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1.
Simple, sensitive, and accurate visible spectrophotometric methods are described for the determination of paroxetine hydrochloride (PA) in tablets. Among them, the first 3 methods are based on the ion-pair complexes of PA formed with bromothymol blue (BTB), bromophenol blue (BPB), and bromocresol green (BCG) in aqueous acidic buffers. The complex species extracted into chloroform were quantitatively measured at 414 nm with BTB and BCG and at 412 nm with BPB. Beer's law was obeyed over the concentration ranges of 2-20, 2-16, and 2-16 microg/mL, respectively. The fourth method described is based on a coupling reaction between PA and 7-chloro-4-nitrobenzofurazon (NBD-Cl) in borate buffer, pH 8.5, in which a yellow reaction product that was measured at 478 nm was formed. The Beer's law range for this method was 2-10 microg/mL. The last method developed describes the interaction of PA base, as an n-electron donor, with 7,7,8,8-tetracyanoquinodimethane (TCNQ), as a pi-acceptor, in acetonitrile to give blue-colored TCNQ- radical anion with absorption maxima at 750 and 845 nm. Measured at 845 nm, the absorbance-concentration plot was rectilinear over the range of 1.5-15 microg/mL. The new methods developed were successfully applied to the determination of PA in tablets without any interference from common tablet excipients. The results of the methods were in good agreement with those obtained with an official liquid chromatographic method. This report describes first colorimetric methods for the determination of PA.  相似文献   

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Simple and sensitive Spectrophotometric methods for the determination of labetalol hydrochloride are described. The first two are based on the oxidative coupling reaction of labetalol hydrochloride withp-N,N-dimethyl-phenylenediamine dihydrochloride (method A, max 685 nm) and 3-methyl-2-benzothiazolinone hydrazone hydrochloride (method B, max 545 nm) in the presence of sodium hypochlorite and eerie ammonium sulphate as oxidants, respectively. The third depends on the formation of an ion-association complex of labetalol hydrochloride with suprachen violet 3B at pH 1.3, which is extracted into chloroform (method C, max 565 nm). The methods obey Beer's law and the precision and accuracy of the methods were checked against the B.P. reference method and the relative standard deviations were in the range 0.35–0.52%. These methods are applied to the determination of labetalol in dosage forms.  相似文献   

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A binary mixture of ciprofloxacin hydrochloride (CIP) and metronidazole (MET) was determined by five simple and accurate methods, without prior separation. In the first method, CIP was determined by second derivative spectrophotometric method ((2)D) by measuring the amplitude at 282 nm (zero ordinate value of MET). On the other hand, the determination of MET was based on isosbestic point technique, where the total content of the mixture was determined at 294.5 nm (isosbestic point), then the content of MET could be calculated by subtraction. The second method was first derivative ratio spectrophotometric method ((1)DD) where the total amplitude at 261 and 285 nm and the amplitude at 295.5 nm were selected to simultaneously determine CIP and MET in binary mixture, respectively. The third method was based on dual wavelength analysis, in which two wavelengths were selected, at which the absorbances of the other component were the same. The fourth method depends on using Q-analysis method (absorbance ratio) which involves the formation of Q-absorbance equation using the respective absorptivity values at 294.5 nm (isosbestic point) and 281.5 nm (λ(max) of CIP). The fifth method is partial least-squares (PLS) chemometric technique for determination of CIP and MET. The developed methods were successfully applied to the analysis of CIP and MET in laboratory prepared mixtures and tablets with good recoveries and their validation was carried out following the International Conference on Harmonization (ICH) guidelines. The results obtained were statistically compared with each other showing no significant difference with respect to accuracy and precision.  相似文献   

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El-Shabouri SR 《Talanta》1986,33(9):743-744
A sensitive spectrophotometric method is reported for the determination of nitrazepam either in pure form or in tablets. The method is based on reduction with zinc dust and calcium chloride followed by reaction with sodium pentacyanoaminoferrate(II) to give a violet product having an absorbance maximum at 560 nm. Beer's law is obeyed over the concentration range 1-20 mug ml in the final solution. The common excipients in tablets do not interfere. The recovery and precision are similar to those of the official B.P. method.  相似文献   

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Three simple, sensitive and reproducible visible spectrophotometric methods (A-C) for the determination of mebeverine hydrochloride (MVH) in bulk samples and pharmaceutical formulations are described. Methods A and B are based on the formation of ion-association complexes between the drug and fast green FCF (FGFCF, max 625 nm) or bromothymol blue (BTB, max 405 nm). Method C is based on the formation of a molecular complex between the drug and cobalt thiocyanate (CTC, max 625 nm). Regression analysis of Beer's plots showed good correlation in the concentration ranges 2–40, 2–25 and 100–600 g/ml for methods A, B and C respectively. No interference was observed from the usually existing additives in pharmaceutical formulations and the applicability of the methods was examined by analysing tablets containing MVH. Standard deviations were typically 0.75 mg per dose (RSD: 0.25–0.5%). Recoveries were 99.0–100.2%.  相似文献   

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Three sensitive, selective, accurate spectrophotometric and spectrofluorimetric methods have been developed for the determination of ropinirole hydrochloride in tablets. The first method was based on measuring the absorbance of drug solution in methanol at 250 nm. The Beer's law was obeyed in the concentration range 2.5-24 microg ml(-1). The second method was based on the charge transfer reaction of drug, as n-electron donor with 7,7,8,8-tetracyanoquinodimethane (TCNQ), as pi-acceptor in acetonitrile to give radical anions that are measured at 842 nm. The Beer's law was obeyed in the concentration range 0.6-8 microg ml(-1). The third method was based on derivatization reaction with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer of pH 8.5 followed by measuring the fluorescence intensity at 525 nm with excitation at 464 nm in chloroform. Beer's law was obeyed in the concentration range 0.01-1.3 microg ml(-1). The derivatization reaction product of drug with NBD-Cl was characterized by IR, 1H NMR and mass spectroscopy. The developed methods were validated. The following analytical parameters were investigated: the molar absorptivity (epsilon), limit of detection (LOD, microg ml(-1)) and limit of quantitation (LOQ, microg ml(-1)), precision, accuracy, recovery, and Sandell's sensitivity. Selectivity was validated by subjecting stock solution of ropinirole to acidic, basic, oxidative, and thermal degradation. No interference was observed from common excipients present in formulations. The proposed methods were successfully applied for determination of drug in tablets. The results of these proposed methods were compared with each other statistically.  相似文献   

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Chiswell B  Rauchle G  Pascoe M 《Talanta》1990,37(2):237-259
A comprehensive and critical review of the available spectrophotometric methods for the determination of manganese is presented. Details are given of a wide range of direct colour-forming reactions of manganese with organic ligands, which have been claimed to be of use in analysis for the metal. The use of the very sensitive kinetic methods of analysis is also discussed. It is found that there is a paucity of reliable detail concerning the general applicability of most methods to manganese determination and that there is even less detail on the comparative value of different methods for determination of the metal in particular types of matrix.  相似文献   

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Sastry CS  Sastry BS  Rao JV  Krishna RR 《Talanta》1993,40(4):571-576
Two simple and sensitive visible spectrophotometric methods (methods A and B) for the determination of tolnaftate in bulk samples and formulations are described. Method A (lambda(max) 490 nm) involves the reaction of tolnaftate with 2,6-dichloroquinone-4-chlorimide (DCQC: Gibb's reagent), while method B (lambda(max) 530 nm) is based on a similar reaction of the drug with p-N,N-dimethylphenylene diamine in the presence of chloramine-T. Both these methods are applicable to pure samples as well as formulations of the drug.  相似文献   

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Sastry CS  Rao JS  Rao KR 《Talanta》1995,42(10):1479-1485
Three simple and sensitive spectrophotometric methods for the determination of tamoxifen citrate have been developed. They are based on the formation of an ion-association complex between the drug and a dye, Erioglaucine A, which is extractable into chloroform and has an absorption maximum at 625 nm (method A), oxidation with excess potassium permanganate and the determination of unconsumed permanganate using Fast Green FCF (method B), or by the formation of a coloured cobalt thiocyante coordination complex which is extracted into benzene and measured at 635 nm (method C). Beer's law limits for methods A, B, and C are 0.5-3.0 mug ml(-1), 1.0-6.0 mug ml(-1) and 100-500 mug ml(-1), respectively. No interference was observed from tableting additives and the applicability of the methods was examined by analysing tablets containing tamoxifen. The quantities determined were 99.0-100.03% of the exptected values.  相似文献   

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A spectrophotometric procedure for the determination of sertraline hydrochloride (Sert) and/or clidinium bromide (Clid) in bulk sample and in dosage forms was developed. The purpose of this work was to develop a rapid, simple, inexpensive, precise, and accurate visible spectrophotometric method. The procedure is based on formation of an ion-pair complex by their reaction with bromocresol green (BCG), bromophenol blue (BPB), and bromothymol blue (BTB) in buffered aqueous solution at pH 3. The colored products are extracted into a polar solvent and measured spectrophotometrically at the optimum λmax for each complex. Optimization of different experimental conditions is described. Regression analysis of Beer-Lambert plots showed good correlation in the concentration range of 1–30 μg mL−1. The apparent molar absorptivity, Sandell sensitivity, detection and quantification limits were calculated. For more accurate analysis, Ringbom optimum concentration range of 2–27 μg mL−1 was used. The developed methods were successfully applied for the determination of sertraline hydrochloride and clidinium bromide in bulk in pharmaceutical formulations without any interference from common excipients. The procedure has the advantage of being highly sensitive and simple for the determination of the studied drugs, weak UV-absorbing compounds.  相似文献   

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Sastry CS  Rao TT  Sailaja A 《Talanta》1991,38(9):1057-1060
A sensitive spectrophotometric method is described for the determination of nicoumalone (NIC), acebutolol hydrochloride (ACBH) or procainamide hydrochloride (PAH) either in pure form or in pharmaceutical formulations. The method is based on the oxidative coupling reaction through the involvement of an aromatic primary amino group (released through reduction in NIC or hydrolysis in ACBH or existing free in PAH) in the drug with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in the presence of ferric chloride [Fe(III)]. The resulting chromophores are measured at 620 nm for NIC and ACBH and 580 nm for PAH. The concentration measurements are reproducible within a relative standard deviation of 1%.  相似文献   

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