伤科跌打片UPLC指纹图谱及10个成分含量测定研究  

Study on UPLC fingerprint of Shangke Dieda tablets and determination of ten components

作　　者：田金苗 张旭 周楠 唐雪婷 孔令锋 周春玲 TIAN Jinmiao;ZHANG Xu;ZHOU Nan;TANG Xueting;KONG Lingfeng;ZHOU Chunling(Liaoning Inspection,Examination&Certification Centre,Liaoning Institute for Drug Control,Shenyang 110036,China)

机构地区：[1]辽宁省检验检测认证中心/辽宁省药品检验检测院,沈阳110036

出　　处：《药学前沿》2025年第2期218-226,共9页China Pharmacist

基　　金：2023年国家药品评价性抽验项目。

摘　　要：目的为了更好控制产品质量,建立伤科跌打片的超高效液相色谱(UPLC)指纹图谱,同时测定芍药苷、柚皮苷、橙皮苷、新橙皮苷、木香烃内酯、去氢木香内酯、芦荟大黄素、大黄酸、大黄素和大黄素甲醚10种成分的含量。方法采用Agilent InfinityLab Poroshell 120 SB-C18色谱柱(100 mm×4.6 mm,2.7μm),以乙腈和0.1%磷酸溶液为流动相,梯度洗脱,流速为1.0 mL/min,柱温为30℃,检测波长为230 nm,进样量为5μL。建立伤科跌打片的UPLC指纹图谱,采用中药色谱指纹图谱相似度评价软件对10个生产企业74批伤科跌打片进行相似度评价,测定伤科跌打片10种成分的含量。结果伤科跌打片UPLC指纹图谱共标定出10个共有峰,74批伤科跌打片的相似度在0.85~0.99范围内。芍药苷、柚皮苷、橙皮苷、新橙皮苷、木香烃内酯、去氢木香内酯、芦荟大黄素、大黄酸、大黄素和大黄素甲醚的线性关系良好,r均≥0.9998,平均回收率在97.0%~105.1%范围内,RSD为0.4%~2.0%(n=6)。74批伤科跌打片中这10种成分的含量分别为:0.028~0.653、0.042~0.931、0.591~3.978、0.021~0.593、0~0.157、0.009~0.231、0.006~0.078、0.022~0.593、0.029~0.143、0.035~0.132 mg/片。结论成功建立伤科跌打片的UPLC指纹图谱,为伤科跌打片的质量评价提供依据,同时测定10个成分含量的方法操作简便,结果准确可靠。Objective To establish an ultra-high performance liquid chromatography(UPLC)fingerprint for Shangke Dieda tablets,in order to better control product quality,and to determine the contents of 10 components including paeoniflorin,naringin,hesperidin,neohesperidin,lignan lactone,dehydrolignan lactone,aloe emodin,rhein,emodin,and emodin methyl ether simultaneously.Methods The chromatographic separation was performed on a Agilent InfinityLab Poroshell 120 SB-C18 column(100 mm×4.6 mm,2.7μm).Acetonitrile-0.1% phosphoric acid aqueous solution was used as mobile phase for gradient elution,the flow rate was 1.0 mL/min,the column temperature was 30℃,the detection wavelength was 230 nm and the sample amount was 5μL.The UPLC fingerprints of Shangke Dieda tablets were established,the similarity of 74 batches of Shangke Dieda tablets from 10 production enterprises were evaluated using traditional Chinese medicine chromatographic fingerprint similarity evaluation software,and the content of 10 components in Shangke Dieda tablets were determined.Results The results showed that a total of 10 common peaks were identified in the UPLC fingerprint of Shangke Dieda tablets,and the similarity of 74 batches of Shangke Dieda tablets were at the range of 0.85 to 0.99.The linear relationships of paeoniflorin,naringin,hesperidin,neohesperidin,lignan lactone,dehydrolignan lactone,aloe emodin,rhein,emodin,and emodin methyl ether were good,with r≥0.9998.The average recovery rate was in the range of 97.0% to 105.1%,with RSD of 0.4%to 2.0%(n=6).The contents of these 10 components in 74 batches of Shangke Dieda tablets were as follows:0.028-0.653,0.042-0.931,0.591-3.978,0.021-0.593,0-0.157,0.009-0.231,0.006-0.078,0.022-0.593,0.029-0.143 and 0.035-0.132 mg/tablet.Conclusion The UPLC fingerprint for Shangke Dieda tablets was established successfully,which can provide a basis for the quality evaluation of Shangke Dieda tablets.The method of simultaneously determining the content of 10 components is easy to operate and the results are accurate a

关 键 词：伤科跌打片 指纹图谱 含量测定 超高效液相色谱 白芍 木香 枳壳和青皮 大黄 

分 类 号：R286.0[医药卫生—中药学]