HPLC-CAD法同时测定元胡止痛胶囊中6种生物碱及香豆素类成分的含量  

Simultaneous determination of 6 alkaloids and coumarins in Yuanhu Zhitong capsules by HPLC-DAD

作　　者：邓磊 和明伟 侯连兵[1] DENG Lei;HE Ming-wei;HOU Lian-bing(Department of Pharmacy,Nanfang Hospital,Southern Medical University,Guangzhou 510515;Department of Pharmacy,Yunnan Hospital of Traditional Chinese Medicine,Kunming 650200)

机构地区：[1]南方医科大学南方医院药学部,广州510515 [2]云南省中医医院药学部,昆明650200

出　　处：《中南药学》2019年第1期88-92,共5页Central South Pharmacy

基　　金：云南省科技攻关计划(编号:2015RA080)

摘　　要：目的建立HPLC-CAD法同时测定元胡止痛胶囊中延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素及异欧前胡素的含量,为元胡止痛胶囊的质量控制提供参考。方法采用高效液相色谱法联合电雾式检测器(HPLC-CAD法),色谱柱为Diamonsil C_(18)(250 mm×4.6 mm,5μm),乙腈(A)-0.05%甲酸铵(甲酸调pH至4.0)(B)为流动相,梯度洗脱(0~10 min,15%A;10~25 min,15%~30%A;25~40 min,30%~40%A;40~50 min,40%~70%A),柱温35℃,雾化器温度35℃,体积流量0.8 mL·min^(-1),进样量20μL,测定元胡止痛胶囊中6种生物碱及香豆素类成分的含量。结果延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素及异欧前胡素的质量浓度分别在0.040~1.010μg(r=0.9991)、0.013~0.320μg(r=0.9994)、0.068~1.700μg(r=0.9994)、0.041~1.020μg(r=0.9997)、0.101~2.520μg(r=0.9991)、0.039~0.980μg(r=0.9993)内与峰面积呈良好的线性关系。延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素及异欧前胡素的平均加样回收率分别为98.5%、98.9%、98.3%、99.4%、98.1%和98.7%,RSD(n=6)分别为0.90%、1.4%、0.70%、1.1%、0.70%和0.90%。结论该方法准确、简便、灵敏度高,可用于元胡止痛胶囊中生物碱和香豆素类多成分的质量控制研究。Objective To develop an HPLC-CAD method to simultaneously determine 6 alkaloids and coumarins of dl-tetrahydropalmatine, palmatine, dehydrocorydaline, d-corydaline, imperatorin, and isoimperation in Yuanhu Zhitong capsules, and provide references for its quality control. Methods HPLC-CAD was used, chromatographic separation was performed on a Diamonsil C18 column(250 mm×4.6 mm, 5 μm). Acetonitrile(A)-0.05% ammonium acetate(acetic acid tone pH4.0)(B) was used as the mobile phase for gradient elution(0-10 min, 15% A;10-25 min, 15%-30% A;25-40 min, 30%-40% A;40-50 min, 40%-70% A), the column temperature was maintained at 35 ℃, the nebulization temperature of detector was 35℃, the flow rate was 0.8 mL·min^-1, and injection volume was 20 μL. The 6 components of Yuanhu Zhitong capsules were determined. Results The 6 components were linearity at 0.040-1.010 μg(r = 0.9991), 0.013-0.320 μg(r= 0.9994), 0.068-1.700 μg(r = 0.9994), 0.041-1.020 μg(r = 0.9997), 0.101-2.520 μg(r = 0.9991) and 0.039-0.980 μg(r = 0.9993), respectively. The average recoveries were 98.5%, 98.9%, 98.3%, 99.4%, 98.1% and 98.7%, and the RSDs were 0.90%, 1.4%, 0.70%, 1.1%, 0.70% and 0.90%. Conclusion The method is accurate, convenient and sensitive for the quality control of multicomponent of alkaloids and coumarins in Yuanhu Zhitong capsules.

关 键 词：电雾式检测器 元胡止痛胶囊 生物碱 香豆素 含量测定 

分 类 号：R917[医药卫生—药物分析学]