基于多成分定量分析结合薄层色谱检查的颠茄流浸膏质量评价

Quality Evaluation of Belladonna Liquid Extract by Multicomponent Quantitation and TLC

关键词:  颠茄流浸膏  东莨菪苷  山柰酚-3-O-半乳糖-(6→1)鼠李糖-7-O-葡萄糖苷  东莨菪内酯  芦丁  硫酸阿托品

Key words:  Belladonna liquid extract  scopolin  kaempferol-3-O-galactosyl (6→1)-rhamnosyl-7-O-glucoside  scopoletin  rutin  atropine sulfate

摘要:

目的 建立颠茄流浸膏中同时测定4种指标成分含量的方法，结合薄层色谱检查，为其质量评价提供依据。方法 采用HPLC，色谱柱：Agilent Kromesil100-5 C₁₈柱（4.6 mm×250 mm，5 μm），流动相为甲醇-0.05%甲酸溶液，梯度洗脱，流速1.0 mL·min^-1，柱温为30℃。采用薄层色谱法进行阿托品检查。结果 4种活性成分东莨菪苷在0.065 76~0.657 6 μg （r=1.000 0）、山柰酚-3-O-半乳糖-（6→1）鼠李糖-7-O-葡萄糖苷在0.082 16~0.821 6 μg （r=0.9999）、东莨菪内酯在0.049 84~0.498 4 μg （r=1.0000）和芦丁在0.010 00~0.099 98μg （r=0.999 9）内，均呈良好线性关系；东莨菪苷、山柰酚-3-O-半乳糖-（6→1）鼠李糖-7-O-葡萄糖苷、东莨菪内酯和芦丁的加样回收率分别为100.6%，99.8%，99.9%和97.9%，RSD分别为1.4%，1.6%，1.4%和1.5%。部分批次指标成分含量低且检出硫酸阿托品。结论 建立的含量测定方法灵敏度高，结果准确，适用于颠茄流浸膏的质量评价。

Abstract:

OBJECTIVE To establish a method of the simultaneous determination of 4 components in Belladonna liquid extract, provide the basis for its quality evaluation by combing with TLC. METHODS Adopting HPLC and using Agilent Kromesil 100-5 C₁₈ chromatographic column(4.6 mm×250 mm, 5 μm), the mobile phase was a mixture of acetonitrile and 0.05% formic acid for gradient elution. The flow rate was 1.0 mL·min^-1. The temperature of column was 30℃. Atropine sulfate was identified with TLC method. RESULTS Four active ingredients had good linear relationships:scopolin was in the range of 0.065 76-0.657 6 μg(r=1.000 0), kaempferol-3-O-galactosyl(6→1)-rhamnosyl-7-O-glucoside was in the range of 0.082 16-0.821 6 μg(r=0.999 9), scopoletin was in the range of 0.049 84-0.498 4 μg(r=1.000 0) and rutin was in the range of 0.010 00-0.099 98 μg(r=0.999 9). The average recoveries of scopolin, kaempferol-3-O-galactosyl(6→1)-rhamnosyl-7-O-glucoside, scopoletin and rutin were 100.6%, 99.8%, 99.9% and 97.9%. And their RSDs were 1.4%, 1.6%, 1.4% and 1.5%. The contents of some ingredients were low and atropine sulfate was detected in some samples. CONCLUSION This method has high sensitivity, it is accurate and suitable for the quality control of Belladonna liquid extract.