中心切割-二维液相色谱分离清热解毒片(胶囊)中的咖啡酰奎宁酸类成分  

Separation of Caffeoylquinic acids in Qingrejiedu tablets( capsules) by Central-cutting Two-dimensional HPLC

作　　者：国金玲 连云岚 张远芳 郭景文 

机构地区：[1]山西中医药大学,太原030024 [2]山西省食品药品检验所,太原030001

出　　处：《中国药品标准》2017年第6期449-454,共6页Drug Standards of China

摘　　要：目的:讨论清热解毒片(胶囊)中三个咖啡酰奎宁酸类成分的分离及含量分析方法。方法:采用在线的中心切割-二维液相色谱系统解决中药复方中某些由于灵敏度低或者受高浓度组分信号的覆盖而无法分离和定量的问题。双梯度二维液相色谱系统与VWD和DAD联用,一维色谱柱为美国赛默飞公司Accucore C_(18)柱(2.1 mm×100 mm,2.6μm)粒径,二维色谱柱为富士填料的自装C18柱(3 mm×150 mm,3μm)。两维流动相均为乙腈和0.4%磷酸水(含0.1%的三氟乙酸),流速分别为0.4 m L·min^(-1)和1 mL·min^(-1),柱温35℃。结果:3,4-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸及4,5-二咖啡酰奎宁酸的线性范围分别为12.109~0.484 mg·L^(-1)(r=0.9998);2.431~0.24 3 mg·L^(-1)(r=0.9993);0.655~0.131 mg·L^(-1)(r=0.9991)。三个分析物的平均回收率在98.41%~98.16%范围内。且含量测定结果显示:4种剂型(包括硬胶囊、软胶囊、糖衣片、薄膜衣片)的含量均在0.0108~0.4831 mg·g^(-1)范围内。结论:该方法使得清热解毒片(胶囊)中的三个分析物的分离效果得到明显改善,同时在对成分复杂的中药复方制剂的分离纯化方面发挥了重要作用。Abstract：Objective： To estabish a method for determination and separation of three caffeoylquinic acids in qingrejiedu tablets（capsules）.Methods： Use the on-line center cutting two-dimensional liquid chromatography system to solve some problems in traditional Chinese medicine compounds that can not be separated and quantified due to low sensitivity or the coverage of other high concentration components.A dual gradient two-dimensional liquid chromatography system is coupled with a UV detector and an DAD detector,2D-HPLC system was used Columns of two dimensions were thermo of US AccucoreC18column（2.1mm×100mm,2.6μm）and Self filling of Fuji packing C18column（3mm×150mm,3μm） respectively. Separation of both dimensions were performed with the mobile phase of Acetonitrile and 0.4% Phosphoric（contain0.1%TFA）.Flow rate was set at 0.4mL·min-1and 1mL·min-1 ,column temperature was set at30℃.Results： The linear range for 3,4-Dicaffeoylquinic acid,3,5-Dicaffeoyiquinic acid and 4,5-Dicaffeoylquinic acid were12.109？0.484mg·L-1,2.431？0.243mg·L-1and0.655？0.131mg·L-1 respectively,and the r were 0.9998,0.9993,0.9991 respectively. The average recoveries within 98.41%？98.16% respectively.Conclusions：The separation of qingrejiedu tablets（capsules） separation has been substantially improved by the method,and it has play important role in the separation and purification of traditional Chinese herbal medicine. Key Words：heart-cut two dimensional liquid chromatography ;qingrejiedu tablets（c apsules） ;caffeoylquinic acids

关 键 词：中心切割-二维液相色谱 清热解毒片(胶囊) 咖啡酰奎宁酸类成分 

分 类 号：R921.2[医药卫生—药学]