HPLC法测定并比较茵陈蒿煎剂与其配方颗粒中有效成分的含量  

Contents Determination and Comparison of Active Ingredients in the Yinchenhao Decoction and Its Dispensing Granule by HPLC

作　　者：林伟豪[1] 陈连剑[2] 高崇凯[3] 吴婵娟[1] 

机构地区：[1]深圳市坪山新区人民医院药剂科,广东深圳518118 [2]深圳市第四人民医院药学部,广东深圳518033 [3]广东药科大学药学系,广州510006

出　　处：《中国药房》2016年第15期2102-2106,共5页China Pharmacy

基　　金：广东省中医药强省科研课题(No.20142125)

摘　　要：目的：建立测定茵陈蒿煎剂与其配方颗粒中大黄素、大黄酸、芦荟大黄素、大黄酚、大黄素甲醚、栀子苷、绿原酸含量的方法,比较茵陈蒿煎剂与其配方颗粒中上述成分含量的差异。方法：采用高效液相色谱法（HPLC）测定煎剂中大黄素、大黄酸、芦荟大黄素、大黄酚、大黄素甲醚的含量：色谱柱为Ecosil C18,流动相为乙腈-0.5%磷酸（梯度洗脱）,流速为1 ml/min,检测波长为254nm,柱温为35℃,进样量为20μl;采用HPLC法测定煎剂中栀子苷的含量：色谱柱为Ecosil C18,流动相为乙腈-水（13∶87,V/V）,流速为1 ml/min,检测波长为238 nm,柱温为35℃,进样量为20μl;采用HPLC法测定煎剂中绿原酸的含量：色谱柱为Ecosil C18,流动相为乙腈-0.05%磷酸（10∶90,V/V）,流速为1 ml/min,检测波长为327 nm,柱温为35℃,进样量为20μl。结果：大黄素、大黄酸、芦荟大黄素、大黄酚、大黄素甲醚、栀子苷、绿原酸检测质量浓度线性范围分别为2-20μg/ml（r=0.996 5）、5.2-52.0μg/ml（r=0.998 5）、2.6-26.0μg/ml（r=0.999 9）、1.0-10.4μg/ml（r=0.999 9）、1.0-10.0μg/ml（r=0.999 8）、20-200μg/ml（r=0.999 9）、20-200μg/ml（r=0.999 9）;精密度、稳定性、重复性试验的RSD〈3%;回收率分别为91.1%-96.9%（RSD=2.0%,n=6）、93.9%-96.1%（RSD=0.8%,n=6）、90.9%-93.4%（RSD=1.2%,n=6）、88.5%-92.7%（RSD=1.8%,n=6）、82.1%-87.9%（RSD=2.5%,n=6）、100.4%-102.0%（RSD=0.7%,n=6）、101.1%-102.2%（RSD=0.4%,n=6）。结论：该方法操作简便、稳定、重复性好,可用于茵陈蒿煎剂与其配方颗粒中有效成分含量的同时测定。茵陈蒿配方颗粒有效成分含量明显高于其煎剂。OBJECTIVE：To establish a method for the contents determination of emodin,rhein,aloe-emodin,chrysophanol,physcion,geniposide,chlorogenic acid in Yinchenhao decoction and its dispensing granule,and to compare the difference among the above-mentioned ingredients. METHODS：HPLC was adopted to determine the contents of emodin,rhein,aloe-emodin,chrysophanol and physcion：the column was Ecosil C18 with mobile phase of acetonitrile-0.5% phosphoric acid（gradient elution）at a flow rate of 1 ml/min,the detection wavelength was 254 nm,column temperature was 35 ℃,and injection volume was 20 μl.When determining the content of geniposide by HPLC,the column was Ecosil C18 with mobile phase of acetonitrile- water（13 ∶ 87,V/V）at a flow rate of 1 ml/min,the detection wavelength was 238 nm,column temperature was 35 ℃,and injection volume was20 μl. When determining the content of chlorogenic acid by HPLC,the column was Ecosil C18 with mobile phase of acetonitrile-0.5% phosphoric acid（10 ∶ 90,V/V）at a flow rate of 1 ml/min,the detection wavelength was 327 nm,column temperature was35 ℃,and injection volume was 20 μl. RESULTS：The linear range was 2-20 μg/ml for emodin（r=0.996 5）,5.2-52.0 μg/ml for rhein（r=0.998 5）,2.6-26.0 μg/ml for aloe-emodin（r=0.999 9）,1.0-10.4 μg/ml for chrysophanol（r=0.999 9）,1.0-10.0 μg/ml for physcion（r=0.999 8）,20-200 μg/ml for geniposide（r=0.999 9）,20-200 μg/ml for chlorogenic acid（r=0.999 9）;RSDs of precision,stability and reproducibility tests were lower than 3%;recoveries were 91.1%-96.9%（RSD=2.0%,n=6）for emodin、93.9%-96.1%（RSD=0.8%,n=6）for rhein、90.9%-93.4%（RSD=1.2%,n=6）for aloe-emodin、88.5%-92.7%（RSD=1.8%,n=6）for chrysophanol、82.1%-87.9%（RSD=2.5%,n=6）for physcion,100.4%-102.0%（RSD=0.7%,n=6）for geniposide、101.1%-102.2%（RSD=0.4%,n=6）for chlorogenic acid. CONCLUSIONS：The method is simple,stable and reproducible,and can be used for the simultaneous contents determination of active ingredients in Yinchenhao

关 键 词：茵陈蒿煎剂 配方颗粒 高效液相色谱法 

分 类 号：R927[医药卫生—药学]