金银花炮制前后咖啡酰奎宁酸类成分变化

目的 建立炒金银花和金银花炭中咖啡酰奎宁酸类成分的含量测定方法,研究金银花炮制前后咖啡酰奎宁酸类成分的含量变化。方法 确定提取方法、检测波长、流动相组成等色谱条件,并且考察了所建立分析方法专属性、线性、耐用性、重复性、回收率和精密度。结果 采用提取溶剂为体积分数50%甲醇,料液比为1∶200,超声提取30 min。含量测定采用高效液相色谱法,色谱柱为十八烷基硅烷键合硅胶(柱长为250 mm,内径为4.6 mm,粒径为5 μm)为填充剂;以乙腈为流动相A,以0.4％磷酸溶液为流动相B,梯度洗脱;柱温为30 ℃;流速为1.0 mL·min^-1;检测波长为327 nm。新绿原酸、绿原酸、隐绿原酸、3,4-O-二咖啡酰奎宁酸、3,5-O-二咖啡酰奎宁酸、4,5-O-二咖啡酰奎宁酸的专属性、线性、耐用性、重复性、回收率和精密度均符合要求。结论 该方法操作简单,可用于炒金银花、金银花炭中6种酚酸类成分含量的同时测定。6种咖啡酰奎宁酸在金银花炮制前后含量、比例变化显著,为其炮制工艺、质量控制和活性研究等提供了依据。

Changes of Caffeoylquinic Acids in Crude and Processed Lonicera japonica

OBJECTIVE To establish a method for determination of caffeoylquinic acids in processed products of Lonicera japonica, and to study the content changes of caffeoylquinic acids in crude and processed L. japonica. METHODS The chromatographic conditions such as extraction method, detection wavelength, and mobile phase composition were determined, and the specificity, linearity, durability, repeatability, recovery, and precision of the established analytical method were investigated. RESULTS The extraction solvent was 50% methanol, the solid-liquid ratio was 1∶200, and ultrasonic extraction was carried out for 30 minutes. The content was determined by HPLC, the column was ostade-cylsilane column(250 mm×4.6 mm, 5 μm), the mobile phase was acetonitrile(A)-0.4% phosphoric acid solution(B) by gradient elution, the detection wavelength was set at 327 nm. The specificity, linearity, durability, repeatability, recovery, and precision of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, 3,4-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid, and 4,5-O-dicaffeoylquinic acid meet corresponding requirements. CONCLUSION The method is simple, and can be used for simultaneous determination of 6 phenolic acids in processed products of L. japonica Furthermore. It is found that the contents and ratio of 6 caffeoylquinic acids changed significantly before and after processed, which provides a basis for the study of processing technology, quality control, and activity researches of L. japonica.