Enantiomeric Separation and Quantitative Determination of Propranolol in Tablets by Chiral High-Performance Liquid Chromatography

This work reports an application of chiral high-performance liquid chromatography (HPLC) in the separation and quantitative determination of propranolol isomers in tablets. The isomers were separated using a Chiralcel OD® column (250 × 4.6 mm, 10 μm) with a mobile phase of hexane:ethanol (75:25 v/v) at a flow rate of 0.7 ml/min and ultraviolet detection at 280 nm. The coefficient of variation and average recovery of (R)-isomer for samples A, B, C, and D were 0.72% and 100.30%, 0.67% and 99.40%, 0.62% and 99.76%, and 0.70% and 99.68%, respectively. The coefficient of variation and average recovery of (S)-isomer for samples A, B, C, and D were 0.74% and 99.62%, 0.64% and 100.27%, 0.71% and 99.99%, and 0.70% and 99.72%, respectively.     

Enantiomeric Separation and Quantitative Determination of Atenolol in Tablets by Chiral High-Performance Liquid Chromatography

The separation and quantitative determination of atenolol isomers by chiral high-performance liquid chromatography (HPLC) are described. Atenolol isomers were separated using a Chiralcel OD® column (250 × 4.6 mm,10 μm); the mobile phase was hexane-ethanol-diethylamine (75:25:0.1 v/v/v); ultraviolet detection was at 276 nm; and flow rate was 0.7 ml/min. The coefficient of variation and average recovery of (R)-isomer were 0.60% and 100.37%, respectively, for sample A and 0.69% and 100.63%, respectively, for sample B. The coefficient of variation and average recovery of (S)-isomer were 0.59% and 100.33%, respectively, for sample A and 0.63% and 99.78%, respectively, for sample B.     

Determination of Steroid Hormones in Oral Contraceptives by High-Performance Liquid Chromatography

ABSTRACT

The aim of this research was to standardize a high-performance liquid chromatographic method for quantitative determination of steroid hormones, like ethinylestradiol (ETE), levonorgestrel (LEVO), and gestodene (GEST), in commercially available oral contraceptives (OCs). The combination ETE– LEVO was analyzed using a LiChrospher® 100 RP-8 column (5 μm, 125×4 mm) in LiChroCART®, with a mobile phase constituted of acetonitrile: water (60:40 v/v). Using the same column, ETE–GEST was analyzed with a mobile phase constituted of acetonitrile:water (50:50 v/v) at pH 7.5 adjusted with 0.02 M ammonium hydroxide. For both methods, a flow rate of 0.8 mL/min was utilized and detection was carried out at 215 nm. All analyses were performed at room temperature (24±2°C).

Calibration curves for ETE–LEVO were obtained using solutions with concentration ranges from 2.40 to 60.0 μg/mL (ETE), and from 12.0 to 300.0 μg/mL (LEVO). Calibration curves for ETE–GEST were obtained using solutions with concentration ranges from 2.40 to 60.0 μg/mL (ETE), and from 9.0 to 160.0 μg/mL (GEST). Correlation coefficients obtained were from 0.9999 to 0.9990. Coefficients of variation for samples containing ETE–LEVO were 0.47% and 0.38%, respectively. For samples with ETE–GEST they were 0.39% and 0.44%, respectively. The average recovery for samples with ETE–LEVO was 103.46% and 100.78%, respectively. For samples containing ETE–GEST it was 100.89% and 101.03%, respectively.     

Simultaneous Determination of Thiabendazole and Mebendazole in Tablets by High-Performance Liquid Chromatography

Reversed-phase high performance liquid chromatography using an RP 18 column (4 × 125 mm), tetrahydrofuran–acetonitrile–0.5% formic acid (5:25:70, v/v/v) as mobile phase and UV detection at 254 nm enabled the simultaneous determination of thiabendazole (TZ) and mebendazole (MZ) in tablets. The method showed linearity over 4.0 to 40.0 μg TZ/ml and 6.0 to 60.0 μg MZ/ml. The correlation coefficient r was. 9999 for both TZ and MZ. The coefficient of variation (CV) was 0.59–0.80% for TZ and 0.49–0.67% for MZ. The average recovery was 100.54–101.17% for TZ and 100.35–101.13% for MZ. The excipients of the tablets did not interfere in the proposed method. The developed method is precise, accurate, and selective for the determination of both benzimidazoles analyzed.     

Quantitation of Propranolol Hydrochloride in Pharmaceutical Dosage Forms by High-Performance Liquid Chromatography

Abstract

A high-performance liquid-chromatography method for the quantitation of propranolol hydrochloride in pharmaceutical dosage forms (capsules, injections and tablets) has been developed. The method can also be used for contents uniformity as required by USP-NF. There is no interference from the excipients present and from hydrochlorothiazide which is often mixed with propranolol hydrochloride. The method is accurate, reproducible and precise with a percent relative standard deviation of 0.6 based on 5 readings. A sample decomposed with sodium hydroxide treatment showed about 9% potency and 2 new peaks in the chromatogram.     

Quantitation of Hydrochlorothiazide in Combination with Methyldopa and Propranolol Hydrochloride by High-Performance Liquid Chromatography

A stability indicating assay method based on highperformance liquid chromatography has been developed for the quantitation of hydrochlorothiazide in combination with methyldopa and propranolol hydrochloride. The method is accurate, reproducible and precise with an average percent relative standard deviation of 1.3. The method can also be used for the quantitation of the only known impurity/decomposition product (4-amino, 6 chloro, 1,3 benzenedisulfonamide) in hydrochlorothiazide. For the complete separation of methyldopa from hydrochlorothiazide, a counterion, 1-heptanesulfonic acid sodium was added to the mobile phase to increase the retention time of methyldopa. A 4-5 minutes time to extract hydrochlorothiazide from tablets appears to be satisfactory.     

Quantitation of Ciprofloxacin Hydrochloride and Norfloxacin in Tablets Using High-Performance Liquid Chromatography

A stability-indicating high-performance liquid chromatography method for the quantitation of ciprofloxacin and norfloxacin in tablets (the only dosage form available at present) has been developed. The method is precise and accurate with a percent relative standard deviation based on 5 readings of 1.2 and 1.4 for ciprofloxacin and norfloxacin, respectively. A number of inactive ingredients present in the tablets did not interfere with the assay procedures. The addition of hydrochloric acid in the extraction procedure was necessary for the quantitative recovery and reproducible results. The recovery from the synthetic mixtures was quantitative. Both the drugs (quinolones) appear to be very stable since 10 minute boiling with either sulfuric acid or sodium hydroxide solution caused very little decomposition.     

Quantitation of Ranitidine Hydrochloride in Tablets and Injections Using High-Performance Liquid Chromatography

Abstract

A stability-indicating reverse-phase high-performance liquid chromatography method without the use of a counterion has been developed to quantify ranitidine hydrochloride in pharmaceutical dosage forms. The method is accurate and precise with a percent relative standard deviation of 1.5 based on 5 injections. The extraction procedure for ranitidine from tablets is very simple and there was no interference from the excipients present. Ranitidine appears to be stable to heat on the acidic side and very susceptible to decomposition on the basic side. It lost 84.4% of potency on 20 minute boiling with sodium hydroxide with a new peak in the chromatogram. It lost 37.8% of the potency on treatment with hydrogen peroxide solution for 20 minutes at room temperature with 2 new peaks in the chromatogram.     

Determination of Clozapine and its Metabolite,Norclozapine in Various Biological Matrices Using High-Performance Liquid Chromatography

Purpose. To develop and validate an HPLC method for the quantitation of clozapine and its metabolite, norclozapine in human plasma, rat plasma, and the various human plasma lipoprotein fractions. Methods. Using liquid-liquid extraction, clozapine, and norclozapine are extracted from the biological matrix with MTBE. After concentration, the residue was reconstituted in 1mM HCl and injected on to a C6 Phenyl column (3μm, 2.0×150 mm). Mobile phase was 10mM Ammonium Acetate, pH 5—Acetonitrile—Methanol (5:3:2, v/v/v). Loxapine served as the internal standard. Absorbance was measured at 254 nm. Results. Quantitation limits for clozapine and norclozapine was 100 ng/mL and 50 ng/mL, respectively. Recovery for both clozapine and norclozapine was near 100%. Percent accuracy for intraday variability in human plasma, rat plasma, and human TRL, HDL, LDL, and LPDP lipoprotein fraction was between 92 to 113% for both analytes. Intraday precision for the same matrices was less than 9% CV for both analytes. Percent accuracy and precision for interday variability in human plasma was 97 to 103% and less than 10% CV, respectively. Samples were stabile in the autosampler for 80 h at 10°C and on the benchtop for 2 h. It should be noted, Clozapine-N-oxide, which is a known metabolite of Clozapine, was not determined since it is not clinically active. Conclusions. This method is a simple, fast and robust HPLC assay for the determination of clozapine and norclozapine in various matrices and lipoprotein fractions.     

High-Performance Liquid Chromatographic Determination of Ibuprofen in Bulk Drug and Tablets

Abstract

A simple and rapid HPLC procedure is described for the assay of ibuprofen in bulk drug and tablets and for dosage uniformity testing. HPLC was carried out on a stainless steel octadecylsilane (5 urn) column (150 × 4.6 mm) using 25% 0.25M glacial acetic acid in acetonitrile as the mobile phase, with UV detection at 254 nm. Results obtained with this procedure compared favorably with those obtained using the USP procedures.     

High-Performance Liquid Chromatographic Determination of Ibuprofen in Bulk Drug and Tablets

A simple and rapid HPLC procedure is described for the assay of ibuprofen in bulk drug and tablets and for dosage uniformity testing. HPLC was carried out on a stainless steel octadecylsilane (5 urn) column (150 × 4.6 mm) using 25% 0.25M glacial acetic acid in acetonitrile as the mobile phase, with UV detection at 254 nm. Results obtained with this procedure compared favorably with those obtained using the USP procedures.     

Simultaneous Determination of Pyridoxine Hydrochloride and Doxylamine Succinate from Tablets by Ion Pair Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC)

A new, simple, precise, and rapid ion pair reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed for the simultaneous determination of pyridoxine hydrochloride (PYR) and doxylamine succinate (DOX) in tablets. The stationary phase was a Microbondapak C18 column (10 μ, 300 mm × 3.9 mm i.d.). The mobile phase was water:methanol (60:40) containing 10 mM heptanesulfonic acid and 0.25% triethylamine and adjusted to pH 2.2 with orthophosphoric acid. Detection was carried out at 263 nm using an ultraviolet (UV) detector. The flow rate was 1.0 ml/min, and retention times were 3.65 min and 7.32 min for PYR and DOX, respectively. The linearity was obtained in the concentration range 0.5–500 μg/ml for PYR and DOX. Mean percentage recoveries were 100.20% and 101.20% for PYR and DOX, respectively.     

高效液相色谱法测定牛磺酸颗粒中牛磺酸的含量

建立了测定牛磺酸含量的高效液相色谱(HPLC)方法。方法采用2,4-二硝基氟苯对牛磺酸进行衍生,在ul-timate C18柱(250×4.6mm,5μm)色谱柱上,0.5%三乙胺(用磷酸调PH=4.0)和乙腈为流动相进行梯度洗脱,检测波长360nm。牛磺酸在4.68×10-10～8.49×10-5mol/L范围内与峰面积呈现良好的线性关系(r=0.9998)。所建立的方法简单、简单,可用于制剂中牛磺酸含量的测定。     

Simultaneous Determination of Pyridoxine Hydrochloride and Doxylamine Succinate from Tablets by Ion Pair Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC)

A new, simple, precise, and rapid ion pair reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed for the simultaneous determination of pyridoxine hydrochloride (PYR) and doxylamine succinate (DOX) in tablets. The stationary phase was a Microbondapak C18 column (10 μ, 300 mm × 3.9 mm i.d.). The mobile phase was water:methanol (60:40) containing 10 mM heptanesulfonic acid and 0.25% triethylamine and adjusted to pH 2.2 with orthophosphoric acid. Detection was carried out at 263 nm using an ultraviolet (UV) detector. The flow rate was 1.0 ml/min, and retention times were 3.65 min and 7.32 min for PYR and DOX, respectively. The linearity was obtained in the concentration range 0.5-500 μg/ml for PYR and DOX. Mean percentage recoveries were 100.20% and 101.20% for PYR and DOX, respectively.     

Simultaneous Determination of Metronidazole Benzoate Methylparaben, and Propylparaben by High-Performance Liquid Chromatography

The simultaneous determination of metronidazole benzoate (MB), methylparaben (MP), and propylparaben (PP) in an oral suspension formulation was developed using high-performance liquid chromatography (HPLC). The method was developed using a Novapak C₁₈ (3.9 × 150 mm, 4 μm) column, methanol-water (50:50, v/v) as the mobile phase and an ultraviolet (UV) detector at 254 nm. The peak area response versus concentration was linear in a concentration range from 40 to 400 μg/ml of MB, 0.8 to 8.0 μg/ml of MP, and 0.2 to 2.0 μg of PP. The correlation coefficients were 0.9997 for MB, 0.9987 for MP, and 0.9983 for PP, with relative standard errors of 1.12%, 1.28%, and 1.67%, respectively.     

Simultaneous Determination of Metronidazole Benzoate Methylparaben,and Propylparaben by High-Performance Liquid Chromatography

The simultaneous determination of metronidazole benzoate (MB), methylparaben (MP), and propylparaben (PP) in an oral suspension formulation was developed using high-performance liquid chromatography (HPLC). The method was developed using a Novapak C₁₈ (3.9 × 150 mm, 4 μm) column, methanol-water (50:50, v/v) as the mobile phase and an ultraviolet (UV) detector at 254 nm. The peak area response versus concentration was linear in a concentration range from 40 to 400 μg/ml of MB, 0.8 to 8.0 μg/ml of MP, and 0.2 to 2.0 μg of PP. The correlation coefficients were 0.9997 for MB, 0.9987 for MP, and 0.9983 for PP, with relative standard errors of 1.12%, 1.28%, and 1.67%, respectively.     

反相高效液相色谱法测定饮用水中的酚类化合物

介绍了反相高效液相色谱法测定饮用水中的酚类物质。该法采用的固相萃取预处理法操作简便,节省溶剂,且稳定性好,回收率高。实验以ODS柱为分离柱,采用梯度洗脱,可编程紫外检测器进行样品检测。方法准确,重现性好,杂质干扰少,检出限低。     

反相高效液相色谱法测定维生素B_1的含量

建立了测定维生素B1含量的高效液相色谱(HPLC)方法。方法采用ultimate C18柱(300×4.6mm,5μm)色谱柱,流动相为0.2%磷酸氢二钾水溶液(含5%甲醇,用磷酸调pH 2.6),检测波长245nm。维生素B1在0.002～2.0mg/mL范围内与峰面积呈现良好的线性关系(r=0.9968)。所建立的方法简单、准确、重现性好,可用于制剂中维生素B1含量的测定。     

Quantitative Determination of Troventol from Aerosols by Reversed Phase Liquid Chromatography

Troventol, an anticholinergic agent and a derivative of atropine was estimated quantitatively from the samples of aerosols. An isocratic, reversed-phase liquid chromatographic method was developed using a C6, 5-um column with mobile phase acetonitrile-water-diethylamine-phosphoric acid (40:60:0.1:0.1, v/v) filtered through 0.45-micron and degassed before use. Salbutamol in combination with troventol from an aerosol preparation was also determined simultaneously by the present method. Recoveries obtained for troventol as well as for salbutamol were in the range 98.0 to 102.0% from aerosols, monitored at wavelength 215 ran. A flow rate of 1.0 mL/min was maintained throughout the analysis.     

Quantitative Determination of Troventol from Aerosols by Reversed Phase Liquid Chromatography

Abstract

Troventol, an anticholinergic agent and a derivative of atropine was estimated quantitatively from the samples of aerosols. An isocratic, reversed-phase liquid chromatographic method was developed using a C6, 5-um column with mobile phase acetonitrile-water-diethylamine-phosphoric acid (40:60:0.1:0.1, v/v) filtered through 0.45-micron and degassed before use. Salbutamol in combination with troventol from an aerosol preparation was also determined simultaneously by the present method. Recoveries obtained for troventol as well as for salbutamol were in the range 98.0 to 102.0% from aerosols, monitored at wavelength 215 ran. A flow rate of 1.0 mL/min was maintained throughout the analysis.