because of the low cost, high speed, and low servicing. Silica gel adsorbents have often been used as adsorbents in all thin-layer chromatography studies. In this study, zeolite was used as an adsorbent in thin- layer chromatography with high selectivity. Materials and Methods: The chromatographic behaviour of amoxicillin, ampicillin, cefazolin, cefixime, ceftriaxone, cefalexin, and penicillin was studied for the first time on a thin layer of zeolite with mobile, organic, and organic- organic phases. Discussion: The best separation of ceftriaxone from amoxicillin, ampicillin, cefazolin, cefixolin, cefalexin, and penicillin on a thin layer of zeolite using methanol as the mobile phase. The distance and rise time are 12 cm and 110 minutes, respectively. Conclusion: The results of the present study showed that using the current method, the selectivity of one antibiotic from other components as well as two-component andthree-component adsorption was obtained. Quantitative identification of antibiotics was also performed in multicomponent mixtures after selection of appropriate isolates.


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