RP-HPLC法同时测定五味清浊散中3种成分的含量  

RP-HPLC for determining the contents of three kind of ingredients in Wuwei Qingzhuo powder

作　　者：李柯 杨蕾 孟令嘉 刘炜 LI Ke;YANG Lei;MENG Ling-jia;LIU Wei(Intravenous Drug Distribution Center,Beijing Shijitan Hospital Affiliated to Capital Medical University,Beijing 100038,China)

机构地区：[1]首都医科大学附属北京世纪坛医院静脉用药调配中心,北京100038

出　　处：《实用药物与临床》2020年第8期744-747,共4页Practical Pharmacy and Clinical Remedies

摘　　要：目的研究建立利用RP-HPLC法同时测定五味清浊散中活性成分山柰素、桂皮醛和胡椒碱含量的分析方法。方法五味清浊散供试品经研细、混匀,75%甲醇溶液超声提取后,Agilent zorbax XDB-C 18色谱柱分离,柱温:30℃;流速:1.0 ml/min;检测波长:319 nm;进样量:20μl;流动相:乙腈(A)-0.5%磷酸溶液(B),梯度洗脱,洗脱程序:0~5 min 17%A,5~21 min 17%~43%A,21~29 min 43%~74%A,29~30 min 74%~17%A,30~35 min 17%A。外标法定量检测。结果山柰素、桂皮醛和胡椒碱在浓度0.1~20.0μg/ml范围内具有良好的线性,相关系数(r 2)均大于0.995;重复性RSD(n=6)分别为3.5%、4.2%、2.8%;平均回收率分别为99.29%、100.25%、100.70%。结论本研究建立的方法具有前处理简单、检测结果准确、重复性好等特点,可以用于五味清浊散中活性成分山柰素、桂皮醛和胡椒碱含量的测定。Objective To explore an analytical method for determining the contents of active ingredients(kaempferol,cinnamic aldehyde and piperine)in Wuwei Qingzhuo powder by reverse phase high performance liquid chromatography(RP-HPLC).Methods Wuwei Qingzhuo powder samples were groud and mixed,then extracted in 75%methanol solution by ultrasound.Agilent zorbax XDB-C 18 column was used for seperation,with column temperature being 30℃.The flow rate was 1.0 ml/min,detection wavelength was setted at 319 nm,and injection volume was 20μl.Mobile phase:acetonitrile(A)and 0.5%phosphoric acid solution(B).Gradient elution procedure:0~5 min 17%A,5~21 min 17%~43%A,21~29 min 43%~74%A,29~30 min 74%~17%A,30~35 min 17%A.Quantitative determination was made by external standard method.Results Kaempferol,cinnamic aldehyde and piperine had good linear relationships in the concentration range of 0.1 to 20.0μg/ml,with correlation coefficients(r 2)all greater than 0.995.Relative standard deviation(RSD)of repeatability was 3.5%,4.2%and 2.8%,respectively.Average recoveries of 3 active components were 99.29%,100.25%and 100.70%.Conclusion The method has the advanfage of simple pretreatment,high accuracy and good repeatability,and can be used for the determination of the contents of the active ingredients(kaempferol,cinnamic aldehyde and piperine)in Wuwei Qingzhuo powder.

关 键 词：RP-HPLC 五味清浊散 山柰素 桂皮醛 胡椒碱 

分 类 号：R286.0[医药卫生—中药学]