A Validated Reverse Phase HPLC Technique for the Determination of TATB Assay (original) (raw)
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Journal of Chromatography A, 1995
A single method was developed for the separation and quantitation of hexahydro-1,3,5-trinitro-1,3,5-triazine, 2,4,6-trinitrotoluene (TNT), and most of the known and suspected biodegradation intermediates of TNT by RP-HPLC and diode array detection. The known biodegradation intermediates of TNT analyzed were 2-amino-4,6-dinitrotoluene, 4-amino-2,6-dinitrotoluene, 2,6-diamino-4-nitrotoluene, 2,4-diamino-6-nitrotoluene, 2,4,6-triaminotoluene, 2,2′,6,6′-tetranitro-4,4′-azoxytoluene, and 4,4′-azoxytoluene, and 4,4′,6,6′-tetranitro-2,2′-azoxytoluene. The suspected biodegradation intermediates of TNT included 1,2,3-benzenetriol (pyrogallol), 1,3,5-benzenetriol (phloroglucinol), 2-methyl-1,3,5-benzenetriol (methyl phloroglucinol) and 4-methylphenol (p-cresol). Mobile phases consisting of aqueous buffers adjusted to three different pH values in a gradient with acetonitrile were examined for their efficiency in separating the intermediate compounds and for the minimization of speciation of the ionizable intermediates (e.g. 2,4,6-triaminotoluene). A final aqueous buffer pH of 3.2 was selected to minimize the interference to the separation caused by 2,4,6-triaminotoluene speciation. Solvent consumption was minimized by the use of a narrow-bore column. All of the known reduction products as well as p-cresol and methylphloroglucinol were identified in culture supernatants from TNT-degrading cultures while pyrogallol and phloroglucinol were not.
International Journal of Advance Research Ideas and Innovations in Technology
The Atrazine and Terbuthylazine molecules are being used alone and a combination as a special herbicide activity to control the broadband leaves in the agricultural industry. Atrazine and Terbuthylazine have a high capillary action in the roots of brad spectrum plants with respect to other herbicide molecules. The solubility of Atrazine and Terbuthylazine also very high solubility in water and this solubility enhanced the capillary action through the broad leaves plant roots. The persistence of this Atrazine and Terbuthylazine is very long period hence the residue levels in the used substrates are being existed in the used substrates. Even though the molecules Atrazine and Terbuthylazine are less toxic to humans and animals, the lowest detection levels have to be determined with a simple HPLC analytical method; which is very effective time and cost of analysis. Within 10 minutes of analysis time these two molecules to be determined by using acetonitrile and water as a mobile phase with a ratio of 80:20 (volume/volume) with the help of Quails BDS C18 (250 x 4.6, 5μ) HPLC column at 1 ml/min. flow rate. The detection wavelength is 220 nm by a Shimadzu LC2030 model HPLC. The results of the analysis deliver that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the identification and quantifications of these molecules interims of validation parameters viz., separation, system suitability, System Precision and linearity in a simple HPLC analysis.
2014
A novel, simple, precise and stability indicating r everse phase high performance liquid chromatography method has been developed and valida ted for the assay determination of Tetrabenazine in bulk drug and dosage form. LC separation was achieved on a Xterra RP18 (4.6x150) mm, 3.5 μm column in isocr ati mode using buffer(0.01M K 2HPO4) and acetonitrile in the ratio 50:50(v/v) as m obile phase, pumped in to the column at flow rate 1.0 ml/min and the detection of eluent from the column was carried out using Photo Diode array detector at 210 nm. The column was maintained at 25 ̊c temperature and the total run time was 15m in. The retention time of Tetrabenazine was 6.4min and the standard curves were linear over the concentrat ion range of 20-150 μg/ml with r = 0.9999. The percentage relative standard deviatio n in accuracy and precision studies was found to be less than 2%. The method wa s successfully validated as per ICH guidelines. Val idation studies demonstrated that the proposed...
1-Triacontanol (TRIA) is gaining a lot of interest in agricultural practice due to its use as bio-stimulant and different types of TRIA-containing products have been presented on the market. Up to date, TRIA determination is performed by GC analysis after chemical derivatization, but in aqueous samples containing low amounts of TRIA determination can be problematic and the derivatization step can be troublesome. Hence, there is the need for an analysis method without derivatization. TRIA-based products are in general plant extracts that can be obtained with different extraction procedures. These products can contain different ranges of concentration of TRIA from units to thousands of mg/kg. Thus, there is the need for a method that can be applied to different sample matrices like plant materials and different plant extracts. In this paper we present a HPLC-ELSD method for the analysis of TRIA without derivatization. The method has been fully validated and it has been tested analyzing the content of TRIA in different dried vegetal matrices, plant extracts, and products. The method is characterized by high sensitivity (LOD = 0.2 mg/L, LOQ = 0.6 mg/L) and good precision (intra-day: <11.2%, inter-day: 10.2%) being suitable for routine analysis of this fatty alcohol both for quality control or research purposes.