【摘要】 目的:建立HPLC法测定通痹胶囊中苯甲酰次乌头原碱含量的方法。方法:采用Agela MP C18(4.6mm×250mm,3μm)色谱柱,流动相乙腈-四氢呋喃(25∶15)-0.1mol/L醋酸铵溶液梯度洗脱,流速:1mL/min,检测波长:235nm,柱温:30℃,碱性硅胶柱纯化供试品溶液。结果:柱纯化洗脱流程为正己烷-乙酸乙酯-二乙胺(15∶1∶0.2)洗脱5个柱体积,收集第3、4、5体积洗脱液(3-5部分),再用正己烷-乙酸乙酯-二乙胺(3∶1∶0.4)洗脱4个柱体积,收集洗脱液(6-9部分)。苯甲酰次乌头原碱在85min内可良好分离,且阴性无干扰;进样量在0.408~8.160μg(r=0.9999)呈良好的线性关系;平均回收率为98.11%(RSD值为2.56%)。结论:供试品制备方法及液相检测方法精准、可重复,适用于通痹胶囊中苯甲酰次乌头原碱的含量测定。更多还原

【Abstract】 Objective: To establish an HPLC method for simultaneous determination of benzoylhypacoitine in Tongbi Capsule. Methods: Agela MP C18(4.6 mm×250 mm, 3μm) was used as chromatographic separation column, and acetonitriletetrahydrofuran(25∶15)-0.1 mol/L ammonium acetate solution(gradient elution) was used as the mobile phase. The detection wavelength was set at 235 nm. The flow rate was 1.0 mL/min and the column temperature was set at 30℃ and the sample solution separated by column chromatograph. Results: The sample solution eluted firstly by hexane-ethyl acetate-diethylamine(15∶1∶0.2) five given column volumes and the 3-5 volume was collected as the first section, secondly, eluted by hexane-ethyl acetatediethylamine(3∶1∶0.4)four given column volumes and the 6-9 volume was collected as the second section. Benzoylhypacoitine was linear in the range of 0.408~8.160μg(r=0.9999). The average recoveries was 98.11% with relative standard deviation(RSD) being 2.56%. Conclusion: The established method for the treatment and detection of the test solution was accurate and reproducible, it could be used to determine the content of benzoylhypacoitine in Tongbi Capsule.更多还原