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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   

2.
Five simple and sensitive methods were developed for the determination of leflunomide (I) in the presence of its degradates 4-trifluoromethyl aniline (II) and 3-methyl-4-carboxy isoxazole (III). Method A was based on differential derivative spectrophotometry by measuring the delta(1)D value at 279.5 nm. Beer's law was obeyed in the concentration range of 2.00-20.00 microg/mL with mean percentage accuracy of 100.07 +/- 1.32. Method B depended on first-derivative spectrophotometry and measuring the amplitude at 253.4 nm. Beer's law was obeyed in the concentration range of 2.00-16.00 microg/mL with mean percentage accuracy of 98.42 +/- 1.61. Method C was based on the reaction of degradate (II) with 2,6-dichloroquinone-4-chloroimide (Gibbs reagent). The colored product was measured at 469 nm. Method D depended on the reaction of degradate (II) with para-dimethyl aminocinnamaldehyde (p-DAC). The absorbance of the colored product was measured at 533.4 nm. Method E utilized 3-methyl-2-benzothiazolinone hydrazone in the presence of cerric ammonium sulfate with degradate (II). The green colored product was measured at 605.5 nm. The linearity range was 40.00-280.00, 2.40-24.00, and 30-250 microg/mL with mean percentage accuracy of 100.75 +/- 1.21, 100.13 +/- 1.45, and 99.74 +/- 1.39 for Methods C-E, respectively. All variables were studied to optimize the reaction conditions. The proposed methods have been successfully applied to the analysis of leflunomide in pharmaceutical dosage forms and the results were statistically compared with that previously reported.  相似文献   

3.
A simple and sensitive spectrophotometric method is suggested for analysis of 3 antihistaminic drugs, acrivastine (I), mequitazine (II), and dimethindene maleate (III). The method is based on reaction of the drugs with 7,7,8,8-tetracyanoquinodimethane (TCNQ) in acetonitrile to form highly stable colored products that are measured at 750, 766, and 844 nm for I and II, and 480 and 618 nm for III. Beer's law is obeyed in the ranges of 5-60 microg/mL for 1, 5-50 microg/mL for II, and 10-70 microg/mL for III. The optimum assay conditions and their applicability to the determination of the cited drugs in pharmaceutical formulations are described. The method is statistically analyzed as compared with the European Pharmacopoeia (2001) method for the analysis of dimethindene maleate and reference methods for acrivastine and mequitazine drugs revealing good accuracy and precision.  相似文献   

4.
A new simple, sensitive, and selective spectrophotometric method was developed for the determination of nitrite. The method is based on the reaction of nitrite with sulfathiazole in acidic medium to form a diazonium cation, which is subsequently coupled with N-(1-naphthyl)ethylenediamine dihydrochloride to form a highly stable, violet azo dye. The reaction product has an absorption maximum at 546 nm and obeys Beer's law over a nitrite range of 0.054-0.816 microg/mL. The molar absorptivity of the colored compound is 4.61 x 10(4) L/mol x cm). The detection limit is 12.1 microg/L. The relative standard deviation is 0.85% for 5 determinations of nitrite at 0.27 microg/mL. The reproducibility and validity of the proposed method are discussed in the present paper. The simplicity of the method is demonstrated by the high stability of the azo-dye product as well as the short time required for its complete formation in a reaction at room temperature without pH control or extra extraction. The sensitivity of the method is shown by the successful determination of nitrite in human saliva and rain water, and of nitrogen dioxide in the atmosphere. The results compare favorably with those obtained by the reference method. The selectivity of the method is indicated by its freedom from most interferences, even at high concentrations of nitrate (500 microg/mL).  相似文献   

5.
Hydrazine is determined spectrophotometrically by forming the derivative 2,4-dinitrophenylhydrazine from 2,4-dinitrochlorobenzene. The formed dinitro derivative undergoes condensation reaction to form the hydrazone with p-dimethylaminobenzaldehyde (p-DAB). The resulting yellow colored product is stable in acidic medium and has a maximum absorption at 458 nm. The colour system obeys Beer's law in the range 0-7 microg of hydrazine in an overall volume of 25 mL. The molar absorptivity is calculated to be 8.1 x 10(4) L mol(-1)cm(-1) with a correlation coefficient of 0.998. The relative standard deviation is 1.7% (n=10) at 6 microg of hydrazine. Interferences due to foreign ions have been studied and the method has been applied for the determination of hydrazine in boiler feed water.  相似文献   

6.
Four different stability-indicating procedures are described for determination of tiapride in pure form, dosage form, and human plasma. Second derivative (D2), first derivative of ratio spectra (1DD), spectrofluorimetric, and high-performance column liquid chromatographic (LC) methods are proposed for determination of tiapride in presence of its acid-induced degradation products, namely 2-methoxy-5-(methylsulfonyl) benzoic acid and 2-diethylaminoethylamine. These approaches were successfully applied to quantify tiapride using the information included in the absorption, excitation, and emission spectra of the appropriate solutions. In the D2 method, Beer's law was obeyed in the concentration range of 1.5-9 microg/mL with a mean recovery of 99.94 +/- 1.38% at 253.4 nm using absolute ethanol as a solvent. In 1DD, which is based on the simultaneous use of the first derivative of ratio spectra and measurement at 245 nm in absolute ethanolic solution, Beer's law was obeyed over a concentration range of 1.5-9 microg/mL with mean recovery 99.64 +/- 1.08%. The spectrofluorimetric method is based on the determination of tiapride native fluorescence at 339 nm emission wavelength and 230 nm excitation wavelength using water-methanol (8 + 2, v/v). The calibration curve was linear over the range of 0.2-3 microg/mL with mean recovery of 99.66 +/- 1.46%. This method was also applied for determination of tiapride in human plasma. A reversed-phase LC method performed at ambient temperature was validated for determination of tiapride using methanol-deionized water-triethylamine (107 + 93 + 0.16, v/v/v) as the mobile phase. Sulpiride was used as an internal standard at a flow rate of 1 mL/min with ultraviolet detection at 214 nm. A linear relation was obtained over a concentration range of 2-30 microg/mL with mean recovery of 99.66 +/- 0.9%. Results were statistically analyzed and compared with those obtained by applying the reference method. They proved both accuracy and precision.  相似文献   

7.
The bidentate ligand diformylhydrazine (OHC-HN-NH-CHO), DFH, combines with iron(II) and iron(III) in alkaline media in the pH range 7.3-9.3 to form an intensely colored red-purple iron(III) complex with an absorption maximum at 470 nm. Beer's law is obeyed for iron concentrations from 0.25 to 13 microg mL(-1). The molar absorptivity was in the range 0.3258x10(4)-0.3351x10(4) L mol(-1) cm(-1) and Sandell's sensitivity was found to be 0.0168 microg cm(-2). The method has been applied to the determination of iron in industrial waste, ground water, and pharmaceutical samples.  相似文献   

8.
Simple, rapid, accurate, and sensitive spectrophotometric methods are described for the determination of dicyclomine hydrochloride. The methods are based on the reaction of this drug as an n-electron donor with 2,3-dichloro-5,6-dicyano-p-benzoqunione (DDQ), p-chloranilic acid (p-CA), and chloranil (CL) as pi-acceptors to give highly colored complex species. The colored products are measured spectrophotometrically at 456, 530, and 650 nm for DDQ, p-CA, and CL, respectively. Optimization of the different experimental conditions were studied. Beer's law was obeyed in concentration ranges of 20-100, 50-250, and 80-600 microg/mL for DDQ, pCA, and CL, respectively. Colored complexes are produced in organic solvents and are stable for at least 1 h. The methods were applied to Spasmorest antispasmotic tablets and ampoules with good accuracy and precision.  相似文献   

9.
A simple, selective, sensitive, and rapid spectrophotometric method has been developed for the determination of thallium(III) using 3-methyl-2-benzothiazolinone hydrazone hydrochloride and N-(1-naphthyl)-ethylenediamine dihydrochloride. The obtained product had an absorption maximum of 590 nm. Beer's law was valid over the concentration range of 0.15-8 microg/mL. The molar absorptivity and Sandell's sensitivity of the colored system were 2.93 x 10(4) L/mol x cm and 0.00723 microg/mL, respectively. The effect of different acids on the sensitivity of the method, interference by foreign substances, the optimum reaction conditions, and other analytical parameters were evaluated. The proposed method has been successfully applied in the analysis of T1(III) in standard reference materials, synthetic mixtures, and water and urine samples. The performance of the proposed method was evaluated in terms of Student's t-test and variance ratio F-test, which indicated the significance of the proposed method over reported methods.  相似文献   

10.
Three simple and sensitive spectrophotometric, difference spectroscopic, and liquid chromatographic (LC) methods are described for the determination of cefixime. The first method is based on the oxidative coupling reaction of cefixime with 3-methyl-2-benzothiazolinon hydrazone HCI in presence of ferric chloride. The absorbance of reaction product was measured at the maximum absorbance wavelength (wavelength(max)), 630 nm. The difference spectroscopic method is based on the measurement of absorbance of cefixime at the absorbance maximum, 268 nm, and minimum, 237 nm. The measured value was the amplitude of maxima and minima between 2 equimolar solutions of the analyte in different chemical forms, which exhibited different spectral characteristics. The conditions were optimized, and Beer's law was obeyed for cefixime at 1 to 16 microg/mL and 10 to 50 microg/mL, respectively. The third method, high-performance LC, was developed for the determination of cefixime using 50 mM potassium dihydrogen phosphate (pH 3.0)-methanol (78 + 22, v/v) as the mobile phase and measuring the response at wavelength(max) 286 nm. The analysis was performed on a Lichrospher RPC18 column. The calibration curve was obtained for cefixime at 5 to 250 microg/mL, and the mean recovery was 99.71 +/- 0.01%. The methods were validated according to the guidelines of the U.S. Pharmacopoeia and also assessed by applying the standard addition technique. The results obtained in the analysis of dosage forms agreed well with the contents stated on the labels.  相似文献   

11.
Simple, accurate, precise, and sensitive ultraviolet spectrophotometric and reversed-phase high-performance liquid chromatographic (RP-HPLC) methods for simultaneous estimation of escitalopram oxalate (ESC) and clonazepam (CLO) in combined tablet dosage form have been developed and validated. The spectroscopic method employs an absorbance correction method using 238.6 and 308 nm as 2 wavelengths for estimation with methanol and water as solvents. Beer's law is obeyed in the concentration range of 10.0-50.0 and 0.5-3.0 micro/mL for ESC and CLO, respectively. The RP-HPLC method uses a Jasco HPLC system with HiQ SiL C18 column (250 x 4.6 mm id) acetonitrile-0.005 M tetrabutylammonium hydrogen sulfate (55 + 45, v/v) as the mobile phase, and satranidazole as an internal standard. The detection was carried out using an ultraviolet detector set at 287 nm. For the HPLC method, Beer's law is obeyed in the concentration range of 10.0-60.0 and 0.5-3.0 microg/mL for ESC and CLO, respectively. Both methods have been successfully applied for the analysis of the drugs in a pharmaceutical formulation. Results of analysis were validated statistically and by recovery studies.  相似文献   

12.
Three sensitive spectrophotometric, spectrofluorimetric, and densitometric methods are described for the determination of indapamide. The first and second methods are based on the oxidative coupling reaction of indapamide with 3-methyl-2-benzothiazolinone hydrazone HCl (MBTH) in the presence of cerium(IV) ammonium sulfate in an acidic medium. The absorbance of the reaction product is measured at the lambdamax, 601 nm. With the same reaction, indapamide is determined by its quenching effect on the fluorescence of excess cerous ions at the emission lambdamax, 350 nm, and the excitation at lambdamax, 300 nm. The reaction conditions were optimized, and Beer's law was obeyed for indapamide at 1.2-9.6 microg/mL with mean recoveries of 99.92 +/- 0.83 and 99.97 +/- 1.11%, respectively. The third method, a stability-indicating densitometric assay, was developed for the determination of indapamide, using toluene-ethyl acetate-glacial acetic acid (69 + 30 + 1, v/v/v) as the developing system and scanning at the lambdamax, 242 nm, in the presence of the degradation product and related substance; for the indapamide concentration range of 0.6-6 microg/spot, the mean recovery was 99.73 +/- 0.71%. The proposed methods were successfully applied to the determination of indapamide in bulk powder and commercial tablets, and the results of the analysis agreed statistically with those obtained with the official method. Furthermore, the methods were validated according to the guidelines of the U.S. Pharmacopeia and also assessed by applying the standard additions technique.  相似文献   

13.
A spectrophotometric method has been developed for the determination of piperazine and its salts (citrate, phosphate, and tartrate) without prior separation, based on the interaction of piperazine or any of its salts with phenothiazine and N-bromosuccinimide in aqueous methanol. The products exhibit absorption maxima at 448, 595 and 645 nm. Measurements are made at 595 nm. Beer's law is obeyed in the concentration range 0.5-5 mug/ml for piperazine salts and 0.5-3 mug/ml for piperazine hexahydrate. The method is rapid, simple and successful for analysis of some pharmaceutical preparations.  相似文献   

14.
Simple chemometrics-assisted spectrophotometric methods are described for determination of 2 antibacterial binary mixtures. The mixtures are composed of norfloxacin in combination with tinidazole and erythromycin (as ethylsuccinate ester or stearate salt) in combination with trimethoprim. The normal UV absorption spectra of each pair of drugs in the studied mixtures, in the range of 200-400 nm, showed a considerable degree of spectral overlapping: 77.5% for the norfloxacin-tinidazole mixture and 84.3% for the erythromycin-trimethoprim mixture. Resolution of the norfloxacin-tinidazole mixture and trimethoprim in the presence of erythromycin was accomplished successfully by using zero-crossing first derivative (1D), classical least-squares (CLS) regression analysis, and principal component regression (PCR) analysis methods. In addition, an alternative simple and accurate colorimetric method was developed for the determination of erythromycin in the presence of trimethoprim using 2,4-dinitrophenylhydrazine. All variables affecting the development of the colored chromogen were studied and optimized, and the product was measured at 526-529 and 538-542 nm for erythromycin stearate and erythromycin ethylsuccinate, respectively. For zero-crossing, first derivative technique Beer's law was obeyed in the general concentration range of 2-50 microg/mL for norfloxacin, tinidazole, and trimethoprim with good correlation coefficients (0.9994-0.9996). Overall limits of detection (LOD) and quantification (LOQ) ranged from 0.59 to 2.81 and 1.96 to 9.33 microg/mL, respectively. The obtained results from CLS and PCR were compared with those obtained from a 1D spectrophotometric method. With the exception of erythromycin, overall recoveries in the average range of 97.33-103.0% were obtained with a considerable degree of accuracy when the suggested methods were applied to analysis of synthetic binary mixtures, some commercial dosage forms such as tablets and oral suspension without interference from the commonly encountered excipients and additives. For the colorimetric method, Beer's law was obeyed in the general concentration range of 7.21-28.84 microg/mL erythromycin with good correlation coefficients (0.9980-0.9996). Overall LOD and LOQ ranged from 0.73 to 1.65 and 2.43-5.49 microg/mL, respectively. Erythromycin derivatives were determined in the commercial dosage form, without interference from trimethoprim-encountered excipients and additives. The obtained results, with both chemometric and colorimetric methods, have been compared with those obtained from reported methods, and proper F- and t-values were observed, indicating no significant difference between the results of the suggested methods and reported method(s). The good percentage recoveries and proper statistical data obtained proved the efficiency of the proposed procedures for the determination of the studied drugs in their binary mixtures as well as in the commercial dosage forms with quite satisfactory precision.  相似文献   

15.
Three simple and sensitive spectrophotometric methods were developed and validated for determination of the hydrochloride salts of fluoxetine, sertraline, and paroxetine in their pharmaceutical dosage forms. These methods were based on the reaction of the N-alkylvinylamine formed from the interaction of the free secondary amino group in the investigated drugs and acetaldehyde with each of 3 haloquinones, i.e., chloranil, bromanil, and 2,3-dichloronaphthoquinone, to give colored vinylamino-substituted quinones. The colored products obtained with chloranil, bromanil, and 2,3-dichloronaphthoquinone exhibit absorption maxima at 665, 655, and 580 nm, respectively. The factors affecting the reactions were studied and optimized. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.9986-0.9999) were found between the absorbances and the concentrations of the investigated drugs in the range of 4-120 microg/mL. The limits of detection for the assays ranged from 1.19 to 2.98 microg/mL. The precision values of the methods were satisfactory; the relative standard deviations were 0.56-1.24%. The proposed methods were successfully applied to the determination of the 3 drugs in pure and pharmaceutical dosage forms with good accuracy; the recoveries ranged from 99.1 to 101.3% with standard deviations of 1.15-1.92%. The results compared favorably with those of reported methods.  相似文献   

16.
偶氮氯膦—DBC光度法测定银合金中镨   总被引:2,自引:0,他引:2  
研究提出镨 ( ) - DBC-偶氮氯膦 -磷酸 - EDTA新体系光度法测定贵金属合金中微量镨。反应体系生成 α型蓝色配合物的 λmax=650 nm,灵敏度高 ,摩尔吸光系数 ε=0 .93× 1 0 5L·mol-1·cm-1,镨浓度在 0~ 50 μg/2 5ml范围内符合比耳定律 ,方法选择性强 ,有较好的适用性 ,用于分析银合金中镨 ,标准偏差 S≤ 0 .0 1 1 ,相对标准偏差 RSD≤ 1 .97%。  相似文献   

17.
研究了吐温20(Tween20)存在下,铝与二甲酚橙(XO)的显色反应,建立了分光光度法测定微量铝的新方法.结果表明,在pH=3.13的乙酸-乙酸钠缓冲介质中,铝与XO及吐温20反应生成有色络合物,络合物的最大吸收波长位于511 nm处, 表观摩尔吸光系数ε为1.99×10~4 L·moL~(-1)·cm~(-1),在10 mL溶液中,铝量在2.2~15.1 μg范围内符合比耳定律,检出限为0.0018 μg/mL.方法应用于茶叶、沙棘叶中铝的测定,样品加标回收率为96%~102.6%.  相似文献   

18.
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   

19.
Three simple, accurate and sensitive spectrophotometric methods are developed for the determination of some new drugs for the treatment of osteoporosis: risedronate sodium (I), alendronate sodium (II) and etidronate disodium (III). The first method is based on the measurement of difference in absorbance (Delta A) of risedronate sodium in 0.01 mol l(-1) hydrochloric and 0.1 mol l(-1) sodium hydroxide at 262 nm. Beer's law is obeyed over a concentration range of 15-150 microg ml(-1) with mean recovery 99.75+/-1.22 and molar absorptivity (epsilon) 1.891 x 10(3). The second method is based on the reaction of the primary amino group of (II) with ninhydrin reagent in methanolic medium in the presence of 0.05 mol l(-1) sodium bicarbonate. The colored product is measured at 568 nm, and the linearity range is found to be 3.75-45 microg ml(-1) with mean recovery 99.77+/-0.73 and epsilon 9.425 x 10(3). The third method is based on oxidation of the three mentioned drugs with ceric (IV) sulphate in 0.5 mol l(-1) sulphuric acid at room temperature and subsequent measurement of the excess unreacted cerium (IV) sulphate at 320 nm. The method obeyed Beer's law over a concentration range of 2-24 microg ml(-1) for the three drugs with mean recovery 99.79+/-1.16, 99.73+/-1.38 and 99.86+/-1.13 and epsilon 14.427 x 10(3), 13.813 x 10(3) and 14.000 x 10(3) for drugs I, II, III respectively. The proposed methods were successfully applied for the determination of the studied drugs in bulk powder and in pharmaceutical formulations. The results were found to agree statistically with those obtained the reported methods. Furthermore, the methods were validated according to USP regulations and also assessed by applying the standard addition technique.  相似文献   

20.
A simple, rapid, and sensitive spectrophotometric method has been developed for the determination of selenium in real samples of water, soil, plant materials, human hair, and synthetic cosmetic and in pharmaceutical preparations. The method is based on the reaction of selenium with potassium iodide in an acidic medium to liberate iodine. The liberated iodine bleaches the violet color of thionin, and which is measured at 600 nm. This decrease in absorbance is directly proportional to selenium concentration and obeys Beer's law in the range 1-5 micro g selenium in a final volume of 10 mL (0.1-0.5 microg mL(-1)). The molar absorptivity and Sandell's sensitivity of the method were found to be 7.33 x 10(4) L mol(-1) cm(-1) and 0.0011 microg cm(-2), respectively. The optimum reaction conditions and other analytical conditions were evaluated. The effect of interfering ions on the determination is described.  相似文献   

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