Reserpine In Tablets Research Articles

Epoxide-derived mixed-mode chromatographic stationary phases for separation of active substances in fixed-dose combination drugs.

A method for the preparation of novel mixed-mode reversed-phase/strong cation exchange stationary phase for the separation of fixed-dose combination drugs has been developed. An epoxysilane bonded silica prepared by vapor phase deposition was used as a starting material to produce diol, octadecyl, sulfonate, and mixed octadecyl/sulfonate groups bonded silica phases. The chemical structure and surface coverage of the functional groups on these synthesized phases were confirmed by fourier-transform infrared and solid-state 13 C NMR spectroscopy and elemental analysis. Alkylbenzene homologs, basic drugs, nucleobases and alkylaniline homologs were used as probes to demonstrate the reversed-phase, ion exchange, hydrophilic interaction and mixed-mode retention behaviors of these stationary phases. The octadecyl/sulfonate bonded silica exhibits pronounced mixed-mode retention behavior and superior retentivity and selectivity for alkylaniline homologs. The mixed-mode retention is affected by either ionic or solvent strength in the mobile phase, permiting optimization of a separation by fine tuning these parameters. The mixed-mode stationary phase was applied to separate two fixed-dose combination drugs: compound reserpine tablets and compound methoxyphenamine capsules. The results show that simultaneous separation of multiple substances in the compound dosage can be achieved on the mixed-mode phase, which makes multi-cycles of analysis for multiple components obsolete.

FIRST-ORDER ULTRAVIOLET DERIVATIVE SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF RESERPINE IN ANTIHYPERTENSION TABLET

A new ultraviolet derivative spectrophotometry (UVDS) method has been developed for determination of reserpine in antihypertension tablets. A first-order UVDS based on the measurement of the distance between peaks to baseline (DZ) at the wavelength of 312 nm was used. Evaluation of analytical performance showed that accuracy as percentage recovery was 99.18-101.13%, precision expressed as relative standard deviation (RSD) was 1.91% and linear correlation was also obtained 0.9998 in the range of 10-50 µg/mL. Estimation of limit of detection and limit of quantitation was 0.8868 µg/mL and 2.6874 µg/mL, respectively. As a reference method, HPLC methods from United States Pharmacopiea (USP) were used. Commercially tablets available were analyzed by the two methods. The content of reserpine in tablets was found 0.2260±0.0033 mg by UVDS and 0.2301±0.0051 mg by the USP methods. The result obtained from the two methods was compared statistically using F-test and t-test and showed no significant differences between the variance and mean values of the two methods at 95% confidence level. This method was faster, easier, low cost and gave result as well as the reference method published by USP.

Resolution of Overlapped Capillary Electrophoresis Peaks by Using Heuristic Evolving Latent Projections to Quantify Chloroquine Phosphate and Promethazine Hydrochloride

AbstractChloroquine phosphate and promethazine hydrochloride are two main components in compound reserpine tablets. It is difficult to separate the two compounds with capillary electrophoresis (CE). Heuristic evolving latent projections (HELP) is a chemometric algorithm which is suitable for resolving overlapped peaks from CE and HPLC. In this paper, HELP was applied to resolving the completely overlapped peaks of chloroquine phosphate and promethazine hydrochloride from CE. Mathematical separation and satisfactory quantification results can be achieved easily without too much time involved in the procedure.

Improved Colorimetric Determination of Reserpine in Tablets Using 4-Caboxyl-2,6-dintrobenzene diazonium ion (CDNBD)

Purpose: To develop a simple, rapid and improved colorimetric method for the assay of reserpine in tablets Method: The method is based on the aromatic ring coupling of reserpine with 4-carboxyl-2,6-dinitrobenzene diazonium ion with the consequent formation of an azo adduct. Optimization of reaction conditions and validation were carried out and the method applied to assay of reserpine in tablets. Result: Reserpine coupled readily with CDNBD and optimization of experimental conditions showed the reaction to be completed in 10 min at room temperature. A 1:1 drug to reagent stoichiometric ratio was obtained for the azo adduct formed. The adduct exhibited a bathochromic shift with respect to the drug and pronounced hyperchromic shift with respect to the reagent. Sample analyses were done using a colorimeter at 470 nm. The assays were linear and reproducible over the concentration range of 2.25 -24 µg/mL. The new method was successfully applied in the assay of reserpine in tablets with a performance similar to the official (USP) spectrophotometric method (p > 0.05). This method represents a profound improvement on the previously reported colorimetric method for reserpine. Conclusion: The method developed is rapid and could find application in in-process quality control of reserpine. Keywords: Reserpine, colorimetry, 4-Caboxyl-2,6-dintrobenzene diazonium ion (CDNBD), diazo coupling > Tropical Journal of Pharmaceutical Research Vol. 6 (2) 2007: pp. 695-703

Resolution of overlapping capillary electrophoresis peaks by using chemometric analysis: Quantification of the components in compound reserpine tablets

The application of multivariate curve resolution with alternating least squares (MCR-ALS) methods to second-order data from capillary electrophoresis with diode array detector (CE-DAD) is reported. Initial qualitative solutions obtained by evolving factor analysis (EFA) and pure-variable detection method can be further optimized by a simultaneous analysis of multiple electrophoresis run data with ALS regression. While unknown samples are analyzed simultaneously against the corresponding standards in different composition ratios, the exact amounts of common components in different CE runs can be determined by the traditional calibration curve method, and quantification can thus be achieved. The above methods are applied to the determination of the components in compound reserpine tablets in overlapping peaks from CE. The quantification results are compared with those of the first derivative of the electropherogram method and artificial neural network (ANN) method.

IMPORTANCE OF THE OXIDATION REACTION OF SODIUM METAPERIODATE FOR SPECTROPHOTOMETRIC ASSAY OF RESERPINE

A new simple, accurate and reasonably sensitive spectrophotometric method is described for the determination of reserpine based on the oxidation with sodium metaperiodate in the presence of acetic acid and coupling with 3-methyl-2-benzo thiazolinone hydazone hydrochloride (MBTH) to form highly blue coloured product showing maximum absorbance at 630 nm. Beer's law is obeyed in the range 0.2–1.6 µg ml−1. The relative standard deviation was found to be less than 1%. The proposed method can be applied for the estimation of reserpine in tablets with no evidence of interference from excipients.

Spectrophotometric determination of Rauwolfia alkaloids: estimation of reserpine in pharmaceuticals.

A simple, sensitive and economically viable spectrophotometric method for the determination of some Rauwolfia alkaloids (ajmaline, ajmalicine, reserpine and yohimbine-HCl) has been developed. The method involves the oxidation of Rauwolfia alkaloids by iron(III) and subsequent complexation of iron(II) with 1,10-phenanthroline, forming a red-colored complex having the maximum absorbance at 510 nm. The method is applied to the determination of reserpine in tablets of pharmaceutical formulations. The common excipients do not interfere with the proposed method. A statistical comparison of these results with those of a reported method shows good agreement and indicates no significant difference in the precision.

Flow injection spectrofluorimetric determination of reserpine in tablets by on-line acetone sensitized photochemical reaction

On-line photochemical reaction of reserpine in the presence of acetone was investigated. Acetone was found to speed up the on-line photochemical conversion of reserpine into an intensively fluorescent compound. Not only reaction acidity but also the acetate buffer concentration affected the on-line photochemical induced fluorescence signal. Based on the observation an automated flow injection photochemical fluorimetric approach was developed. An injected sample zone was carried by a water stream to be merged with a acetate buffer (pH 3.4) solution containing 0.02% acetone in a knotted PTFE reactor (KR), which was freely coiled around a 6-W low pressure mercury lamp. While passing the KR, reserpine was transformed into an intensively fluorescent compound. It was on-line detected in a flow-through cell at the emission wavelength of 490 nm and excitation wavelength of 386 nm. At optimized conditions, a detection limit 0.45 μg l −1 was achieved at a sampling rate of 90 h −1. Eleven determinations of a 0.5 mg l −1 reserpine standard solution gave a R.S.D. of 0.3%. The linear dynamic range of reserpine calibration curve was 0.01–0.75 mg l −1. The proposed method was applied to assay the reserpine content in tablets and to monitor the dissolution profile of reserpine tablets. Satisfactory results were obtained for both the assays and dissolution studies.

Determination of reserpine by in situ sensitized photochemical spectrofluorimetry

An in situ photochemical spectrofluorimetic method for the rapid and precise determination of reserpine was proposed. Adding acetone to the reserpine solution in acetic acid medium will speed up the photochemical conversion of reserpine into an intensively fluorescent compound. The determination can be carried out by measuring the fluorescence intensity at a fixed time. The mechanism of the sensitization of acetone was also discussed. The linear concentration range of the calibration graphs was found to be 0-0.91 μg ml −1. The detection limit was 0.40 ng ml −1 reserpine and the relative standard deviation was 0.75% for 0.40 ng ml −1 reserpine ( n = 6). The recovery for its application to reserpine injections was 97.3–103%. Through a standard addition recovery test, we obtained a recovery between 91.3 and 100% in urine samples. Interference effects of some common ions in serum and foreign substances coexisting with reserpine in complex reserpine tablets were also tested.

Determination of Reserpine in Tablets by Liquid Chromatography with Fluorescence Detection: Revised Procedure

A procedure is presented for the determination of reserpine in tablets by liquid chromatography (LC) that is a slight modification of a method presented in a previous publication. The sample is extracted with methanol, and solutions are filtered through filter paper. For LC, a 7.5 cm column is used; the mobile phase is methanol containing a small volume of an aqueous solution of the sodium salt of 1-pentanesulfonic acid. Detection is by fluorescence with 280 nm excitation and 360 nm emission. Two commercial samples containing 0.1 and 0.25 mg reserpine were analyzed. For each sample, 2 determinations were made on a group composite. Ten tablets were also analyzed individually. A linearity study was conducted, with solutions ranging in concentration from 80 to 120% of the amount present in the reference solution.

High Performance Liquid Chromatographic Determination of Diuretic-Antihypertensive Combination Products. II. Polythiazide and Reserpine

Abstract A high performance liquid chromatographic method for the simultaneous determination of polythiazide and reserpine in tablets is described. Polythiazide, reserpine, and vanillin (an excipient) are separated isocratically on an octadecylsilane column using a methanol-water-acetic acid (55:44:1) mobile phase. The column effluent was monitored by ultraviolet ab-sorbance at 254 nm. Recoveries from synthetic formulations were 100.2 ± 1.7% for polythiazide and 98.7 ± 1.1% for reserpine.

Stability of reserpine injections and tablets submitted by U.S. hospitals

The stability of reserpine injections and tablets that had been stored in hospital pharmacies across the United States was studied. Through a voluntary FDA drug stability program, all hospital pharmacies in the United States were asked to complete a response card indicating information about the reserpine injections and tablets they had in stock. Based on the responses, FDA selected 93 samples of reserpine injections and 51 samples of reserpine tablets. The samples of injections were subjected to tests for identification, pH, presence of other alkaloids, presence of 3,4-dehydroreserpine, and strength. All samples of reserpine injections met USP requirements. Two samples of reserpine tablets representing one lot each from two manufacturers failed to meet USP requirements for content uniformity. Reserpine injections and tablets appear to be stable under actual marketplace conditions.

Effect of Processing Factors on the Qualities of Reserpine Tablets

AbstractReserpine tablets were made by five different processing techniques. The tablets were tested for weight variation, content uniformity, hardness, friability and disintegration. The stability of reserpine in the com-pressed tablets was evaluated at accelerated conditions of 50° and 83% R. H. for a period of 6 months and at room conditions for 18 months. In-vitro availability studies were conducted on the tablets produced by the various techniques. It is shown that the method of preparation of tablets influences their properties in cluding stability and in-vitro availability.

Differential Pulse and AC Polarography of Reserpine, Using an Aprotic Organic Solvent System

Previously demonstrated advantages of aprotic organic solvent for analysis of organic pharmaceuticals have been applied to the assay of reserpine tablets. A procedure using high sensitivity electroanalytical relaxation methods was developed which is simpler and more sensitive than the USP assay. Most data were obtained with a commercial differential pulse polarograph which is widely available. However, less extensive measurements with other instruments established the general applicability of the differential pulse method, as well as various acpolarographic techniques. The results of differential pulse polarographic (DPP) and USP assays of synthetically formulated reserpine tablets compare favorably. The DPP method yields an average recovery for 0.1 mg reserpine/tablet of 100%, with a range of 97.6-102.3%. Corresponding data for 0.25 mg reserpine/tablet are 99.3%, with a range of 97.6-100.6%. Satisfactory results also were obtained in content uniformity studies, using single 0.1 and 0.25 mg tablets.

Collaborative Study of a Semiautomated Fluorometric Method for the Determination of Reserpine in Tablets

A semiautomated fluorometric method for the determination of resperpine in tablets was collaboratively studied by 7 laboratories. The method is a modification of the semiautomated method of Urbányi and Stober, which involves formation of a fluorogen with vanadium pentoxide. Collaborators were supplied with 3 composites, each from a different dosage level of commercial tablets. The results obtained agreed well with the AOAC manual fluorometric method; coefficients of variation ranged from 0.45 to 2.70%. The method has been adopted as official first action.

Photooxidation of Reserpine

The final product of the irradiation of reserpine in a chloroform solution was isolated and shown to be 3,4,5,6‐tetradehydroreserpine. The structure was determined by NMR spectroscopy as well as by chemical oxidation of reserpine. 3,4‐Dehydroreserpine was found to be an intermediate in both the chemical and photooxidation reactions. TLC examination of several reserpine tablets showed the presence of small amounts of dehydroreserpine but no tetradehydroreserpine.

Study of the AOAC Chromatographic Procedure for Reserpine Tablets

Abstract The procedure developed by Barkan and Kunze was used to analyze uncoated reserpine tablets representing 108 formulations from 60 drug manufacturers. To assay certain products, changes in the original method were required because of interferences from excipients; these changes involved column and sample preparation. The standard deviations of the modified procedure were 1.54% of declared (ultraviolet assay) and 0.90% of declared (colorimetric assay) at the 0.25 mg/tablet level.

Semiautomated Method for the Determination of Reserpine in Tablets

Abstract A chloroform solution of reserpine tablets is automatically sampled, washed successively with aqueous solutions of citric acid and sodium bicarbonate, and diluted with methanol. The chloroform-methanol solution is split into 3 streams: one flows sequentially through 2 UV spectrophotometers, recording the absorbances at 268 and 295 nm; the other 2 streams are used for the colorimetric assay (addition of hydrochloric acid and sodium nitrite) and blank (hydrochloric acid only). Day-to-day relative standard deviations were 0.40–0.95%. Comparisons with Barkan’s chromatographic procedure and the USP XVII method are presented.

Chromatographic Procedure for Determination of Reserpine in Tablets. II. Collaborative Study

Abstract A method is described for the quantitative determination of reserpine in tablet formulations. A suitable amount of tablet material is triturated with dimethylsulfoxide (DMSO), incorporated onto Celite, and transferred to a chromatographic column containing acid, base, and water layers. The reserpine is eluted with chloroform and quantitated spectrophotometrically. Duplicate results from 16 collaborators averaged 100.7% recovery as determined by UV, 98.8% recovery determined by colorimetric analysis. The method is recommended for adoption as official first action.

Chromatographic Procedure for Determination of Reserpine in Tablets. I. Comparison with USP Method

Abstract A column partition procedure for the analysis of reserpine in tahlets is presented. The sample formulation is triturated with dimethyl sulfoxide (DM SO), incorporated on Celite, and transferred to a column containing hase, acid, and water layers. Recovery is quantitative; no degradation of reserpine by DM SO is evidenced.