溃疡油高效液相色谱特征图谱研究及5种成分的含量测定  

Characteristic chromatogram of Kuiyang oil by HPLC and determination of 5 components

作　　者：韩锋 肖宏华 胡妍文 马秉智[2] 刘开玉 HAN Feng;XIAO Hong-hua;HU Yan-wen;MA Bing-zhi;LIU Kai-yu(Food and Drug Safety Monitoring Center of Chaoyang District,Beijing 100124;China-Japan Friendship Hospital,Beijing 100029)

机构地区：[1]北京市朝阳区食品药品安全监控中心,北京100124 [2]中日友好医院,北京100029

出　　处：《中南药学》2021年第7期1420-1424,共5页Central South Pharmacy

摘　　要：目的建立溃疡油的高效液相色谱特征图谱,并同时测定欧前胡素、藁本内酯、异欧前胡素、大黄素、大黄酚的含量。方法采用Waters XBridge C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇(A)-0.2%磷酸溶液(B)为流动相,进行梯度洗脱,采用DAD检测器,检测波长254 nm,流速1.0 mL·min^(-1),柱温40℃。通过10批样品建立特征图谱,对市售的5批样品进行测定。结果初步建立了溃疡油的HPLC特征图谱,确定了13个特征峰,市售各批次与对照图谱相似度均在0.85以上,并对特征峰进行了化学成分的识别及药味归属。5个指标成分欧前胡素、藁本内酯、异欧前胡素、大黄素、大黄酚分别在20.44~510.9 ng(r=0.9999)、33.16~829.0 ng(r=0.9999)、4.119~103.0 ng(r=0.9999)、4.224~105.6 ng(r=0.9999)、8.540~213.5 ng(r=0.9999)与峰面积线性关系良好,平均回收率分别为94.2%、91.0%、109.8%、102.7%、99.2%,RSD分别为0.86%、1.9%、1.0%、2.8%、2.1%(n=6)。结论该方法简便易行、准确可靠,可为溃疡油的质量评价及控制提供参考。Objective To establish the characteristic chromatogram of Kuiyang oil by HPLC and to determine the content of imperatorin,ligustilide,isoimperatorin,emodin and chrysophanol.Methods The HPLC column was Waters XBridge C_(18)(4.6 mm×250 mm,5μm).The mobile phase was methanol(A)-0.2%phosphoric acid(B)with gradient elution,the flow rate was 1.0 mL·min^(-1),the detection wavelength was 254 nm,and the column temperature was 40℃.Characteristic chromatogram was established for 10 batches of samples,and 5 batches of commercially available samples were measured.Results The characteristic chromatogram of Kuiyang oil was established primarily,and 13 peaks were identified,with the similarity of the commercially available batches and the control chromatogram over 0.85.The chemical components of the characteristic peaks were identified and the drug flavor was assigned.The methods achieved good linearity at 20.44-510.9 ng(r=0.9999)for imperatorin,33.16-829.0 ng(r=0.9999)for ligustilide,4.119-103.0 ng(r=0.9999)for isoimperatorin,4.224-105.6 ng(r=0.9999)for emodin,and 8.540-213.5 ng(r=0.9999)for chrysophanol.The average recovery of the 5 components were 94.2%,91.0%,109.8%,102.7%,and 99.2%,with the RSD of 0.86%,1.9%,1.0%,2.8%and 2.1%,respectively(n=6).Conclusion The method is simple,accurate,specific,which can be used for the quality control of Kuiyang oil.

关 键 词：溃疡油 特征图谱 含量测定 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学] R284[医药卫生—药学]