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نویسندگان: 

ANUMOLU PANIKUMAR DURGA | RANI SOWNDARYA NANDURI SATYAKALA | GALENNAGARI RAJESHWARI | ACHANTA RADHAGAYATHRI | GURRALA SUNITHA

اطلاعات دوره: 
  • سال: 

    2017
  • دوره: 

    11
  • شماره: 

    2
  • صفحات: 

    39-50
تعامل: 
  • استنادات: 

    0
  • بازدید: 

    503
  • دانلود: 

    0
چکیده: 

Two simple, specific, accurate, precise, sensitive and cost effective spectrophotometric methods have been developed and validated for quantification of linagliptin in pure form and pharmaceutical formulations. Method A is established on the computation of absorbance of purple coloured chromogen complex at 463 nm which is formed by the condensation reaction of the primary amine group of linagliptin with vanillin (Schiff base formation). Method B is established on computation of absorbance of orange coloured chromogen at 454 nm which is formed by the condensation reaction of the primary amino group of linagliptin with NQS (1, 2-naphtho quinine 4- sulphonic acid sodium salt) reagent. Two methods executed linearity in the concentration range of 2.5-20 mg/ml and 10-90 mg/ml for method A and B respectively. Linear relationship with good correlation coefficients of 0.998 and 0.995 were monitored between absorbance and corresponding concentrations of linagliptin in vanillin and NQS respectively. The limit of detection, limit of quantification, molar absorptivity, sandell’s sensitivity and ring born concentrationvalues were determined for the two spectrophotometric methods. The contemplated methods were validated statistically as per ICH guidelines. The reliability of both the methods is further ascertained by performing recovery tests by standard addition method. No significant interference was inspected from the excipients commonly used as pharmaceutical aids with the assay procedure. The contemplated methods were simple, sensitive, specific and can be successfully employed in routine analysis of linagliptin in pharmaceutical dosage forms.

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بازدید 503

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اطلاعات دوره: 
  • سال: 

    621
  • دوره: 

    19
  • شماره: 

    1
  • صفحات: 

    61-67
تعامل: 
  • استنادات: 

    0
  • بازدید: 

    17
  • دانلود: 

    0
چکیده: 

Mometasone furoate is a synthetic glucocorticoid with anti-inflammatory and anti-allergic effects, used for the treatment of allergic rhinitis, asthma, and dermatoses. In this study, a spectrophotometric method, as a selective and sensitive method, was developed for the determination of mometasone furoate after DERIVATIZATION. For this purpose, mometasone was first reacted with sodium cyanide to prepare the drug derivatives. After that, the effects of different variables such as reaction solvent, concentration of the reagents, pH, and reaction time were studied. The final results showed that the determination method was linear in the range of 2-18 μg/ml. It seems that after 24 hours, the reaction was complete. The reaction product was characterized by NMR and FT-IR spectroscopy, and the accuracy and precision of the developed method were also studied. At last, the method was checked on Mometasone Ointment (0. 1%), and the results were compared with the results of the HPLC method as a standard method.

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نویسنده: 

MALEKI R. | DARVISH M. | GHESHLAGHI M.

اطلاعات دوره: 
  • سال: 

    2014
  • دوره: 

    22
تعامل: 
  • بازدید: 

    147
  • دانلود: 

    0
چکیده: 

FATTY ACID IS A CARBOXYLIC ACID WITH LONG ALIPHATIC CHAIN, WHICH IS EITHER SATURATED OR UNSATURATED. FATTY ACIDS FOUND IN FATS, OILS AND IN CELL MEMBRANES AS A COMPONENT OF PHOSPHOLIPIDS AND TRIGLYCERIDES [1]. THE INDUSTRIAL EXPLOITATION OF OILS AND FATS IS BASED ON CHEMICAL MODIFICATION OF BOTH THE CARBOXYL AND UNSATURATED GROUPS PRESENT IN FATTY ACIDS. CHEMICAL DERIVATIZATION IS A USEFUL PROCEDURE FOR IMPROVING CHROMATOGRAPHIC BEHAVIOR AND DETECTS ABILITY OF ORGANIC COMPOUNDS BY GAS CHROMATOGRAPHY [2]. IN THIS STUDY, CATALYTIC ACTIVITY OF AL2O3 NANOPARTICELS FOR SYNTHESIS FATTY ACID METHYL ESTERS HAS BEEN INVESTIGATED. AL2O3 NANOPARTICELS HAS BEEN SUCCESSFULLY SYNTHESIZED BY SOL-GEL PROCEDURE FROM AL (NO3) 3.9H2O AND CHARACTERIZED BY SCANNING ELECTRON MICROSCOPY (SEM) [3]. FATTY ACIDS WERE ESTERIFIED BY METHANOL IN THE PRESENCE OF AL2O3 NANOPARTICELS AS NANOCATALYST. THE EFFECT OF REACTION TIME, TEMPERATURE, METHANOL VOLUME AND AMOUNT OF NANOCATALYST WERE STUDIED AND OPTIMUM CONDITIONS WERE SELECTED. THE USE OF NANOCATALYST NOT ONLY FACILITATES THE REACTION BUT ALSO MEETS THE GOALS OF GREEN CHEMISTRY. THE COMMON PROCEDURE HAS DIFFERENT STEPS (HYDROLYSIS, ESTERIFICATION AND SEPARATION), USES HIGH CONCENTRATION OF H2SO4 AND NORMAL HEPTANE BUT THE PROPOSED METHOD IS SIMPLE, RAPID AND USE ONLY METHANOL AS SOLVENT AND REAGENT. SEPARATION, DETECTION AND QUANTITATION OF FATTY ACIDS AFTER PROPOSED DERIVATIZATION PROCESS WERE PERFORMED WITH A GAS CHROMATOGRAPH FITTED WITH A DB-225MS CAPILLARY COLUMN (30 M×0.25 MM I.D., 0.25 MM FILM THICKNESS), A SPLIT–SPLITLESS INJECTOR AND FLAME IONIZATION DETECTOR.

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بازدید 147

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اطلاعات دوره: 
  • سال: 

    2014
  • دوره: 

    20
تعامل: 
  • بازدید: 

    140
  • دانلود: 

    0
کلیدواژه: 
چکیده: 

GAS CHROMATOGRAPHY (GC) IS A POPULAR TECHNIQUE FOR THE ANALYSIS OF PHENOL COMPOUNDS.HOWEVER, BECAUSE OF THEIR HIGH POLARITY, THESE ANALYTES TEND TO GIVE BROAD, TAILED PEAKS, AND THESE EFFECTS INCREASE AS THE CHROMATOGRAPHIC COLUMN AGES. TO AVOID THESE DRAWBACK, SEVERAL DERIVATIZATION REACTIONS HAVE BEEN PROPOSED TO TRANSFORM PHENOLS IN LESS POLAR COMPOUNDS, WITH BETTER CHROMATOGRAPHIC CHARACTERISTICS. PHENOL ACETYLATION WITH ACETIC ANHYDRIDE IN PRESENCE OF CARBONATE OR HYDROGENCARBONATE, IS ONE OF THE MOST COMMON DERIVATIZATION PROCEDURES. REACTION CAN BE PERFORMED IN AQUEOUS SAMPLES IN A FEW MINUTES WITH HIGH EFFICIENCY. PHENYL ACETATE WAS EXTRACTED BY SEVERAL METHODS [1-3].IN THIS RESEARCH, WE COMPARED SOLID-PHASE EXTRACTION (SPE) WITH CONVENTIONAL REVERSED PHASE ADSORBENT SUCH AS C18 AND LIQUID-LIQUID EXTRACTION (LLE) WITH N-HEXAN. ACCORDING TO RESULTS, EXTRACTION EFFICIENCY IN SPE PROCEDURE IS LOWER THAN LLE AND TIME CONSUMING. THE EXTRACTED SAMPLES WAS ANALYZED BY GAS CHROMATOGRAPHY WITH MASS SPECTROMETRY DETECTION (GC–MS).EXPERIMENTS, WERE PERFORMED TO CHECK THE EFFECT OF SAMPLE CONCENTRATION AND DETERMINATION OF EFFICIENCY OF RECOVERY, ULTRAPURE WATER WAS SPIKED BY THREE CONCENTRATION LEVELS OF PHENOL.THE MEAN RECOVERY AND RELATIVE STANDARD DEVIATION IS 85±7.8%. CALIBRATION CURVE WAS LINEAR IN THE CONCENTRATION RANGE OF 10 NG ML-1 TO 2 MG ML-1 IN THE ORIGINAL SOLUTION AND CORRELATION COEFFICIENT IS 0.9998. THE DEVELOPED METHOD HAS BEEN USED TO MONITOR PHENOL CONTAMINATION IN RIVER WATER SAMPLES COLLECTED FROM ZAYANDEROUD RIVER IN ISFAHAN PROVINCE, IRAN.

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بازدید 140

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نویسندگان: 

HAJ MOHAMMADI M.R. | JAFARI S.

اطلاعات دوره: 
  • سال: 

    2006
  • دوره: 

    25
  • شماره: 

    1
  • صفحات: 

    19-23
تعامل: 
  • استنادات: 

    0
  • بازدید: 

    403
  • دانلود: 

    0
چکیده: 

Separation of some biogenic amines via RP-HPLC using mixed micellar mobile phase was investigated. The compounds were derivatized before hand by dansyl chloride as a chromophoric reagent. Appropriate conditions for separation, were determined by studying factors such as temperature, type and percentage of organic modifier, concentration of surfactants (SDS and Brij-35) and the pH of the mobile phase. The number of theoretical plates (N), asymmetry factor (B/A) and selectivity factor (α) considered as criteria for finding the appropriate conditions for separation. Appropriate condition, were: 40˚C, 40 mM SDS, 0.5 mM Brij-35 and 10% 1-propanol at pH=5.

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بازدید 403

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نشریه: 

Acta Medica Iranica

اطلاعات دوره: 
  • سال: 

    2006
  • دوره: 

    44
  • شماره: 

    4
  • صفحات: 

    225-229
تعامل: 
  • استنادات: 

    0
  • بازدید: 

    326
  • دانلود: 

    0
چکیده: 

Fatty acids play important roles in biological systems and the newborns fatty acids requirements are covered only by the milk. It is of particular interest to qualify the content of the fatty acids in the milk. This study was performed to determine the levels of some fatty acids in the infant formulas and also to describe a method without DERIVATIZATION for the fatty acids analysis and applying it to the control of infant formulas. Free fatty acids were produced by adding isopropanol-KOH to milk fat extract and heating it to saponify and acidify by H2SO4. Free fatty acids were extracted and were quantified by capillary gas chromatography on a fused silica column (AT-1000) and flame ionization detector. The average experimental values of lauric, palmitic, stearic and linoleic fatty acids contents of twenty infant formulas were 6.47, 16.52, 2.11 and 14.56 g/100g, respectively. The obtained experimental values of lauric and linoleic fatty acids contents of twenty infant formulas were in good agreement with the values proposed by standards of codex alimentary.

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بازدید 326

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اطلاعات دوره: 
  • سال: 

    2015
  • دوره: 

    12
  • شماره: 

    6
  • صفحات: 

    1061-1069
تعامل: 
  • استنادات: 

    0
  • بازدید: 

    339
  • دانلود: 

    0
چکیده: 

In this study, a simple, rapid, and an economical method has been proposed for the extraction, preconcentration, and determination of parabens (methyl-, ethyl-, and propylparaben) in different samples based on DERIVATIZATION by acetic anhydride and preconcentration using air-assisted liquid–liquid microextraction in a single step. In this method, 1, 1, 2, 2-tetrachloroethane (extraction solvent) containing mL-level of acetic anhydride (DERIVATIZATION agent) is injected into aqueous sample containing parabens and picoline (catalyst). The mixture of aqueous and organic phases is withdrawn into a glass syringe and then injected into the test tube for several times till a turbid solution is obtained. After centrifuging, 1 mL of the sedimented phase is injected into gas chromatography-flame ionization detector. The effect of catalyst volume, DERIVATIZATION agent volume, extraction solvent type and volume, ionic strength of the solution, pH, and numbers of extraction on the extraction efficiency is investigated. Under the optimal conditions, the enrichment factors and enhancement factors for the parabens were obtained in the ranges of 310-353 and 2,484-5,298, respectively. Limits of detection were between 0.18 and 8.5 mg L-1. The method was found to be linear over the range of 10-10,000 mg L-1 with good coefficients of determination (R2 > 0.999). The obtained extraction recoveries ranged from 69 to 107 % and precision of the method, expressed as relative standard deviation (RSD %), was within the range of 4.0-13 %. The proposed method was successfully applied for determination of parabens in different samples such as cream, toothpaste, and mouthwash.

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بازدید 339

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نویسندگان: 

نشریه: 

Antioxidants (Basel)

اطلاعات دوره: 
  • سال: 

    2022
  • دوره: 

    11
  • شماره: 

    -
  • صفحات: 

    1165-1165
تعامل: 
  • استنادات: 

    1
  • بازدید: 

    1
  • دانلود: 

    0
کلیدواژه: 
چکیده: 

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بازدید 1

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اطلاعات دوره: 
  • سال: 

    2014
  • دوره: 

    20
تعامل: 
  • بازدید: 

    130
  • دانلود: 

    0
کلیدواژه: 
چکیده: 

PHENOLS ARE FOUND AMONG THE OXYGENATED COMPOUNDS PRESENT IN PETROLEUM. THE INTEREST IN THE DETERMINATION OF PHENOLS IN CRUDE OILS AND FUELS LIES IN THE FACT THAT, UPON STORAGE, PHENOLS AND OTHER POLAR COMPOUNDS PROMOTE DEPOSIT FORMATION, WITH DELETERIOUS EFFECTS FOR FUEL QUALITY AND STABILITY [1]. SEVERAL SAMPLE PREPARATION METHODS HAVE BEEN DEVELOPED FOR THE ANALYSIS OF PHENOLS SUCH AS LIQUID–LIQUID EXTRACTION, SOLID-PHASE MICROEXTRACTION, SUPERCRITICAL-FLUID EXTRACTION, ULTRASONIC EXTRACTION, MICROWAVE-ASSISTED EXTRACTION, AND DISPERSIVE LIQUID–LIQUID MICROEXTRACTION.THE GOAL OF THIS STUDY WAS TO DEVELOP A SIMPLE AND RAPID METHOD FOR ISOLATION, ENRICHMENT, AND DETERMINATION OF PHENOLS IN FUELS BY COMBINATION OF LIQUID-LIQUID EXTRACTION AND AIR-ASSISTED LIQUID-LIQUID MICROEXTRACTION (AALLME) FOLLOWED BY GC-FID DETERMINATION [2]. THIS METHOD CONSIST OF TWO STEPS: (I) EXTRACTION OF PHENOLS FROM FUELS BY BACK EXTRACTION INTO NAOH SOLUTION, AND (II) SIMULTANEOUS DERIVATIZATION AND ENRICHMENT OF PHENOLS WITH DURING AN AALLME PROCEDURE. IN THE SECOND STEP, BUTYLCHLOROFORMATE (AS DERIVATIZATION AGENT) AND TETRACHLORO ETHANE (AS EXTRACTION SOLVENT) WERE TRANSFERRED INTO AQUEOUS SAMPLE SOLUTION IN A CONICAL TEST TUBE. THE MIXTURE WAS REPEATEDLY SUCKED INTO A GLASS SYRINGE AND INJECTED INTO THE TUBE. BY THIS ACTION THE TURBIDITY OF SOLUTION INCREASED MORE AND MORE. AFTER PERFORMING PREDETERMINED CYCLES, THE MIXTURE WAS CENTRIFUGED AND 1 ML OF THE SEDIMENTED PHASE WAS ANALYZED BY GC-FID. THIS TECHNIQUE WAS SUCCESSFULLY APPLIED FOR THE EXTRACTION/PRECONCENTRATION AND DERIVATIZATION OF THE SELECTED PHENOLS FROM DIFFERENT SAMPLES SUCH AS GASOLINE, KEROSENE, GAS OIL, AND ENGINE OIL.UNDER THE OPTIMUM CONDITIONS, ENRICHMENT FACTORS, EXTRACTION RECOVERIES, AND LIMIT OF DETECTION WERE IN THE RANGES OF 568 TO 1128, 70-100%, AND 0.81-2.00 MG L-1, RESPECTIVELY.

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اطلاعات دوره: 
  • سال: 

    2013
  • دوره: 

    10
  • شماره: 

    6
  • صفحات: 

    1257-1262
تعامل: 
  • استنادات: 

    0
  • بازدید: 

    286
  • دانلود: 

    0
چکیده: 

Electrochemical oxidation of levodopa (LD) as one of the most well-known neurotransmitters has been studied in the presence of some aniline derivatives. The electron transfer of LD is followed by two competitive reactions in the presence of these amines. The reactions are the Michael additions of side chain amine group of LD and/or aromatic amines to electrochemically generated o-quinone. There are two ECE mechanisms for both pathways and the competition between these inter and intramolecular reactions drastically depends on the pH of the medium. The pH dependence of reactions has been studied and the observed homogeneous rate constants of the reactions were estimated by digital simulation of cyclic voltammograms. The effect of aniline substituents was also studied with regard to their reactivities toward o-quinone of LD and the competitive reactions. Based on the obtained results, the products of intermolecular reactions are electroactive diphenylamine derivatives and their half-wave potentials depend on the nature of the aniline substituent.

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