目的测定香丹注射液中丹参素钠、原儿茶醛和丹酚酸B的含量。方法采用反相高效液相色谱法分析．色谱柱为Diamnsil C18（250mm x 4．6ram，5vm），流动相为0．1％冰醋酸-乙腈（90：10），流速为1．0mL·min-1，检测波长为280nm。结果...目的测定香丹注射液中丹参素钠、原儿茶醛和丹酚酸B的含量。方法采用反相高效液相色谱法分析．色谱柱为Diamnsil C18（250mm x 4．6ram，5vm），流动相为0．1％冰醋酸-乙腈（90：10），流速为1．0mL·min-1，检测波长为280nm。结果丹参素钠、原儿茶醛和丹酚酸B分别在S．06～101．10vg·mL-1、5．60～111．90ug·mL-1。和5．43～108．50utg·mL-1。的求度范围内有较好的线性关系．加样回收率分别为102．4796、98．36％和99．71％。结论该方法简便、准确、重复性好，并为该制荆的质量控制提供了依据。展开更多
Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulat...Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulation. The drug separation was performed on Hibar-240, Li-chrosphere-100 C18 ODS (250 × 4.6 mm, 5 μm) column, at a flow rate of 1 mL/min. The mobile phase used was a mixture of methanol: potassium di-hydrogen phosphate buffer at a ratio of 70:30 v/v. The detection was carried out at a wavelength of 266 nm. The retention times of sitagliptin phosphate and metformin hydrochloride were found as 6.1 and 4.9 min respectively. Linear calibration curves with good correlation coefficients were obtained over the concentration ranges of 10 - 50 μg/mL for sitagliptin and 20 - 100 μg/mL for metformin. The limit of detection was 0.016 and 0.14 μg/mL and the limit of quantification was 0.048 and 0.42 μg/mL for sitagliptin phosphate and metformin hydrochloride respectively. Validation of the method demonstrated system selectivity, specificity, linearity, accuracy and precision. The developed method was found useful in the simultaneous analysis of sitagliptin phosphate and metformin hydrochloride in formulation.展开更多
A simple, precise, accurate stability-indicating gradient reversed-phase high-performance liquid chromatographic （RP-HPLC） method was developed for the quantitative determination of zotepine （ZTP） in bulk and phar...A simple, precise, accurate stability-indicating gradient reversed-phase high-performance liquid chromatographic （RP-HPLC） method was developed for the quantitative determination of zotepine （ZTP） in bulk and pharmaceutical dosage forms in the presence of its degradation products （DPs）. The method was developed using Phenomenex C18 column （250 mm ~ 4.6 mm i.d., 5 mm） with a mobile phase containing a gradient mixture of solvents, A （0.05%trifluoroacetic acid （TFA）, pH ？ 3.0） and B （acetonitrile）. The eluted compounds were monitored at 254 nm;the run time was within 20.0 min, in which ZTP and its DPs were well separated, with a resolution of 41.5. The stress testing of ZTP was carried out under acidic, alkaline, neutral hydrolysis, oxidative, photolytic and thermal stress conditions. ZTP was found to degrade significantly in acidic, photolytic, thermal and oxidative stress conditions and remain stable in basic and neutral conditions. The developed method was validated with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness as per ICH guidelines. This method was also suitable for the assay determination of ZTP in pharmaceutical dosage forms. The DPs were characterized by LC-MS/MS and their fragmentation pathways were proposed.展开更多
文摘目的测定香丹注射液中丹参素钠、原儿茶醛和丹酚酸B的含量。方法采用反相高效液相色谱法分析．色谱柱为Diamnsil C18（250mm x 4．6ram，5vm），流动相为0．1％冰醋酸-乙腈（90：10），流速为1．0mL·min-1，检测波长为280nm。结果丹参素钠、原儿茶醛和丹酚酸B分别在S．06～101．10vg·mL-1、5．60～111．90ug·mL-1。和5．43～108．50utg·mL-1。的求度范围内有较好的线性关系．加样回收率分别为102．4796、98．36％和99．71％。结论该方法简便、准确、重复性好，并为该制荆的质量控制提供了依据。
文摘Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulation. The drug separation was performed on Hibar-240, Li-chrosphere-100 C18 ODS (250 × 4.6 mm, 5 μm) column, at a flow rate of 1 mL/min. The mobile phase used was a mixture of methanol: potassium di-hydrogen phosphate buffer at a ratio of 70:30 v/v. The detection was carried out at a wavelength of 266 nm. The retention times of sitagliptin phosphate and metformin hydrochloride were found as 6.1 and 4.9 min respectively. Linear calibration curves with good correlation coefficients were obtained over the concentration ranges of 10 - 50 μg/mL for sitagliptin and 20 - 100 μg/mL for metformin. The limit of detection was 0.016 and 0.14 μg/mL and the limit of quantification was 0.048 and 0.42 μg/mL for sitagliptin phosphate and metformin hydrochloride respectively. Validation of the method demonstrated system selectivity, specificity, linearity, accuracy and precision. The developed method was found useful in the simultaneous analysis of sitagliptin phosphate and metformin hydrochloride in formulation.
文摘A simple, precise, accurate stability-indicating gradient reversed-phase high-performance liquid chromatographic （RP-HPLC） method was developed for the quantitative determination of zotepine （ZTP） in bulk and pharmaceutical dosage forms in the presence of its degradation products （DPs）. The method was developed using Phenomenex C18 column （250 mm ~ 4.6 mm i.d., 5 mm） with a mobile phase containing a gradient mixture of solvents, A （0.05%trifluoroacetic acid （TFA）, pH ？ 3.0） and B （acetonitrile）. The eluted compounds were monitored at 254 nm;the run time was within 20.0 min, in which ZTP and its DPs were well separated, with a resolution of 41.5. The stress testing of ZTP was carried out under acidic, alkaline, neutral hydrolysis, oxidative, photolytic and thermal stress conditions. ZTP was found to degrade significantly in acidic, photolytic, thermal and oxidative stress conditions and remain stable in basic and neutral conditions. The developed method was validated with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness as per ICH guidelines. This method was also suitable for the assay determination of ZTP in pharmaceutical dosage forms. The DPs were characterized by LC-MS/MS and their fragmentation pathways were proposed.
