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用于药物制剂中舒马曲坦琥珀酸盐分析的稳定指示胶束电动色谱法。

Stability-indicating micellar electrokinetic chromatography method for the analysis of sumatriptan succinate in pharmaceutical formulations.

机构信息

Unit Kanser MAKNA-USM, Advanced Medical & Dental Institute, Suite 121 & 141, EUREKA Complex, Universiti Sains Malaysia, 11800 Penang, Malaysia.

出版信息

J Pharm Biomed Anal. 2011 Dec 15;56(5):937-43. doi: 10.1016/j.jpba.2011.08.007. Epub 2011 Aug 10.

Abstract

A micellar electrokinetic chromatography method for the determination of sumatriptan succinate in pharmaceutical formulations was developed. The effects of several factors such as pH, surfactant and buffer concentration, applied voltage, capillary temperature, and injection time were investigated. Separation took about 5 min using phenobarbital as internal standard. The separation was carried out in reversed polarity mode at 20 °C, 26 kV and using hydrodynamic injection for 10s. Separation was achieved using a bare fused-silica capillary 50 μm×40 cm and background electrolyte of 25 mM sodium dihydrogen phosphate-adjusted with concentrated phosphoric acid to pH 2.2, containing 125 mM sodium dodecyl sulfate and detection was at 226 nm. The method was validated with respect to linearity, limits of detection and quantification, accuracy, precision and selectivity. The calibration curve was linear over the range of 100-2000 μg mL(-1). The relative standard deviations of intra-day and inter-day precision for migration time, peak area, corrected peak area, ratio of corrected peak area and ratio of peak area were less than 0.68, 3.48, 3.28, 2.97 and 2.83% and 2.01, 5.50, 4.46, 4.92 and 4.07%, respectively. The proposed method was successfully applied to the determinations of the analyte in tablet. Forced degradation studies were conducted by introducing a sample of sumatriptan succinate standard solution to different forced degradation conditions using neutral (water), basic (0.1 M NaOH), acidic (0.1 M HCl), oxidative (10% H(2)O(2)) and photolytic (exposure to UV light at 254 nm for 2 h). It is concluded that the stability-indicating method for sumatriptan succinate can be used for the analysis of the drug in various samples.

摘要

建立了一种胶束电动毛细管色谱法测定药物制剂中舒马曲坦琥珀酸盐的方法。考察了 pH 值、表面活性剂和缓冲液浓度、外加电压、毛细管温度和进样时间等多种因素的影响。以苯巴比妥为内标,分离约 5 min。在 20°C、26 kV 下,采用反相极性模式,以 10 s 的水力进样进行分离。采用 50 μm×40 cm 熔融石英毛细管,以 25 mM 磷酸二氢钠为背景电解质,用浓磷酸调至 pH 2.2,含 125 mM 十二烷基硫酸钠,检测波长为 226nm。该方法在线性、检测限和定量限、准确度、精密度和选择性方面均得到验证。校准曲线在 100-2000μg mL(-1)范围内呈线性。迁移时间、峰面积、校正峰面积、校正峰面积比和峰面积比的日内和日间精密度的相对标准偏差均小于 0.68%、3.48%、3.28%、2.97%和 2.83%,分别为 2.01%、5.50%、4.46%、4.92%和 4.07%。该方法成功应用于片剂中分析物的测定。通过将舒马曲坦琥珀酸盐标准溶液样品引入不同的强制降解条件(中性(水)、碱性(0.1 M NaOH)、酸性(0.1 M HCl)、氧化(10% H(2)O(2))和光解(在 254 nm 紫外光下暴露 2 h)),对舒马曲坦琥珀酸盐进行了强制降解研究。结果表明,该方法可用于各种样品中舒马曲坦琥珀酸盐的分析。

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