摘要
目的:采用星点设计响应曲面法优选醋焖法炮制白屈菜的最佳炮制工艺。方法:建立原阿片碱、白屈菜碱、盐酸黄连碱、血根碱、小檗碱和白屈菜红碱等6种生物碱成分含量的HPLC法,色谱柱:Kromasil C18(250 mm×4.6 mm,5μm);流动相:0.1%三乙胺(用磷酸调节pH至3.0)-乙腈,梯度洗脱;检测波长:274 nm;流速:1.0 ml·ml^-1;柱温:35℃。以6种生物碱总含量为评价指标,采用响应曲面设计法,考察醋用量、闷润时间、烘干时间和烘干温度对白屈菜醋焖法炮制工艺的影响,确定最佳炮制工艺。结果:原阿片碱等6个对照品在0.640~12.800,1.024~20.480,0.862~17.240,0.436~8.720,0.226~4.520,0.324~6.480μg质量范围内线性关系良好(r值范围0.9997~0.9999),平均加样回收率分别为97.5%,99.4%,100.8%,99.7%,98.9%和98.6%,RSD在1.82%~2.43%之间(n=6)。白屈菜总碱含量提取的最佳工艺条件为:醋用量17%,闷润时间2 h,烘干时间16 h,烘干温度75℃。结论:所建立的白屈菜红碱等6种生物碱含量的HPLC法稳定可行。优选的醋焖法炮制白屈菜炮制工艺方法可行,为白屈菜的进一步研究提供了科学依据。
Objective:To optimize the vinegar processing technology of Chelidonium majus by central composite design-response surface methodology.Methods:An HPLC method for the determination of six alkaloids was established.The column was Komasil C18(250 mm×4.6 mm,5μm).The mobile phase was 0.1%triethylamine(adjusting pH to 3.0 with phosphoric acid).The detection wavelength was 274 nm.The flow rate was 1.0 ml·ml^-1.The column temperature was 35℃.Taking the total content of six alkaloids as the evaluation index,response surface design was used to investigate the influences of vinegar dosage,drenching time,drying time and drying temperature on the vinegar processing technology of cheerkraut to determine the best processing technology.Results:Six reference substances had a good linear relationship in the range of 0.640-12.800,1.024-20.480,0.862-17.240,0.436-8.720,0.226-4.520,0.324-6.480μg.The linear correlation r value of the six control samples was 0.9997-0.9999,and the average recovry was 97.5%,99.4%,100.8%,99.7%,98.9%and 98.6%with the RSDs of 1.82%-2.43%(n=6).The best extraction conditions of the total alkali content were as follows:the amount of vinegar was 17%,the drenching time was 2 hours,the drying time was 16 hours,and the drying temperature was 75℃.Conclusion:The established method for the determination of 6 alkaloids including protoopioids is stable and feasible.The optimum vinegar braising method is feasible,which provides scientific basis for the further study of Chelidonium majus.
作者
赵安敏
李瑞海
贾天柱
Zhao Anmin;Li Ruihai;Jia Tianzhu(Department of Pharmacy,Dandong Hospital of Traditional Chinese Medicine,Liaoning Dandong 118000,China;Liaoning University of Traditional Chinese Medicine)
出处
《中国药师》
CAS
2020年第6期1091-1093,1123,共4页
China Pharmacist
基金
国家药典委员会项目(编号:20180604005)。
关键词
响应面法
白屈菜
生物碱
原阿片碱
白屈菜碱
盐酸黄连碱
血根碱
小檗碱
白屈菜红碱
炮制
醋制
Response surface methodology
Chelidonium majus
Alkaloids
Protopine
Chelidonine
Coptisine hydrochloride
Sanguinarine
Berberine
Chelerythrine
Processing
Vinegar processing