摘要
目的建立三黄泻心汤中黄芩苷含量的高效毛细管电泳内标测定方法,比较3种三黄泻心汤不同制备方式样品中黄芩苷含量差异。方法以3,5-二硝基苯甲酸为内标物,熔融石英毛细管柱为分离通道(75μm×53.5 cm,有效长度为45.3 cm);40 mmol·L-1的硼砂(pH=3.0)作为缓冲溶液;DAD检测器,检测波长280 nm;工作电压为15 kV;压力进样:5 kPa,15 s,电解质封口:1 kPa,5 s;柱温15℃;每次进样前用缓冲液冲柱10 min。结果当3,5-二硝基苯甲酸内标溶液的浓度为0.061 0 mg·ml-1时,黄芩苷在4.05~74.89μg·ml-1范围内线性关系良好;通过测定,配方浸膏中黄芩苷含量明显高于传统汤剂和复方浸膏中的含量。结论该方法准确可靠,重复性好,适合复方制剂中黄芩苷的含量测定。从化学成分角度分析,配方浸膏中黄芩苷含量较传统汤剂和复方浸膏存在明显差异,可为临床应用提供科学依据。
Objective To establish a method for the determination of baicalin for three different formulations in Sanhuang Xiexin Decoction by capillary zone electrophoresis, and to compare the content of baiealin in three different formulations. Methods 3,5 - Dinitrobenzoic acid was used as the internal standard with a fused silica capillary （75 μm × 53.5 cm, with effective length of 45. 3 cm）. The analysis was completed in 40 mmol . L^-1 Na2B407 （ pH =3.0） as running buffer at a capillary temperature of 15 ℃ and a vohage of 15 kV. With the DAD detection at wavelength of 280nm , the sample was injected by air pressure injection（ 5 kPa x 15 s） ,and sealed by electrolyte（ 1 kPa x 5 s）. The column was rinsed with buffer solution for 10rain before putting the sample. Results When the concentration of the internal standard 3,5 - Dinitrobenzoic acid was 0. 0610 mg ~ ml-l, the linear responses covered the range from 4.05 - 74.89 p^g ~ ml 1. The content of baicalin in extract recipe was significantly higher than others by the method. Conclusion The method is accurate,reliable and has good repeatability,which is suitable for the determination of the contents of baicalin in the compound. Analyzing from the chemical composition, there was an obvious difference between the con tent of baicalin in extract recipe and others, which can provide scientific basis for clinical application.
出处
《时珍国医国药》
CAS
CSCD
北大核心
2014年第2期279-281,共3页
Lishizhen Medicine and Materia Medica Research
基金
国家自然科学基金(No.30860364)
关键词
三黄泻心汤
黄芩苷
3
5-二硝基苯甲酸内标物
高效毛细管电泳内标法
Sanhuang Xiexin Decoction
Baicalin
3,5 - Dinitrobenzoic acid as the internal standard
High performance capillary eleetrophoresis（HPCE） with internal standard method
