Quantitation of Sulfacetamide,Sulfadiazine, Sulfamerazine and Sulfame Thazine in Various Cominations Dsing High-Performance Liquid Chromatography

Abstract

A reverse phase high-performance liquid chromatography method for the quantitation of sulfacetamide, sulfadiazine, sulfamerazine, and sulfamethazine in various combinations has been developed. The method is simple, accurate, precise and reproducible. The percent relative standard deviations based on 6 injections were 2.1, 0.6, 1.9, and 1.6 for sulfacetamide, sulfadiazine, sulfamerazine, and sulfamethazine, respectively. The ratio of peak heights (drug/internal standard) wer closely related (r value 0.99 or better) to concentrations (± 20% of the standard solution concentrations). The results of synthetic mixtures showed quantitative recovery and method was successfully applied to commercial dosage forms (tablets and suspension). Extraction of sulfa drugs from the dosage forms required a very simple procedure.     

Surface-enhanced Raman analysis of sulfa drugs on colloidal silver dispersion

Surface-enhanced Raman spectrometry (SERS) of three sulfa drugs (sulfadiazine, sulfamerazine, and sulfamethazine) is reported. Silver colloidal dispersions prepared by simple borohydride reduction of silver nitrate are used as substrates. The capability of SERS for spectral fingerprinting of analytes with close structural properties using easily prepared substrates and relatively simple instrumentation is illustrated. By careful attention to the timing in the measurement, quantitative information can be obtained from silver colloids. Linearity was achieved up to 100 ng mL-1. Limits of detection range in the low nanograms per milliliter level.     

Stability-Indicating HPLC Method for Betaxolol HCl and Its Pharmaceutical Dosage Forms

Abstract

The present work describes a specific, stability-indicating high-performance liquid chromatographic method for determination of betaxolol HCl and its pharmaceutical dosage forms. Betaxolol HCl was chromatographed on a microbondapak C18 column utilizing a simple mixture of methanol: acetonitrile:0.1% diethylamine (pH 3.0 adjusted using orthophosphoric acid). It was detected at 222 nm. The method is accurate and precise with a percent relative standard deviation of 0.11 based on 6 readings. A number of inactive ingredients present in the dosage forms (eye drop, tablet, gel) did not interfere in the assay procedure. The recovery from synthetic mixtures was quantitative. The extraction procedure from the dosage forms is very simple. The drug appears to be very sensitive to acids (such as sulfuric acid) since 100% of the drug decomposed on boiling for 5 min.     

Quantitation of Cefadroxil in Pharmaceutical Dosage Forms Using High-Performance Liquid Chromatography

A high-performance liquid chromatography method for the quantitation of cefadroxil has been developed. The method has been applied to quantify cefadroxil in pharmaceutical dosage forms (capsules, suspensions and tablets) of 2 different manufacturers. A simple extraction procedure to extract cefadroxil from the dosage forms has been developed. The results were excellent with percent relative standard deviation of 1.2 based on 5 readings. A variety of inactive ingredients present in the dosage forms did not interfere with the assay procedure. After formulating, the suspensions were stable for longer periods at 5^o than recommended on the label.     

How to search the experimental conditions that improve a Partial Least Squares calibration model: Application to a flow system with electrochemical detection for the determination of sulfonamides in milk

This paper deals with the selection of experimental conditions and how the signals obtained in these conditions influence the fitted Partial Least Squares calibration model. The multivariate signals come from a flow analysis system with amperometric detection when determining sulfadiazine, sulfamerazine and sulfamethazine in milk.The solution (carrier plus analyte) was pumped through the system to provide a continuous supply of analyte to the cell. The detector was programmed for a scan mode operation being the multivariate signal the hydrodynamic voltammogram. To obtain an analytical signal of enough analytical quality, the Net Analyte Signal and its standard deviation have been optimised by using an experimental design. The conflicting behaviour of the two responses has been solved by estimating the Pareto-optimal front.The multivariate signals recorded in the optimal conditions found have been calibrated by Partial Least Squares regression and their figures of merit validated according to the criteria established in European Decision 2002/657/EC.In relation to the permitted limit, 100 µg l^− 1 in milk, for the total content of sulfonamides established in the Commission Regulation EC no. 281/96 the proposed method has a decision limit of 109.1 µg l^− 1 and the capability of detection is 117.9 µg l^− 1 for both probability of false non-compliance and of false compliance equal to 5%. A recovery of 86.5% ± 2.4% (n = 5) has been obtained.     

Determination of Sulfonamides in Triplesulfa Cream by Hplc Method

A fast, accurate, economical, and reproducible HPLC procedure has been developed to quantitate sulfacetamide (I), sulfabenzamide (II), and sulfathiazole (III) in vaginal creams, using sulfapyridine (IV) as internal standard. The method employed u Bondapak phenyl column, Waters Liquid Chromatograph, Hewlett-Packard 3390A reporting integrator and UV detector set at 280 nm. The mobile phase consisted of 7:3 mixture of 0.01 M ammonium hydrogen phosphate and methanol (pH 7.2). The method met USP requirements for system suitability and linearity (R=0.998). The USP method consistently gave low and widely varying results ranging from 75 to 102% for sulfacetamide. The results for sulfabenzamide and sulfathiazole were comparable by both methods. The relative retention time for I, II, III, IV were 0.4, 0.5, 0.9, and 1.0 respectively for the proposed method and 0.8, 2.5, 1.8, and 1.0 for the USP method. The USP method was tedious and unreliable for assay of (I). Considering the cost of the column and mobile phase, the proposed method was 70% less costly than the USP method.     

Quantitation of Cephalexin in Pharmaceutical Dosage Forms Using High-Performance Liquid Chromatography

A high-performance liquid chromatography method has been developed to quantify cephalexin in pharmaceutical dosage forms, capsules, pediatric drops and suspensions. The method is accurate and precise with a percent relative standard deviation of 0.8 based on 6 readings. There is no interference from a variety of excipients present in the dosage forms. The procedure for the extraction of cephalexin from the dosage forms is very simple. The method is stability indicating since a sample decomposed using sodium hydroxide showed very little potency and new peaks in the chromatogram. In the powder form cephalexin appears to be very stable.     

Quantitation of Cephalexin in Pharmaceutical Dosage Forms Using High-Performance Liquid Chromatography

Abstract

A high-performance liquid chromatography method has been developed to quantify cephalexin in pharmaceutical dosage forms, capsules, pediatric drops and suspensions. The method is accurate and precise with a percent relative standard deviation of 0.8 based on 6 readings. There is no interference from a variety of excipients present in the dosage forms. The procedure for the extraction of cephalexin from the dosage forms is very simple. The method is stability indicating since a sample decomposed using sodium hydroxide showed very little potency and new peaks in the chromatogram. In the powder form cephalexin appears to be very stable.     

Gold immunochromatographic sensor for the rapid detection of twenty-six sulfonamides in foods

A gold immunochromatographic sensor (GICS) was developed for the rapid detection of 26 sulfonamides in honey samples.The sensor was based on a group-specific monoclonal antibody (mAb) that can recognize all 26 sulfonamides.Three haptens (hapten 1 with a thiazole ring,hapten 2 with a benzene ring,and hapten 3 with a straight carbon chain) were used for antigen preparation.With hybridoma technology,a group-specific mAb was screened with a 50％ maximal inhibitory concentration (IC50) against sulfathizole (STZ) and the other 25 analogues ranging from 0.08 to 90.18 ng/mL.Mono-dispersed gold nanoparticles were conjugated with the mAb to develop the lateral immunochromatographic strip.A labeled antibody concentration of 0.1 μg/mL and a coating antigen concentration of 0.2 μg/mL in the test line were chosen for strip preparation.Under optimized conditions,the visual limits of detection (vLOD) for the concentrations of STZ,sulfamethoxazole,sulfamethizole,sulfadiazine,sulfamerazine,sulfadimethoxine,sulfamonomethoxine,sulfameter,sulfamethoxypyridazine,and sulfachloropyridazine were 5,0.25,0.25,10,5,10,25,2.5,5,0.25,and 10 μg/kg,respectively.Scanner analysis in honey samples revealed good performance for detection of the 26 sulfonamides.Commercial honey samples were tested with the sensor and positive results were confirmed with high-performance liquid chromatography.The proposed strip sensor provides a convenient method for the rapid and reliable determination of sulfonamides pollutants in honey samples.     

Determination of azathioprine and its related substances by capillary zone electrophoresis and its application to pharmaceutical dosage forms assay

The development of a stability-indicating capillary zone electrophoresis (CZE) method for the determination of the drug azathioprine (AZA) and its related substances in bulk and dosage forms is described. Theophylline was used as an internal standard to improve quantitative results. The method was fully validated in terms of repeatability (n = 10, RSD for migration time and peak area ratio were 0.15% and 0.60%, respectively), reproducibility (n = 5, RSD of peak area ratio was 0.84%), linearity at two ranges of the azathioprine concentration, limits of detection (LOD) and quantitation (LOQ), and robustness. The method was applied for determination of the drug in bulk and a commercial tablet dosage form (recovery 98.3-101.3%) and in powder for injection (recovery 98.7-100.6%). The method was fast and reliable for the analysis of AZA and its related substances in bulk and dosage forms.     

Quantitation of Phenylephrine Hydrochloride in Pharmaceutical Dosage Forms

A reverse phase high-pressure liquid chromatography method for the quantitation of phenylephrine hydrochloride in a variety of pharmaceutical dosage forms has been developed. The developed method did not require the use of a counter-ion t o increase the retention time of phenylephrine. The method is simple, accurate, precise and reproducible with a percent relative standard deviation of 0.54 based on 6 injections. The results were in excellent agreement with the results obtained using a colorimetric method. The separation between phenylephrine, the internal standard and other ingredients is greatly affected by pH changes (between 5.9-6.1) and the particle size of the column materials (5 micron versus 10 micron). A number of other active ingradinents brompheniramine maleate, chlopheniramine maleate, phenylpropanolamine and guaifenesin, etc. and the excipients such as parabens and sodium benzoate did not interfere with the assay procedure.     

Stability Indicating Hplc Method for Ribavirin and its Pharmaceutical Dosage Forms

The present work describes a specific, stability indicating HPLC method for determination of Ribavirin (1) and its pharmaceutical dosage forms.

Ribavirin was chromatographed on a microbondapak C18 column utilizing a simple mixture of 0.01M dibasic potassium phosphate and methanol (95: 5). The detection was done at 207 nm.

The available literature was scanned to locate the various methods(2,3) available along with the one reported in USP XXII.

A comparative study was made of the proposed method and USP method and the advantages over the USP method have been discussed.

The low value of Relative standard deviation and recovery of the drug in the range of 99.1% to 101.5% indicates a good precision and non-interference of the method.     

Electrospun poly(ε-caprolactone) matrices containing silver sulfadiazine complexed with β-cyclodextrin as a new pharmaceutical dosage form to wound healing: preliminary physicochemical and biological evaluation

Cooperation between researchers in the areas of medical, pharmaceutical and materials science has facilitated the development of pharmaceutical dosage forms that elicit therapeutic effects and protective action with a single product. In addition to optimizing pharmacologic action, such dosage forms provide greater patient comfort and increase success and treatment compliance. In the present work, we prepared semipermeable bioactive electrospun fibers for use as wound dressings containing silver sulfadiazine complexed with β-cyclodextrin in a poly(?-caprolactone) nanofiber matrix aiming to reduce the direct contact between silver and skin and to modulate the drug release. Wound dressings were prepared by electrospinning, and were subjected to ATR-FT-IR and TG/DTG assays to evaluate drug stability. The hydrophilicity of the fibrous nanostructure in water and PBS buffer was studied by goniometry. Electrospun fibers permeability and swelling capacity were assessed, and a dissolution test was performed. In vitro biological tests were realized to investigate the biological compatibility and antimicrobial activity. We obtained flexible matrices that were each approximately 1.0?g in weight. The electrospun fibers were shown to be semipermeable, with water vapor transmission and swelling indexes compatible with the proposed objective. The hydrophilicity was moderate. Matrices containing pure drug modulated drug release adequately during 24?h but presented a high hemolytic index. Complexation promoted a decrease in the hemolytic index and in the drug release but did not negatively impact antimicrobial activity. The drug was released predominantly by diffusion. These results indicate that electrospun PCL matrices containing β-cyclodextrin/silver sulfadiazine inclusion complexes are a promising pharmaceutical dosage form for wound healing.     

Quantitation of Cefaclor in Pharmaceutical Dosage Forms Using High Performance Liquid Chromatography

A stability-indicating high-performance liquid chromatography for the quantitation of cefaclor in pharmaceutical dosage forms has been developed. The method is accurate and precise with a percent relative standard deviation of 1.2 based on 5 readings. A number of inactive ingredients present in the capsules and suspensions did not interfere with the assay procedure. The extraction procedure from the dosage forms is very simple. The recovery from the synthetic mixtures was quantitative. The capsules which had expired 3 years ago lost only 3% of the potency. The drug appears to be very sensitive to strong acids or bases since a 5 minute boiling caused 100% degradation of drug in both the solutions.     

Quantitation of Cefaclor in Pharmaceutical Dosage Forms Using High Performance Liquid Chromatography

Abstract

A stability-indicating high-performance liquid chromatography for the quantitation of cefaclor in pharmaceutical dosage forms has been developed. The method is accurate and precise with a percent relative standard deviation of 1.2 based on 5 readings. A number of inactive ingredients present in the capsules and suspensions did not interfere with the assay procedure. The extraction procedure from the dosage forms is very simple. The recovery from the synthetic mixtures was quantitative. The capsules which had expired 3 years ago lost only 3% of the potency. The drug appears to be very sensitive to strong acids or bases since a 5 minute boiling caused 100% degradation of drug in both the solutions.     

Optimization of Chemiluminescent Nitrogen Detection for Packed-Column Supercritical Fluid Chromatography with Methanol-Modified CO(2)

A chemiluminescent nitrogen detector was optimized for packed-column supercritical fluid chromatography. Methanol modifier concentrations of 15% or less, an ozone flow of 5.8 mL/min, and a decompressed CO(2) flow between 240 and 310 mL/min were found to exhibit a maximum sensitivity of 5 ng for sulfamethazine (1 ng of N). The addition of a membrane drier to the "optimized" system further decreased the minimum detectable quantity (MDQ) to 0.5 ng (0.1 ng of N). In addition, by using a microbore column (2 mm i.d.) instead of an analytical scale column, the postcolumn decompressed flow split could be eliminated, further reducing the MDQ to 0.125 ng of sulfamethazine (0.025 ng of N).     

反相液相色谱法测定复方泰妙菌素注射液中泰妙菌素、磺胺嘧啶钠的含量

目的：建立反相液相色谱法测定复方泰妙菌素注射液中泰妙菌素、磺胺嘧啶钠的含量的方法。方法：采用Shim—packCLC—ODS柱（150mm×6mm,5μm）,流动相为80％乙腈-0．7％磷酸氢二铵（体积比为0．3：0．7）并用氨试液调节pH至8．0±0．1。流速为1．0mL／min,检测波长为208nm,柱温为40℃。结果：在此色谱条件下两者能完全分离,泰妙菌素在5-40μg／mL和磺胺嘧啶钠在10—80μg／mL的范围内浓度与峰面积呈良好的线性关系,回归方程和相关系数分别为：A=47205．9p＋2003．72,R=0．9999;A=77050p＋5514．75,R=0．9999。泰妙菌素和磺胺嘧啶钠的平均回8：4分别为99．99％、99．7％;RSD分别为0．70％、0．95％。结论：方法简便、快速、准确,可用作复方泰妙菌素注射液的含量测定。     

Quantitation and Stability of Verapamil Hydrochloride using High-Performance Liquid Chromatography

A high-performance liquid chromatography method for the quantitation of verapamil hydrochloride in pharmaceutical dosage forms has been developed. The method is precise and accurate with a relative standard deviation of 0.63% based on six injections. No preliminary extraction procedure is required to assay injections and a very simple extraction procedure is needed for tablets. There is no interference from the excipients and the method appears to be stability-indicating. The optimum pH range of stability is about 3.2 to 5.6 and the phosphate buffer and ionic strength have very little effect on the stability. Verapamil hydrochloride appears to be a very stable compound since in 105 days at 50°, the aqueous solutions (0.5 mg/ml) did not decompose.     

Development and Validation of a High-Performance Liquid Chromatographic Method for the Analysis of Propylthiouracil in Pharmaceuticals

A simple, rapid, and stability-indicating high-performance liquid chromatographic (HPLC) method was developed and validated for the assay of propylthiouracil (PTU). The method was used to quantify PTU in topical formulations and in tablets. Excellent linearity was observed between PTU concentration and the peak area (R² = 0.999). The limit of detection was 1 ng, and the limit of quantitation was 1.2 ng. The method proved to be selective. Selectivity was validated by subjecting a stock solution of PTU to acidic, basic, and oxidative degradations. The peaks of the degradation products did not interfere with the peak of PTU. Excipients present in the dosage forms did not interfere with the analysis, and the recovery of PTU from each dosage form was quantitative.     

Validation of Liquid Chromatographic Method of Assay for Acetaminophen, Butalbital and Caffeine in Solid Dosage Forms

The validation of a liquid chromatographic procedure for the determination of acetaminophen, butalbital and caffeine in solid dosage forms is described. The dosage content of tablets or capsules is diluted and chromatographed on a Radialpak Cyanopropylsilane Cartridge with a mobile phase of water-acetonitrile-1M dibutylamine phosphate (90+9+1, V/V) with detection at 215 nm. The calibration curve is linear with correlation coefficients of 0.999 for each component. Recoveries of spiked excipient blend averaged 99.5% for acetaminophen, 102.5% for butalbital and 101.0% for caffeine. The method met USP requirements for system suitability with proper resolution between two adjacent peaks. The relative standard deviation (RSD) of peak response of each component (obtained by chromatographing six replicates of standard solution) is less than 2.0% and the tailing factor of each component is not greater than 1.5. The method can be used for composite, content uniformity and dissolution assay of acetaminophen, butalbital and caffeine in tablet and capsule formulations.