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1.
Thin-layer chromatography, first derivative, ratio spectra derivative spectrophotometry and Vierordt's method have been developed for the simultaneous determination of paracetamol and drotaverine HCl. TLC densitometric method depends on the difference in Rf values using ethyl acetate:methanol:ammonia (100:1:5 v/v/v) as a mobile phase. The spots of the two drugs were scanned at 249 and 308 nm over concentration ranges of 60-1200 microg/ml and 20-400 microg/ml with mean percentage recovery 100.11%+/-1.91 and 100.15%+/-1.87, respectively. The first derivative spectrophotometric method deals with the measurements at zero-crossing points 259 and 325 nm with mean percentage recovery 99.25%+/-1.08 and 99.45%+/-1.14, respectively. The ratio spectra first derivative technique was used at 246 and 305 nm with mean percentage recovery 99.75%+/-1.93 and 99.08%+/-1.22, respectively. Beer's law for first derivative and ratio spectra derivative methods was obeyed in the concentration range 0.8-12.8 and 0.4-6.4 microg/ml of paracetamol and drotaverine HCl, respectively. Vierordt's method was applied to over come the overlapping of paracetamol and drotaverine HCl in zero-order spectra in concentration range 2-26 and 2-40 microg/ml respectively. The suggested methods were successfully applied for the analysis of the two drugs in laboratory prepared mixtures and their pharmaceutical formulation. The validity of the methods was assessed by applying the standard addition technique. The obtained results were statistically agreed with those obtained by the reported method.  相似文献   

2.
A new RP-LC method and two new spectrophotometric methods, principal component regression (PCR) and first derivative spectrophotometry, are proposed for simultaneous determination of diflucortolone valerate (DIF) and isoconazole nitrate (ISO) in cream formulations. An isocratic system consisting of an ACE C18 column and a mobile phase composed of methanol-water (95 + 5, v/v) was used for the optimal chromatographic separation. In PCR, the concentration data matrix was prepared by using synthetic mixtures containing these drugs in methanol-water (3 + 1, v/v). The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbances at 29 wavelengths in the range of 242-298 nm for DIF and ISO in the zero-order spectra of their combinations. In first derivative spectrophotometry, dA/dlambda values were measured at 247.8 nm for DIF and at 240.2 nm for ISO in first derivative spectra of the solution of DIF and ISO in methanol-water (3 + 1, v/v). The linear ranges were 4.00-48.0 microg/mL for DIF and 50.0-400 microg/mL for ISO in the LC method, and 2.40-40.0 microg/mL for DIF and 60.0-260 microg/mL for ISO in the PCR and first derivative spectrophotometric methods. These methods were validated by analyzing synthetic mixtures. These three methods were successfully applied to two pharmaceutical cream preparations.  相似文献   

3.
Derivative spectrophotometry has been applied for the elimination of the mutual spectral interferences and the analysis of binary, ternary and quaternary mixtures of complexes of microgram amounts of divalent ions of cobalt, copper, lead, manganese, nickel, zinc and iron with 4-(pyridyl-2-azo)resorcinol (PAR) in the range of 0.05-1 microg/ml (0.2-4 microg/ml for lead). The first derivative spectra can be used for the determination of both components in the majority of binary mixtures except of Cu(II) and Co(II) and systems containing Fe(II). The second and the third derivative spectra allow to determine one constituent in some ternary and quaternary mixtures.  相似文献   

4.
Ferreira SL  Costa AC  de Jesus DS 《Talanta》1996,43(10):1649-1656
A major problem with spectrophotometric methods for nickel is cobalt interference, because many of the reagents for nickel also react with cobalt. In this work, the interference of cobalt in the determination of nickel using 2-(5-bromo-2-pyridylaxo)-5-diethylaminophenol (Br-PADAP) was eliminated by the use of derivative spectrophotometry, using the zero-crossing method for evaluation of the derivative signal. Br-PADAP reacts with nickel(II) in the presence of Triton X-100 to form a red complex with absorption maxima at 530 and 562 nm. The reactions parameters and the conditions for the measurements of the first-derivative signal were studied and the results demonstrated that using the derivative technique, Br-PADAP can be used for nickel determination with a selectivity higher than that of ordinary spectrophotometry and with a limit of detection of 0.2 ng ml(-1). The pH should be in the range 5.0-6.0 using an acetate buffer. The determination of nickel in the presence of cobalt was performed with conventional and derivative procedures, and the results demonstrated that only the derivative method should be used and, of the methods used for evaluation of the derivative signal, the zero-crossing method is the best. The proposed procedure was used for nickel determination in steels standards. The results demonstrated that the procedure has satisfactory accuracy and precision. Cobalt interference can be also eliminated by using dual-wave-length spectroscopy.  相似文献   

5.
在碱性介质中,铁(Ⅱ)和钴(Ⅱ)可与硫代巴比妥酸-NO2-体系反应分别形成一种稳定的兰色和黄色配合物,铁(Ⅱ)配合物在656nm和386nm具有吸收峰,钴(Ⅱ)配合物只有一个吸收峰位于423nm,体系的吸光度A6Fe56、A4F2e3、AC42o3与铁、钴含量在一定的范围内呈良好的线性关系,且铁(Ⅱ)、钴(Ⅱ)配合物在423nm波长处的吸光度具有良好的加和性,建立了一种同时测定微量铁和钴的新的分光光度法。方法的线性范围分别为铁0~50μg/(25mL)、钴0~25μg/(25mL)。将该法应用于水样中微量铁和钴的同时测定,其结果分别与原子吸收光谱法和紫尿酸光度法相吻合,加标回收率分别为98%~102%和94%~106%,相对标准偏差(RSD)分别为1.0%~1.8%和3.1%~4.7%(n=5)。  相似文献   

6.
Wei J  Naixing W  Quanjie M  Zhikun S  Xiuqin X  Fuxiang L 《The Analyst》2001,126(8):1440-1443
Ciprofloxacin (CPFX) is proposed as a reagent for the derivative spectrophotometric determination of praseodymium in mixed rare earths. The absorption spectra of 4f electron transitions of the praseodymium complex with CPFX was studied by normal and derivative spectrophotometry. The stoichiometry of the praseodymium-CPFX complex was calculated by the molar ratio and continuous variations methods. A ratio of Pr to CPFX of 1:3 was found. The absorption bands of the 4f electron transitions of the complex were enhanced markedly. Using the third derivative spectrum. Beer's law was obeyed up to 35 microg cm(-3) of praseodymium. The relative standard deviation is 0.62% for 14 microg cm(-3) of praseodymium. The detection and quantification limits were 0.17 and 0.56 microg cm(-3) of praseodymium, respectively. A method for the direct determination of praseodymium in mixtures of rare earths with good accuracy and selectivity is described.  相似文献   

7.
Three accurate, rapid and simple atomic absorption spectrometric (AAS), conductometric and colorimetric methods were developed for the determination of gatifloxacin (GTF), moxifloxacin (MXF) and sparfloxacin (SPF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at lambda(max) 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone. The optimizations of various experimental conditions were described. Optimum concentration ranges for the determination of GTF, MXF and SPF were 5.0-150, 40-440 microg mL(-1) and 0.10-1.5 mg mL(-1) using atomic absorption (AAS), conductometric and colorimetric methods, respectively. Detection and quantification limits are ranges from 1.5 to 2.3 microg mL(-1) using AAS method or 30-45 microg mL(-1) using colorimetric method. The proposed procedures have been applied successfully to the analysis of these drugs in pharmaceutical formulations and the results are favourably comparable to the reference methods.  相似文献   

8.
A highly selective, convenient, and precise method, first-order derivative spectrophotometry, was applied for the determination of astaxanthin in Haematococcus pluvialis. Ethyl acetate and ethanol (1:1, v/v) were found to be the best extraction solvent tested due to their high efficiency and low toxicity compared with nine other organic solvents. Astaxanthin coexisting with chlorophyll and beta-carotene was analyzed by first-order derivative spectrophotometry in order to optimize the conditions for the determination of astaxanthin. The results show that when detected at 432 nm, the interfering substances could be eliminated. The dynamic linear range was 2.0-8.0 microg/mL, with a correlation coefficient of 0.9916. The detection threshold was 0.41 microg/mL. The RSD for the determination of astaxanthin was in the range of 0.01-0.06%; the results of recovery test were 98.1-108.0%. The statistical analysis between first-order derivative spectrophotometry and HPLC by T-testing did not exceed their critical values, revealing no significant differences between these two methods. It was proved that first-order derivative spectrophotometry is a rapid and convenient method for the determination of astaxanthin in H. pluvialis that can eliminate the negative effect resulting from the coexistence of astaxanthin with chlorophyll and beta-carotene.  相似文献   

9.
Three spectrophotometric methods including Vierordt's method, derivative, ratio spectra derivative, and thin layer chromatography (TLC)-UV densitometric method were developed for simultaneous determination of drotaverine HCl (DRT) and nifuroxazide (NIF) in presence of its impurity, 4-hydroxybenzohydrazide (4-HBH). In Vierordt's method, (E(1 cm)(1%)) values were calculated at 227 and 368 nm in the zero-order spectra of DRT and NIF. By derivative spectrophotometry, the zero-crossing method, drotaverine HCl was determined using the second derivative at 245 nm and the third derivative at 238 nm, while nifuroxazide was determined using the first derivative at 399 nm and the second derivative at 411 nm. The ratio spectra derivative spectrophotometry is basedon the measure of the amplitude at 459 nm for DRT and at 416 nm for NIF in the first derivative of the ratio spectra. Calibration graphs of the three spectrophotometric methods were plotted in the range 1-10 mug/ml of DRT and 2-20 mug/ml of NIF. TLC-UV densitometric method was achieved on silica gel plates using ethyl acetate : methanol : ammonia 33% (10 : 1 : 0.1 v/v/v) as the mobile phase. The Rf values were 0.74, 0.50, 0.30+/-0.01 for DRT, NIF and 4-HBH, respectively. On the fluorescent plates, the spots were located by fluorescence quenching and the densitometrical area were measured at 308 and 287 nm with linear range 0.2-4 mug/spot and 0.6-12 mug/spot for DRT and NIF, respectively. The proposed methods have been successfully applied to the commercial pharmaceutical formulation without any interference of excipients. Mean recoveries, relative standard deviations and the results of the proposed methods were compared with those obtained by applying the alternate methods.  相似文献   

10.
Four methods were developed for the determination of intact disopyramide phosphate in the presence of its degradation product. In the first and second methods, third-derivative spectrophotometry and first derivative of the ratio spectra were used. For the third-derivative spectrophotometric method, the peak amplitude was measured at 272 nm, while for the derivative ratio spectrophotometric method, disopyramide phosphate was determined by measuring the peak amplitude at 248 and 273 nm. Both methods were used for the determination of disopyramide phosphate in the concentration range 12.5-87.5 microg/mL, with corresponding mean recovery 100.8 +/- 0.7% for the first method and 99.9 +/- 0.7% and 99.6 +/- 0.7% for the second method at 248 and 273 nm, respectively. In the third method, an ion selective electrode (ISE) was fabricated using phosphotungstic acid as an anionic exchanger, PVC as the polymer matrix, and dibutylsebacate as a plasticizer. The ISE was used for the determination of disopyramide phosphate in pure powder form in the concentration range 10(-2)-10(-5) M. The slope was found to be 58.5 (mV/decade), and the average recovery was 99.9 +/- 1.6%. The fourth method depended on the quantitative densitometric determination of the drug in concentration range of 0.25-2.5 microg/spot using silica gel 60 F245 plates and ethyl acetate-chloroform-ammonium hydroxide (85 + 10 + 5, v/v/v) as the mobile phase, with corresponding mean accuracy of 100.3 +/- 1.1%. The 4 proposed methods were found to be specific for disopyramide phosphate in presence of up to 80% of its degradation product for the spectrophotometric methods, 90% of its degradation for the densitometric method, and 40% for the ISE method. The 4 proposed procedures were successfully applied for the determination of disopyramide phosphate in Norpace capsules. Statistical comparison between the results obtained by these methods and the official method of the drug was done, and no significant differences were found.  相似文献   

11.
The partial least squares regression method (PLS) was tested as a calibration procedure for the simultaneous determination of phenol, o-nitrophenol, m-nitrophenol and p-nitrophenol by both conventional and first derivative UV/Vis spectrophotometry. The experiments were conducted in the acidic, neutral and basic media. The results obtained by the application of the PLS procedure on the conventional and first derivative spectra in two solvent media were compared. It was found that the results obtained in the basic medium have better performance characteristics than those obtained in the acidic or neutral media. Comparable results were obtained in the case of both conventional and first derivative absorbance data. The proposed method was applied to the determination of the four phenol derivatives in natural spiked water samples at concentration levels between 1.0 and 10.0 microg ml(-1) with average recoveries in the range 96% - 99%.  相似文献   

12.
Murti MV  Khopkar SM 《Talanta》1976,23(3):246-248
Thiobenzoylacetone in benzene is used for the extraction and spectrophotometric determination of cobalt at pH 8.4-9.1. The orange-yellow complex is measured at 460 nm. The system conforms to Beer's law over the range 0.20-4.58 microg ml of extract. The colour of the complex is stable for at least 144 hr. Cobalt(II) is quantitatively extracted and determined in the presence of 200:1 (w w ratios) of various ions. The method is made selective by using common sequestering agents such as thiourea or fluoride or by selective extraction with mesityl oxide, tributylphosphate and acetylacetone. It is possible to determine cobalt in the presence of nickel by simultaneous spectrophotometry. The method is rapid, simple, selective and sensitive.  相似文献   

13.
Four new methods were developed and validated for the determination of cinnarizine HCl in its binary mixture with piracetam in pure and pharmaceutical preparations. The first one was a densitometric analysis that provides a simple and rapid method for the separation and quantification of cinnarizine HCI. The method depends on the quantitative densitometric evaluation of thin-layer chromatograms of cinnarizine HCI at 252 nm over concentration range of 1-6 microg/spot, with a mean accuracy of 100.05 +/- 0.91%. The second method was determination of the drug using a colorimetric method that utilizes the reaction of 3-methyl-benzothiazolin-2-one in the presence of FeCl3 as an oxidant. The green color of the resulting product was measured at 630 nm over concentration range 10-40 microg/mL, with a mean accuracy of 100.10 +/- 1.13%. The third method was a direct spectrophotometric determination of cinnarizine HCI at 252 nm over the concentration range 7-20 microg/mL, while piracetam was determined by derivative ratio spectrophotometry at 221.6 nm over concentration range 5-30 microg/mL, with a mean accuracy of 100.14 +/- 0.79 and 100.26 +/- 1.24% for cinnarizine HCI and piracetam, respectively. The last method was a liquid chromatography analysis of both cinnarizine HCI and piracetam, depending on quantitative evaluation of chromatograms of cinnarizine HCI and piracetam at 252 and 212 nm, respectively, over the concentration range 10-200 microg/mL for cinnarizine HCI and 20-500 microg/mL for piracetam, with a mean accuracy of 100.03 +/- 0.89 and 100.40 +/- 0.94% for cinnarizine HCI and piracetam, respectively. The proposed procedures were checked using laboratory-prepared mixtures and successfully applied for the analysis of their pharmaceutical preparations. The validity of the proposed procedures was further assessed by applying the standard addition technique. Recoveries were quantitative, and the results obtained agreed with those obtained by other reported methods.  相似文献   

14.
Two stability-indicating methods, namely densitometric TLC and derivative spectrophotometry for the determination of the fluoroquinolone antibacterials lomefloxacin (Lfx), moxifloxacin (Mfx), and sparfloxacin (Sfx) in the presence of their acid degrades are described. Acid degradation was adopted and the main decarboxylated product separated by TLC. Degradation products were identified confirming a previously mentioned degradation scheme. The densitometric method is based on the separation of the intact drug from its acid degradation product on silica gel G plates using different mobile phases and the spots of the intact drugs were scanned at 288, 290, and 292 nm for Lfx, Mfx, and Sfx, respectively. The derivative spectrophotometric method utilizes first derivative D(1) UV spectrophotometry with zero crossing points at 295.2 nm for Lfx, 280.4 and 303.4 nm for Mfx, and 280.8 nm for Sfx. Regression analysis of Beer's plots showed good correlation in the concentration ranges 0.2-1.2, 0.1-1.4, and 0.5-2.0 microg/spot for Lfx, Mfx, and Sfx, respectively, in the densitometric method and 2-16 microg/ml for all drugs in the derivative spectrophotometric method. The proposed methods were successfully applied for the determination of the investigated drugs in bulk powder with mean percentage accuracy ranges from 98.93 to 101.25% for the TLC method and from 98.18 to 100.35% for the D(1) method. The proposed methods were also applied for the determination of the investigated drugs in their pharmaceutical dosage forms and their validity was assessed using the standard addition technique with mean percentage recovery ranging from 100.25 to 101.70% in the TLC method and from 99.27 to 102.12% in the D(1) method. The selectivity of the proposed methods was tested by the analysis of laboratory-prepared mixtures containing different percentages of the studied drugs and their acid degrades. The proposed methods were found selective for the determination of the intact drugs in the presence of up to 90% of their degrades in the TLC method and 70% for Lfx and 90% for Mfx and Sfx in the D(1) method.  相似文献   

15.
Two methods for determining Tartrazine and Sunset Yellow in mixtures by first derivative spectrophotometry and by first derivative of the ratio spectra are described. The procedures do not require any separation step. By the first method, the measurements are obtained in the zero-crossing wavelengths and the calibration graphs are linear up to 20 microg/ml of Tartrazine and up to 40 microg/ml of Sunset Yellow. The determinations of Tartrazine and Sunset Yellow are also done by the first derivative of the ratio spectra. The methods are applied for determining both compounds in four commercial food products.  相似文献   

16.
Three new, different, simple, sensitive, and accurate methods were developed for quantitative determination of nifuroxazide (I) and drotaverine hydrochloride (II) in a binary mixture. The first method was spectrophotometry, which allowed determination of I in the presence of II using a zero-order spectrum with an analytically useful maximum at 364.5 nm that obeyed Beer's law over a concentration range of 2-10 microg/mL with mean percentage recovery of 100.08 +/- 0.61. Determination of II in presence of I was obtained by second derivative spectrophotometry at 243.6 nm, which obeyed Beer's law over a concentration range of 2-10 microg/mL with mean recovery of 99.82 +/- 1.46%. The second method was spectrodensitometry, with which both drugs were separated on a silica gel plate using chloroform-acetone-methanol-glacial acetic acid (6 + 3 + 0.9 + 0.1) as the mobile phase and ultraviolet (UV) detection at 365 nm over a concentration range of 0.2-1 microg/band for both drugs, with mean recoveries of 99.99 +/- 0.15 and 100.00 +/- 0.34% for I and II, respectively. The third method was reversed-phase liquid chromatography using acetonitrile-water (40 + 60, v/v; adjusted to pH 2.55 with orthophosphoric acid) as the mobile phase and pentoxifylline as the internal standard at a flow rate of 1 mU/min with UV detection at 285 nm at ambient temperature over a concentration range of 2-10 microg/mL for both drugs, with mean recoveries of 100.24 +/- 1.51 and 100.08 +/- 0.78% for I and II, respectively. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulations containing the above drugs with no interference from other dosage form additives. The validity of the suggested procedures was further assessed by applying the standard addition technique which was found to be satisfactory, and the percentage recoveries obtained were in accordance with those given by the EVA Pharma reference spectrophotometric method.  相似文献   

17.
A new combined method including fiber optic-linear array detection spectrophotometry (FO-LADS) and cloud point extraction (CPE) was developed using a cylindrical micro cell for simultaneous preconcentration and determination of different species. The CPE and FO-LADS methods have good matching conditions for combination because FO-LADS is suitable as a detection technique for the low volume of remained phase obtained after CPE. This combination was carried out using 50 μL cylindrical micro cell and then employed for simultaneous preconcentration and determination of cobalt and nickel.Cloud point extraction method was based on the chromogenic reaction of metal ions and 1-(2-pyridylazo)-2-naphthol (PAN) and then preconcentration of formed complexes using octylphenoxypolyethoxyethanol (Triton X-114). The remained phase after CPE was transferred into cylindrical micro cell and located at the cell holder of FO-LADS. The spectra of cobalt and nickel complexes were collected by FO-LADS and processed for ordinary and first derivative spectrophotometry.Optimization of different parameters was evaluated. Under optimum conditions, calibration curves were linear in the range of 0.6-30.0 and 0.1-15.0 μg L−1 with detection limits of 0.2 and 0.04 μg L−1 for Co and Ni respectively. The relative standard deviations (R.S.D.s) were lower than 4%. The obtained enhancement factors were 198 and 199 for cobalt and nickel, respectively.The proposed method was compared with the other methods and applied to the analysis of several real and spiked samples.  相似文献   

18.
快速测定蜂王浆中蜂王酸的分光光度法研究   总被引:5,自引:0,他引:5  
栗风珍  唐波 《分析化学》1995,23(1):56-59
本文提出了用差示分光光度法和一阶导数分光光度法测定蜂王浆中蜂王酸的含量,差示光谱最大测定波长为(+)228.0nm;一阶导数光谱测定波长为(+)204.5nm和(-)233.5nm。线性范围为0-20μg/ml(差示分光光度法)和0-15μg/ml(一阶异数分光光度法)。二法在实际测定中具有操作简便,快速和准确度高等优点。  相似文献   

19.
ABSTRACT: Three simple and rapid spectrophotometric methods were developed for detection and trace determination of benzophenone (the main impurity) in phenytoin bulk powder and pharmaceutical formulations. The first method, zero-crossing first derivative spectrophotometry, depends on measuring the first derivative trough values at 257.6 nm for benzophenone. The second method, zero-crossing third derivative spectrophotometry, depends on measuring the third derivative peak values at 263.2 nm. The third method, ratio first derivative spectrophotometry, depends on measuring the peak amplitudes of the first derivative of the ratio spectra (the spectra of benzophenone divided by the spectrum of 5.0 μg/mL phenytoin solution) at 272 nm. The calibration graphs were linear over the range of 1-10 μg/mL. The detection limits of the first and the third derivative methods were found to be 0.04 μg/mL and 0.11 μg/mL and the quantitation limits were 0.13 μg/mL and 0.34 μg/mL, respectively, while for the ratio derivative method, the detection limit was 0.06 μg/mL and the quantitation limit was 0.18 μg/mL. The proposed methods were applied successfully to the assay of the studied drug in phenytoin bulk powder and certain pharmaceutical preparations. The results were statistically compared to those obtained using a polarographic method and were found to be in good agreement.  相似文献   

20.
A simple and fast method was developed for the simultaneous determination of dapsone and pyrimethamine by first-order digital derivative spectrophotometry. Acetonitrile was used as a solvent to extract the drugs from the pharmaceutical formulations, and the samples were subsequently evaluated directly by digital derivative spectrophotometry. The simultaneous determination of both drugs was performed by the zero-crossing method at 249.4 and 231.4 nm for dapsone and pyrimethamine, respectively. The best signal-to-noise ratio was obtained when the first derivative of the spectrum was used. The linear range of determination for the drugs was from 6.6 x 10(-7) to 2.0 x 10(-4) and from 2.5 x 10(-6) to 2.0 x 10(-4) mol/L for dapsone and pyrimethamine, respectively. The excipients of commercial pharmaceutical formulations did not interfere in the analysis. Chemical and spectral variables were optimized for determination of both analytes. A good level of repeatability, 0.6 and 1.7% for dapsone and pyrimethamine, respectively, was observed. The proposed method was applied for the simultaneous determination of both drugs in pharmaceutical formulations.  相似文献   

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