Emtricitabine and Tenofovir Disoproxil Fumarate and its related impurities obtained from Veeprho laboratories Ltd. Marketed formulation of Emtricitabine and Tenofovir Disoproxil Fumarate purchased from local market manufactured by Emcure pharmaceuticals ltd with brand name Tavin-EM.
This is an open access article distributed under the Creative Commons Attribution Licensewhich permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Abstract In the course of research and development of a new pharmaceutical formulation of azelaic acid in the liposomal form, we developed a rapid and accurate method for the detection of impurities using high-performance liquid chromatography.
Detection of the impurities and the active substance was performed by an evaporative light-scattering detector. The method was validated for selectivity, system precision, method precision, limit of detection, and response rates.
The proposed method can be used to detect impurities in the liposomal formulation of azelaic acid.
The method enables separation of azelaic acid from the identified and unidentified impurities and from the excipients used in the drug form. Introduction Chemically, azelaic acid is a saturated dicarboxylic acid, also known as nonanedioic acid. Under natural conditions, azelaic acid forms on human skin from the interaction of nonanoic acid with Malassezia furfur, a microbe of the Development of validated rp hplc method for bacterial flora.
The azelaic acid structure is shown in Figure 1. Molecule of azelaic acid. Azelaic acid is a relatively new therapeutic substance used in the treatment of acne.
Azelaic acid has several pharmacological effects: The antibacterial activity is based primarily on its biocidal activity against Propionibacterium acnes and Staphylococcus epidermidis.
The inhibitory effect on the 5-alpha-reductase reduces the formation of dihydrotestosterone, normally synthesised in the skin from testosterone: The separation and quantitative determination of the content of carboxylic acids, especially dicarboxylic acids, by chromatography have been relevant issues in analytical chemistry since the s and were initially accomplished using simple systems, such as paper-based chromatography or chromatography with simple silica gel columns [ 45 ].
New methods proposed for the determination of azelaic acid and other dicarboxylic acids include advanced LC, HPLC, and GC with the respective detection systems.
One of the first fast GC qualitative and quantitative analyses of fatty acids was described by Metcalfe and Schmitz—it relies on the derivatisation of fatty acids to methyl esters with a solution of boron trifluoride in methanol [ 6 ].
GC combined with the derivatisation of fatty acids to methyl esters has been used to determine the amount of azelaic acid in the oil paints of old Flemish masters [ 7 ]. A similar method has been applied for evaluating the composition of wall paints [ 8 ]. Modified GC-MS has been used to study the composition of medieval and Renaissance Florentine paintings originally containing proteins and fatty acids, including azelaic acid [ 9 ].
GC-MS has also been used to determine the content of azelaic acid in samples of air from the natural environment [ 1011 ]. An interesting GC method for evaluating the content of azelaic acid in the natural aquatic environment was offered by Pusvaskiene et al. The GC method has been intensively developed due to the difficulties in providing sufficiently precise determinations [ 13 ].
The azelaic acid content in tobacco leaves has been determined by modified GC-MS using methyl derivatives and by means of solid-phase microextraction solid-phase microextraction, SPME [ 14 ].
Attempts to assess azelaic acid in very complex analytical matrices, for example, in biological samples of human or vegetable origin, have been made using both HPLC [ 15 ] and GC-MS methods [ 16 ]. Mansour and Ibrahiem solved the problem of simultaneous quantification of azelaic acid and benzoic acid by using isocratic, reversed-phase HPLC [ 17 ].
In another RP-HPLC method with a fluorescence detector, 2-bromoacetylmethoxynaphthalene was used as a fluorescent marker in an aqueous micellar solution and in acetonitrile.
This method enabled simultaneous determination of the azelaic acid and meglutol, that is, 3-hydroxymethylglutaryl acid, in one sample [ 19 ]. In a complex mixture of carboxylic and dicarboxylic acids and amino acids, azelaic acid was assessed as a derivative of isobutyl chloroformate in GC, coupled with positive chemical ionisation MS GC-MS-PCI [ 20 ].
Preparation of the samples in GC methods is time consuming and requires considerable work. In addition, during the methylation of the sample, aggressive methylating reagents shorten the life of the chromatographic column and the integrity of the autosampler needle in a gas chromatograph.
The mentioned disturbances cause frequent replacement of the column and needle and are associated with additional costs and time. Due to the obstacles encountered when using GC methods for dicarboxylic acid assessments, we decided to develop an alternative method to determine the limit of azelaic acid impurities in the final product—the liposomal form of azelaic acid.
According to the available references, it is possible to use an evaporative light-scattering detector ELSD within an HPLC device to assess the fatty acids [ 2122 ]. In the last decade, the HPLC-ELSD method was intensively developed to analyse pharmaceutical products; the influence of the melting point and volatility of the analytes on the method efficiency was evaluated [ 2324 ].
The use of an ELSD in the study of the lipid composition of the mixtures was introduced at the beginning of the last century [ 26 ]. The HPLC-ELSD method for the evaluation of serum lipids has been optimised and validated, which allows the separation and simultaneous determination of the following components in plasma: The aim of this study was to develop an analytical method that enables quick and reliable determination of the presence of azelaic acid impurities above a certain limit in new liposomal pharmaceutical formulations using HPLC with an ELSD.
Materials and Equipment The following materials and equipment were used: Shexanedioic acid I2, Aldrich, serial number: Soctanedioic acid I4, Aldrich, serial number: Sdecanedioic acid I5, Aldrich, serial number: Sundecanedioic acid I6, Aldrich, serial number: Detection was performed by an ELSD.Available online lausannecongress2018.com Journal of Chemical and Pharmaceutical Research, , 7(4) Research Article ISSN: CODEN(USA): JCPRC5.
Determination of capsaicin and dihydrocapsaicin in some hot chilli varieties by RP-HPLC-PDA International Food Research Journal 19(3): Hence, the overall objective of this work was the development and validation of a routine reversed-phase (RP) HPLC UV method for the quantification of SVT, SVA and coenzyme Q10 CoQ10 from a lecithin/chitosan nanoparticles drug delivery system.
Eurasian Journal of Analytical Chemistry is a peer-reviewed journal and published 8 times per year in January, March, May, July, August, September, October, . Development and Validation of RP-HPLC Method for Simultaneous Determination of Granisetron and Dexamethasone.
The developed method was evaluated for various system suitability parameters and validated for linearity, accuracy, precision, LOD, LOQ as per ICH guidelines. It was also evaluated for bench top stability and freeze/thaw stability. RPHPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms to µL by adding water.
The concentration of RIV.
A simple RP-HPLC method has been developed and validated for the estimation of Rivaroxaban in formulation. Rivaroxaban is a direct factor Xa inhibitor which is indicated for the prevention various coagulative disorders. RPHPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms to µL by adding water. The concentration of RIV. Development and Validation of RP-HPLC Method for Simultaneous Determination of Granisetron and Dexamethasone. The developed method was evaluated for various system suitability parameters and validated for linearity, accuracy, precision, LOD, LOQ as per ICH guidelines. It was also evaluated for bench top stability and freeze/thaw stability.