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作 者:杨庆芳 YANG Qingfang(Anyang Market Supervision and Evaluation Centre·Anyang Pharmacovigilance Centre,Anyang,Henan,China 455000)
机构地区:[1]河南省安阳市市场监管审评中心·河南省安阳市药物警戒中心,河南安阳455000
出 处:《中国药业》2025年第7期77-80,共4页China Pharmaceuticals
摘 要:目的建立同时测定解毒化瘀丸中橙皮苷、大黄素和大黄酚含量的高效液相色谱法。方法色谱柱为Symmetry C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长分别为284 nm(橙皮苷)、254 nm(大黄素、大黄酚),柱温为30℃,进样量为10μL。结果橙皮苷、大黄素、大黄酚的进样量分别在0.3435~3.4346μg(r=0.9999,n=6)、0.0439~0.4392μg(r=0.9999,n=6)、0.0817~0.8166μg(r=0.9999,n=6)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验结果的RSD均小于2.0%(n=6);平均加样回收率分别为95.92%,93.57%,97.06%,RSD分别为1.62%,1.84%,2.26%(n=6)。3批样品中橙皮苷、大黄素、大黄酚的平均含量分别为2.1000,0.1608,0.3680 mg/g。结论该方法操作简便、结果准确,重复性和稳定性均较好,可用于同时测定解毒化瘀丸中橙皮苷、大黄素、大黄酚的含量,有助于进一步完善其质量标准。Objective To establish a high-performance liquid chromatography(HPLC)method for simultaneous determination of hesperidin,emodin,and chrysophanol in Jiedu Huayu Pills.Methods The chromatographic column was Symmetry C18 column(250 mm×4.6 mm,5µm),the mobile phase was methanol-0.1%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was set at 284 nm for hesperidin and 254 nm for emodin and chrysophanol,the column temperature was 30℃,and the injection volume was 10µL.Results The linear ranges of hesperidin,emodin,and chrysophanol were 0.3435-3.4346µg(r=0.9999,n=6),0.0439-0.4392µg(r=0.9999,n=6),and 0.0817-0.8166µg(r=0.9999,n=6),respectively.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%(n=6).The average recoveries of hesperidin,emodin,and chrysophanol were 95.92%,93.57%,and 97.06%,with RSDs of 1.62%,1.84%,and 2.26%(n=6),respectively.The average contents of hesperidin,emodin,and chrysophanol in the three batches of samples were 2.1000,0.1608,and 0.3680 mg/g,respectively.Conclusion The method is simple,accurate,and has good repeatability and stability,which can be used for the simultaneous determination of hesperidin,emodin,and chrysophanol in Jiedu Huayu Pills.It is helpful to further improve the quality standard of Jiedu Huayu Pills.
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