HPLC法同时测定颠茄片5个指标成分含量及特征图谱分析  

Study on simultaneous determination of five main marker components in belladonna tablets and fingerprint analysis by HPLC

作　　者：张文婷[1] 高杰[1] 岳超[1] 黄伟[2] 赵维良[1] 

机构地区：[1]浙江省食品药品检验所,杭州310004 [2]浙江医学高等专科学校,杭州310053

出　　处：《药物分析杂志》2014年第12期2154-2159,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：建立不同生产企业颠茄片中5个指标成分的含量和专属的颠茄片特征图谱检测方法。方法：采用Welch XB-C18（250 mm×4.6 mm,5μm）色谱柱,流动相为甲醇-0.05%磷酸,梯度洗脱,流速1.0 m L·min^-1,检测波长344 nm柱温30℃。结果：5个指标成分东莨菪苷、绿原酸、山柰素-3-O-半乳糖-（6→1）鼠李糖-7-O-葡萄糖苷、东莨菪内酯和芦丁在含量分析测定条件下,各组分分离,线性范围分别为32.60-978.0、10.00-300.0、31.90-957.0、36.3-1089和10.10-303.0 ng,加样回收率在97.6%-99.7%之间;在特征图谱研究中,以东莨菪内酯为参照峰,标定了16个共有峰,分析的13批颠茄片与共有模式之间有良好的相似性,相似度在0.9以上。结论：建立的含量测定及特征图谱分析方法灵敏度高、结果准确、专属性强,可用于颠茄片的质量控制。Objective： To establish a simultaneous determination of five main marker components and specific HPLC fingerprint method for the quality evaluation of belladonna tablets from different manufactories. Methods： A Welch XB - Clscolumn（250 mm ×4. 6 mm,5 μm） was adopted with methanol -0.05% phosphoric acid as the mo- bile phase for gradient elution at a flow rate of 1.0 mL ·min-t ;the detection wavelength was 344 nm and the col- umn temperature was 30 ℃. Results： The result showed that five main marker components （scopolin, chlorogenic acid, kaempferol - 3 - O - -β D （ 6 - O - α - L - rhamnogalactoside ） - 7 - O -β - D - glucoside, scopoletin and turin） were separated well. The correlation coefficients were 0. 9998,0. 9996,0. 9995,0. 9994 and,0. 9994 respec- tively,the linear ranges of five components were 32.60 - 978. 0, 10. 00 - 300.0 ng,31.90 - 957.0,36.30 - 1089 ng and 10. 10 -303.0 ng, respectively, and the average recoveries ranged from 97.6% to 99.72%. Totally 16 com- mon peaks were calibrated with scopoletin as the reference peak. There were good similarities between the standard fingerprint chromatogram and each fingerprint chromatogram of the thirteen samples with their similarity coefficients no less than 0. 9. Conclusion： The method is fast, accurate, sensitive and suitable for the quality control of bella- donna tablets.

关 键 词：颠茄片 东莨菪苷 绿原酸 山柰素-半乳糖-鼠李糖-葡萄糖苷 东莨菪内酯 芦丁 指标成分 特征图谱 高效液相色谱 

分 类 号：R283.6[医药卫生—中药学]