超高效液相色谱法同时测定伤科跌打片大黄中5种游离蒽醌含量  

Simultaneous Determination of Five Free Anthraquinones in Rhei Radix et Rhizoma from Shangke Dieda Tablets by UPLC

作　　者：唐雪婷 王兆琦 田金苗 孔令锋 周春玲 TANG Xueting;WANG Zhaoqi;TIAN Jinmiao;KONG Lingfeng;ZHOU Chunling(Liaoning Inspection,Examination and Certification Centre,Shenyang,Liaoning,China 110036;Shenyang Pharmaceutical University,Shenyang,Liaoning,China 110016)

机构地区：[1]辽宁省检验检测认证中心,辽宁沈阳110036 [2]沈阳药科大学,辽宁沈阳110016

出　　处：《中国药业》2025年第7期65-68,共4页China Pharmaceuticals

基　　金：2023年国家药品评价性抽验项目[67]。

摘　　要：目的建立伤科跌打片大黄中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚含量的超高效液相色谱法。方法色谱柱为Agilent Poroshell 120 SB-C18柱(100 mm×4.6 mm,2.7μm),流动相为甲醇-0.1%磷酸溶液(85∶15,V/V),流速为1.6 m L/min,柱温为30℃,检测波长为254 nm,进样量为2μL。结果芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的质量浓度分别为0.3775~56.6280μg/mL、0.4683~70.2448μg/mL、0.4381~65.7216μg/mL、0.4314~64.7094μg/mL、0.1647~24.7092μg/m L范围内与峰面积线性关系良好(r=0.9999,n=6);精密度、稳定性、重复性试验结果的RSD均小于2.5%(n=6);平均加样回收率分别为97.11%,102.73%,105.00%,96.30%,105.12%,RSD分别为1.28%,1.69%,1.87%,1.81%,1.16%(n=6)。10家企业生产的74批伤科跌打片的上述5种成分的平均总含量为每片0.59 mg,高于限度每片0.24 mg。结论该方法操作简便快速、结果准确,可用于伤科跌打片的质量控制。Objective To establish an ultra-high performance liquid chromatography(UHPLC)method for the simultaneous determination of aloe-emodin,rhein,emodin,chrysophanol,and physcion in Rhei Radix et Rhizoma from Shangke Dieda Tablets.Methods The chromatographic column was Agilent Poroshell 120 SB-C18 column(100 mm×4.6 mm,2.7µm),the mobile phase was methanol-0.1%phosphoric acid solution(85∶15,V/V),the flow rate was 1.6 mL/min,the column temperature was 30℃,the detection wavelength was 254 nm,and the injection volume was 2µL.Results The linear ranges of aloe-emodin,rhein,emodin,chrysophanol,and physcion were 0.3775–56.6280µg/mL,0.4683-70.2448µg/mL,0.4381-65.7216µg/mL,0.4314-64.7094µg/mL,and 0.1647-24.7092µg/mL(r=0.9999,n=6),respectively.The RSDs of precision,stability,and repeatability tests were all lower than 2.5%(n=6).The average recoveries of aloe-emodin,rhein,emodin,chrysophanol,and physcion were 97.11%,102.73%,105.00%,96.30%,and 105.12%,with RSDs of 1.28%,1.69%,1.87%,1.81%,and 1.16%(n=6),respectively.The average total content of the five components in 74 batches of Shangke Dieda Tablets from 10 manufacturers was 0.59 mg/tablet,exceeding the specified limit of 0.24 mg/tablet.Conclusion The method is simple,rapid,and accurate,which can be used for quality control of Shangke Dieda Tablets.

关 键 词：超高效液相色谱法 伤科跌打片 大黄 芦荟大黄素 大黄酸 大黄素 大黄酚 大黄素甲醚 含量测定 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0