建立乳块消胶囊中3种活性成分同时检测的RP-HPLC方法  

Establishment of a RP-HPLC method for simultaneous determination of three active components in Rukuaixiao capsule

作　　者：张国民 王宝锋 赵侠 ZHANG Guo-min;WANG Bao-feng;ZHAO Xia(Changge Food and Drug Inspection Institute,Changge 461500,Henan;Xiangcheng Food and Drug Inspection Institute,Xiangcheng 452670,Henan)

机构地区：[1]长葛市食品药品检验所,河南长葛461500 [2]襄城县食品药品检验所,河南襄城452670

出　　处：《中药与临床》2022年第5期24-27,共4页Pharmacy and Clinics of Chinese Materia Medica

摘　　要：目的:研究创建RP-HPLC法检测乳块消胶囊中橙皮苷、丹酚酸B和黄酮苷3种活性成分含量的分析方法。方法:乳块消胶囊样品经95%甲醇溶液提取,0.45μm滤过后,Waters ACQUITY BEH C18液相色谱柱(100 mm×2.1 mm,1.7μm)分离,流速:0.5 mL·min^(-1);检测波长:283 nm;柱温:30℃;进样量:10μL;流动相A:乙腈,流动相B:0.3%磷酸溶液,梯度洗脱,洗脱程序(0~4 min,12%A;4~10 min,12%~48%A;10~12 min,48%~82%A;12~17 min,82%A;17~18 min,82%~12%A;18~22 min,12%A),外标法定量。结果:在上述色谱条件下,黄酮苷、橙皮苷和丹酚酸B分离良好;3种活性成分分别在1.032~103.2μg·mL^(-1)、0.832~83.2μg·mL^(-1)、1.063~106.3μg·mL^(-1)范围内线性关系良好,相关系数均大于0.995;加标回收分别为98.33%、99.68%和96.80%;重复性和精密度RSD均在5.0%以内,供试品溶液在24 h内稳定。结论:此方法具有检测速度快、准确度高等优点,可以用于乳块消胶囊产品的质量控制。Objective:To establish an analytical method for the content determination of three active components including hesperidin,salvianolic acid B and flavone glycoside in Rukuaixiao capsule by RP-HPLC.Method:The Rukuaixiao capsule samples were extracted with 95%methanol solution,filtered with 0.45μm filter membrane,and separated on Waters ACQUITY BEH C18 column(100 mm×2.1 mm,1.7μm)with the flow rate of 0.5 mL·min^(-1).Detection wavelength was set at 283 nm.Column temperate was 30℃with injection volume of 10μL.Gradient elution was carried out with the mobile phase A of acetonitrile solution and mobile phase B of 0.3%phosphoric acidsolution,and the gradient elution program was(0~4 min,12%A;4~10 min,12%~48%A;10~12 min,48%~82%A;12~17 min,82%A;17~18 min,82%~12%A;18~22 min,12%A).External standard method was used for quantitative analysis.Result:Flavonoid glycoside,hesperidin and salvianolic acid B were well separated under the above chromatographic conditions.The three active components showed good linear relationships in the concentration range of 1.032~103.2μg·mL^(-1),0.832~83.2μg·mL^(-1)and 1.063~106.3μg·mL^(-1),respectively.The correlation coefficients were all greater than 0.995.The average recoveries were 98.33%,99.68%and 96.80%,respectively.The relative standard deviations(RSD)of repeatability and precision were within 5.0%(n=6),and the test solutions was stable within 24 hours.Conclusion:This method has the advantages of high detection speed and accuracy,which can be used for the quality control of Rukuaixiao capsule.

关 键 词：HPLC 乳块消胶囊 橙皮苷 丹酚酸B 黄酮苷 

分 类 号：R283.1[医药卫生—中药学]