scholarly journals Liquid Chromatographic Determination of Fentin Acetate in Fentin and Maneb Formulations

1996 ◽  
Vol 79 (4) ◽  
pp. 829-832
Author(s):  
Euphemia Papadopoulou-Mourkidou ◽  
John Patsias ◽  
George Papadopoulos ◽  
Costas Galanis

Abstract A normal-phase liquid chromatographic (LC) system is presented for determination of fentin acetate in fentin and fentin-maneb wettable powder formulations. Fentin acetate is extracted from both formulations with glacial acetic acid-hexane (20 + 80), and the extract is analyzed after appropriate dilution. An isocratic LC system equipped with a photodiode array detector and a silica gel column, which is eluted with glacial acetic acid-hexane (5 + 95), are used. Quantitation at 258.5 nm is based on an external standard calibration curve. Relative standard deviations were 0.2 and 2.3% for the mean levels (w/w) of fentin acetate determined in fentin and fentin-maneb formulations, respectively.

1982 ◽  
Vol 65 (4) ◽  
pp. 927-929
Author(s):  
Brian R Bennett ◽  
Gregory S Grimes

Abstract Chlorophacinone and diphacinone are extracted at the 0.005% level from grain or paraffinized baits with glacial acetic acid. The target concentration is 0.01 mg/mL. The filtered supernate is chromatographed on a Partisil PXS ODS10/25 liquid chromatography column with premixed and degassed glacial acetic acid-tetrahydrofuran-water (14 + 2 + 9) and detected at 288 nm. The concentration is calculated by using an external standard. The recovery from spiked samples averaged 96.6% for both analytes. The response is linear from 0.001 to 0.040 mg/mL. The coefficient of variation of within-day replicates ranged from 1.1 to 2.5%.


1988 ◽  
Vol 71 (2) ◽  
pp. 321-322 ◽  
Author(s):  
Rodney J Bushway ◽  
L Brian Perkins ◽  
King M Joan

Abstract A liquid chromatographic (LC) method has been developed to analyze simultaneously separate formulations of diazinon and chlorpyrifos. Samples of each formulation were mixed in a Polytron mixer with the internal standard butylated hydroxytoluene and were diluted with acetonitrile. An aliquot was injected into an Ultremex LC column. The mobile phase was acetonitrile-water-tetrahydrofuran-glacial acetic acid-monoethanolamine (480 + 230 + 55 + 2 + 0.75); all 3 compounds were monitored at 230 nm. Total analysis time was 11 min. Combinations of 11 different samples of each formulated pesticide were analyzed 9 times for coefficients of variation generally less than 3%. Purity of the diazinon, chlorpyrifos, and butylated hydroxytoluene was checked by using a photodiode array detector in the spectrum and absorbance ratio modes. No interferences were noted at 230 nm.


Author(s):  
Saniye Özcan ◽  
Serkan Levent ◽  
Nafiz Öncü Can

: The alkyl esters of p-hydroxybenzoic acid at the C-4 position, “the parabens,” including methyl, ethyl, propyl, and butyl, are widely used as antimicrobial preservatives in foods, cosmetics, and pharmaceuticals. Official regulations on the use of these compounds make their analysis essential for the estimation of their exposure. On this basis, the presented study was realized to develop a simple, selective and cheap high-performance liquid chromatographic method for the quantitative determination of methyl paraben (MP), ethyl paraben (EP), n-propyl paraben (NPP), isopropyl paraben (IPP), n-butyl paraben (NBP), isobutyl paraben (IBP) and benzyl paraben (BP) in pharmaceuticals and cosmetic products. The chromatographic separation of the analytes was achieved under flow rate gradient elution conditions using a C18-bonded core-shell silica particle column (2.6 μm particle size, 150 × 3.0 mm from Phenomenex Co.). The samples were injected into the system as aliquots of 1.0 μL, and the compounds were detected by using a photodiode array detector set at 254 nm wavelength. With this technique, seven paraben derivatives can be determined in the concentration range of 250-2000 ng/mL. The recovery of the method is in the range of 99.95-13.84%, and the RSD is at a maximum value of 3.95%. The proposed method was fully validated and successfully applied to different pharmaceutical and cosmetic samples (n=16), including syrups, suspensions, oral sprays, gels, etc. At least one paraben derivative was detected in six of the samples, and was determined quantitatively. The maximum amount of a paraben derivative found in the analyzed samples is 321.7 ng/mL, which was MP. To the best of our knowledge, this is the first LC method, which is applicable both on pharmaceutical and cosmetic samples.


2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Chang-Seob Seo ◽  
Jung Hoon Kim ◽  
Hyeun-Kyoo Shin

A simple, rapid, and accurate high-performance liquid chromatographic method was applied to the quantitative analysis of six components of a traditional herbal formulation, Insampaedok-san (ISPDS): liquiritin (1), ferulic acid (2), naringin (3), hesperidin (4), neohesperidin (5), and glycyrrhizin (6). The six components were separated within 35 min using a Gemini C18 column maintained at 40°C. The mobile phase was composed of 1.0% (v/v) aqueous acetic acid (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient elution. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254, 280, and 320 nm. The calibration curves showed good linearity (R2=1.0000) for different concentration ranges. The recovery of each component was in the range of 92.62%–105.96%, with a relative standard deviation (RSD) of less than 4.0%. The RSDs for intra- and interday precision were 0.04%–1.70% and 0.06%–2.56%, respectively. The concentration of each of the six components of ISPDS was in the range 0.72–9.88 mg g−1.


1984 ◽  
Vol 67 (4) ◽  
pp. 707-709 ◽  
Author(s):  
Gaman Shah ◽  
Dorothy Bradley ◽  
Efraim Shek

Abstract A relatively simple analytical method is presented for determination of oxfendazole (2-(methoxycarbonylamino)-5-phenylsulfinyl-benzimidazole) at levels as low as 0.012% in swine feeds, using cation exchange liquid chromatography (LC). The sample was extracted with a solvent mixture of methanol-glacial acetic acid (90 + 10) at 45°C, using a gyrorotory shaker. Plant pigments and other feed excipients were removed using zinc acetate treatment and pH-controlled extraction. Oxfendazole was further separated from the remaining interferences and quantitatively determined by LC on a Partisil SCX column with acetonitrile-1.01M phosphate buffer as mobile phase. The method is stability-specific, linear, precise, and accurate at 80-120% labeled strength (relative standard deviation 0.9-1.7 with mean recovery of 98-99%). Supporting data at a level of 0.0135% oxfendazole in swine feed indicated that this method is capable of complete recovery of oxfendazole from medicated swine feeds.


2006 ◽  
Vol 89 (4) ◽  
pp. 937-941 ◽  
Author(s):  
Alpana Srivastava ◽  
Richa Pandey ◽  
Ram K Verma ◽  
Madan M Gupta

Abstract A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanolwater (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 μm, 125 × 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 μg/mL). Detection limits were 10 μg/mL for sennoside B and 35 μg/ML for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 μg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.


2007 ◽  
Vol 90 (6) ◽  
pp. 1566-1572 ◽  
Author(s):  
Paulo Renato Oliveira ◽  
Thiago Barth ◽  
Vitor Todeschini ◽  
Sérgio luiz Dalmora

Abstract A reversed-phase liquid chromatographic (LC) method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical dosage forms. The LC method was carried out on a Synergi fusion C18 column (150 mm 4.6 mm id) maintained at 45C. The mobile phase consisted of phosphate buffer 0.03 M, pH 4.5acetonitrile (35 + 65, v/v) run at a flow rate of 0.6 mL/min, and detection was made using a photodiode array detector at 234 nm. The chromatographic separation was obtained within 15.0 min, and calibration graphs were linear in the concentration range of 0.5200 g/mL. Validation parameters such as specificity, linearity, precision, accuracy, and robustness were evaluated, giving results within the acceptable range for both compounds. Moreover, the proposed method was successfully applied for the routine quality control analysis of pharmaceutical products.


2000 ◽  
Vol 83 (1) ◽  
pp. 237-240 ◽  
Author(s):  
Eshwar Jagerdeo ◽  
Erin Passetti ◽  
Sumer M Dugar

Abstract This paper describes a reversed-phase liquid chromatographic method for the determination of vanillin, associated natural aromatic compounds and/or synthetic precursors, ethyl vanillin, and coumarin, a commonly encountered adulterant in nonbeverage and beverage alcohol products using a ternary gradient mobile phase. The compounds were separated on a Nova-Pak C18 column by using water, methanol, and tetrahydrofuran as the mobile phase. Measurements were made by using a photodiode array detector at 275 nm. The choice of the mobile phase and the column provides baseline resolution of vanillin and the associated aromatic compounds commonly found in vanilla-flavoring material. Because this method provides low-level detection/quantitation, it is suitable for the characterization of vanilla flavoring materials that are currently added to vanilla flavored beverage alcohol products.


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