Determination of ambroxol hydrochloride in tablets using flow-injection UV spectrophotometry and HPLC

A flow-injection UV spectrophotometric method was developed for the determination of ambroxol hydrochloride in tablets. The quantitative determination of ambroxol was performed at 245 nm using distilled water as the carrier solvent. In this study, the flow rate, loop volume, and the number of injections per hour were 15 mL/min, 193 μL, and 100, respectively. The analytical signal of ambroxol was linear in the concentration range of 40–200 μg/mL. The detection limit and limit of quantification were found as 11.55 and 38.49 μg/mL, respectively. The results for the determination of ambroxol in tablets, 29.99 ± 0.23 mg (mean ± SD), were in good agreement with the labeled quantities (30 mg/tablet). A relatively high recovery value (100.4%) shows the accuracy of the proposed method. Furthermore, the results obtained were in accordance with those obtained by the HPLC method, which were used as a comparison method for the determination of ambroxol HCl, as far as the Student’s t-test and Fisher test results were concerned. It was concluded that the proposed flow-injection UV spectrophotometric method was fast, accurate, precise, and suitable for automation in the determination of ambroxol. The text was submitted by the authors in English.     

Chemometric determination of naproxen sodium and pseudoephedrine hydrochloride in tablets by HPLC

A new chemometric determination by high-performance liquid chromatography (HPLC) with photodiode array (PDA) detection was implemented for the simultaneous determination of naproxen sodium and pseudoephedrine hydrochloride in tablets. Three chemometric calibration techniques, classical least squares (CLS), principle component regression (PCR) and partial least squares (PLS) were applied to the peak area at multiwavelength PDA detector responses. The combinations of HPLC with chemometric calibration techniques were called HPLC-CLS, HPLC-PCR and HPLC-PLS. For comparison purposes the HPLC method called the classic HPLC method was used to confirm the results obtained from combined HPLC-chemometric calibration techniques. A good chromatographic separation between two drugs with losartan potassium as an internal standard was achieved using a Waters Symmetry C18 Column 5 microm 4.6+/-250 mm and a mobile phase containing 0.2 M acetate buffer and acetonitrile (v/v, 40:60). The multiwavelength PDA detection was measured at five different wavelengths. The chromatograms were recorded as a training set in the mobile phase. Three HPLC-chemometric calibrations and the classic-HPLC method were used to test the synthetic mixtures of naproxen sodium and pseudoephedrine hydrochloride in the presence of the internal standard. The HPLC-chemometric approaches were applied to real samples containing drugs of interest. The experimental results obtained from HPLC-chemometric calibrations were compared with those obtained by a classic HPLC method.     

高效液相色谱法测定盐酸甲氯芬酯胶囊的含量

建立了用高效液相色谱测定盐酸甲氯芬酯胶囊含量的方法.采用Hypersil C18柱(5 μm,4.6 mm i.d.×200 mm),流动相为V(乙腈)∶V(0.12% NH4HCO3-0.50%三乙胺)溶液＝33∶67 (甲基磺酸调pH至3.0),流速: 1.0 mL/min,检测波长为225 nm.盐酸甲氯芬酯的线性范围为1.632～163.2 μg/mL,平均回收率为99.67%,RSD=1.8% (n=9).     

Determination of benzhexol hydrochloride in tablets by high-performance liquid chromatography

Separation on a LiChrosorb C₂ reversed-phase column with methanolic ammonium dihydrogenphosphate as eluent provides a simple determination of benzhexol hydrochloride in tablets containing 2–5 mg of the drug. Common excipients do not interfere.     

Determination of chlorpromazine hydrochloride in tablets by molecular emission cavity analysis

Sulphur in chlorpromazine hydrochloride (2–50 mg) is oxidized by dichromate in condensed phosphoric acid (CPA) to sulphate, which in turn is reduced to hydrogen sulphide by heating with tin dissolved in CPA. The gas is carried by nitrogen to a steel cavity situated in a hydrogen/nitrogen flame and the S₂ emission is measured at 384 nm. The method is applied to determine the drug in powdered tablets. No sample pretreatment is needed; the procedure takes 10 min.     

Determination of metformin hydrochloride in tablets by nuclear magnetic resonance spectrometry

The ¹H-n.m.r. signal of the drug (10–35 mg ml^?1) in deuterium oxide, with maleic acid as internal reference standard, is used. The integral of the peak at 3.06 ppm with respect to 3-trimethylsilylpropionic acid is compared with that at 6.3 ppm for the internal standard. The method is quantitative and free from interference by tablet excipients.     

Determination of ethambutol hydrochloride in the combination tablets by precolumn derivatization

A new high-performance liquid chromatography method for the quantitative determination of ethambutol hydrochloride in combination tablets is presented. Ethambutol is derivatized with phenylethylisocyanatate at room temperature (22 +/- 2 degrees C) for 5 min. Separation is performed by a C(18) column using methanol-water-glacial acetic acid (70:30:0.2, v/v/v) as the mobile phase. The method is linear for drug concentrations in the range of 20-120 microg/mL (r=0.9995). The intra- and inter-day precisions are lower than 1.46% and 2.22%, respectively. The average recovery of the samples at three levels is 99.8%. The results show that derivatization of ethambutol is stable at 30 degrees C for 24 h. This method is simple, rapid, and stable in the presence of common excipients and antituberculosis drugs in the tablets.     

光散射分析技术测定盐酸环丙沙星含量

在pH 4.6的乙酸-乙酸钠缓冲溶液中,环丙沙星能与四苯硼钠作用生成沉淀产生光散射信号(LS)能应用普通荧光分光光度计检测,从而建立了环丙沙星的光散射分析法.LS光谱在385.0 nm处,具有特征散射峰,且增强的光散射强度(ΔILS)与0.03～0.2 μg/mL,0.2～2.5 μg/mL两个范围内的环丙沙星溶液呈线性关系,相对应的检出限分别为7.4,2.7 ng/mL.本实验中研究了酸度、聚乙二醇600溶液的浓度、四苯硼酸钠溶液的浓度以及共存物质对LS强度的影响.方法已用于盐酸环丙沙星片剂中环丙沙星的测定,RSD为0.3%～0.6%.     

Determination of nebivolol hydrochloride and hydrochlorothiazide in tablets by first-order derivative spectrophotometry and liquid chromatography

Two simple and accurate methods for analysis of nebivolol hydrochloride (NEB) and hydrochlorothiazide (HCTZ) in their combined dosage forms were developed using first-order derivative spectrophotometry and reversed-phase liquid chromatography (LC). NEB and HCTZ in their combined dosage forms (tablets) were quantified using first-derivative responses at 294.6 and 334.6 nm in the spectra of their solutions in methanol. The calibration curves were linear in the concentration range of 8-40 microg/mL for NEB and 10-60 microg/mL for HCTZ. LC analysis was performed on a Phenomenex Gemini C18 column (250 x 4.6 mm id, 5 microm particle size) in the isocratic mode with 0.05 M potassium dihydrogen phosphate-acetonitrile-methanol (30 + 20 + 50, v/v/v; pH 4) mobile phase at a flow rate of 1 mL/min. Detection was made at 220 nm. Both of the drugs and the internal standard (ezetimibe) were well resolved with retention times of 5.1 min for NEB, 2.9 min for HCTZ, and 8.2 min for ezetimibe. The calibration curves were linear in the concentration range of 1-14 microg/mL for NEB and 0.3-28 microg/mL for HCTZ. Both methods were validated and found to be accurate, precise, and specific, and results were compared statistically. Developed methods were successfully applied for the estimation of NEB and HCTZ in their combined dosage forms.     

微流控芯片非接触电导检测法测定药片中盐酸奈福泮

建立了微流控芯片非接触电导检测法测定片剂中盐酸奈福泮含量的方法.探讨并优化了缓冲溶液种类和配比、添加剂、分离电压和进样时间等电泳分离条件.结果表明,以2mmol/L HAc+1mmol/L NaAc( pH4.5)不加添加剂为运行缓冲溶液,分离电压2.00 kV、进样时间10 s时,1min内可实现盐酸奈福泮快速分离检...     

盐酸二甲双胍的毛细管电泳法快速测定

建立了毛细管电泳高频电导法快速测定片剂中盐酸二甲双胍的方法。考察了缓冲溶液、有机溶剂添加剂、毛细管长度以及分离电压和进样条件等因素对分离检测的影响。在最佳条件下5.0 min内即可实现盐酸二甲双胍分离检测,盐酸二甲双胍的线性范围为1.50μg/mL~130μg/mL,检出限为1.0μg/mL。该方法成功地测定了盐酸二甲双胍片剂中的盐酸二甲双胍。     

微流控芯片毛细管电泳激光诱导荧光检测法测定片剂中盐酸美西律的含量

建立了微流控芯片毛细管电泳激光诱导荧光检测法测定片剂中盐酸美西律含量的方法,对衍生条件和电泳条件进行了系统的考察。盐酸美西律经异硫氰酸荧光素(FITC)40℃衍生6h,以20 mmol/L硼砂为电泳缓冲溶液,进样30s后,分离电压2000V,可在1 min内完成一次检测。方法的检出限为0.022 mg/L、线性范围0.108～1.079 mg/L、相关系数0.994,加标回收率为99.7%～102.3%,方法适用于盐酸美西律的检测和质量控制。     

Determination and validation of duloxetine hydrochloride in capsules by HPLC with pre-column derivatization and fluorescence detection

A high-performance liquid chromatographic (HPLC) method is described for the determination of duloxetine hydrochloride in capsules. The method was based on pre-column derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole using the fluorimetric detection technique. Duloxetine hydrochloride was analyzed by HPLC using an Inertsil C18 column (5 μm, 150 × 4.6 mm) and mobile phase consisted of methanol and water (65:35, v/v). The fluorescence detector was adjusted at excitation and emission wavelengths of 461 and 521 nm, respectively. The linearity of the method was in the range of 10-600 ng/mL. Limits of detection and quantification were 0.51 and 1.53 ng/mL, respectively. The proposed method was successfully applied for determination of duloxetine hydrochloride in its pharmaceutical preparation. The results were in good agreement with those obtained using a reference method.     

Estimation of pioglitazone hydrochloride and metformin hydrochloride in tablets by derivative spectrophotometry and liquid chromatographic methods

Two simple and accurate methods of analysis to determine pioglitazone hydrochloride (PIO) and mefformin hydrochloride (MET) in combined dosage forms were developed using second-derivative spectrophotometry and reversed-phase liquid chromatography (LC). PIO and MET in combined preparations (tablets) were quantified using the second-derivative responses at 227.55 nm for PIO and 257.25 nm for MET in spectra of their solutions in a mixture of methanol and acetonitrile (30 + 70). The calibration curves were linear [correlation coefficient (r) = 0.9984 for PIO and 0.9986 for MET] in the concentration range of 8-40 microg/mL for PIO and 4-12 microg/mL for MET. In the LC method, analysis was performed on a Hypersil ODS-C18 column with 5 microm particle size using the mobile phase acetonitrile-water-acetic acid (75 + 25 + 0.3), adjusted to pH 5.5 with liquor ammonia, at a flow rate of 0.5 mL/min. Measurement was made at a wavelength of 230 nm. Both the drugs were well resolved on the stationary phase, and the retention times were 8.5 min for PIO and 16.0 min for MET. The calibration curves were linear (r = 0.9933 for PIO and 0.9958 for MET) in the concentration range of 4-20 microg/mL for PIO and MET. Both methods were validated, and the results were compared statistically. They were found to be accurate, precise, and specific. The methods were successfully applied to the estimation of PIO and MET in combined tablet formulations.     

Validated HPLC determination of the two fixed dose combinations (chlordiazepoxide hydrochloride and mebeverine hydrochloride; carvedilol and hydrochlorothiazide) in their tablets

Simple, rapid, and selective RP-HPLC methods with UV detection were developed for simultaneous determination of chlordiazepoxide hydrochloride and mebeverine hydrochloride (Mixture I) and carvedilol and hydrochlorothiazide (Mixture II). The chromatographic separation in both mixtures was achieved by using an RP-C8 (octylsilyl) analytical column. For Mixture I, a mobile phase composed of acetonitrile-0.05 M disodium hydrogen phosphate-triethylamine (50 + 50 + 0.2, v/v/v), pH 2.5, was used; the detector wavelength was 247 nm. For Mixture II, the mobile phase consisted of acetonitrile-0.05 M disodium hydrogen phosphate (50 + 50, v/v), pH 4.0, and the detector was set at 220 nm. Quantification of the analytes was based on measuring their peak areas. Both mixtures were resolved in less than 6 min. The reliability and analytical performance of the proposed HPLC procedures were statistically validated with respect to linearity, range, precision, accuracy, selectivity, robustness, LOD, and LOQ. The linear dynamic ranges were 2.5-150 and 2.5-500 microg/mL for chlordiazepoxide HCI and mebeverine HCI, respectively, and 0.25-200 and 0.25-150 microg/mL for carvedilol and hydrochlorothiazide, respectively. The validated HPLC methods were successfully applied to the analysis of their commercial tablet dosage forms, for which no interfering peaks were encountered from common pharmaceutical adjuvants.