基于特征图谱及D-苦杏仁苷转移率评价燀桃仁配方颗粒的关键生产环节

Evaluation of key production processes of Chan Taoren formula granules based on characteristic chromatogram and D-amygdalin transfer rate

建立燀桃仁配方颗粒的特征图谱和含量测定方法,基于特征图谱相关性和D-苦杏仁苷转移率评价燀桃仁配方颗粒的生产环节,明确关键控制点。采用Waters CORTECS C18色谱柱(4. 6 mm×150 mm,2. 7μm),流动相为乙腈-0. 1%磷酸水溶液,等度洗脱,流速0. 6 m L·min-1,检测波长207 nm,柱温20℃。与燀桃仁标准汤剂相比,饮片、提取液、浓缩液、喷干粉、配方颗粒中均存在5个特征峰,相对保留时间、峰型基本一致,且D-苦杏仁苷从燀桃仁饮片到配方颗粒的总转移率满足标准汤剂转移率范围。D-苦杏仁苷在提取、浓缩、喷干、制粒各环节间的平均转移率分别为56. 65%,72. 85%,94. 58%,99. 29%,故进一步对提取环节中D-苦杏仁苷的影响因素进行分析。结果显示,在水提取环节中D-苦杏仁苷易向L-苦杏仁苷转化,导致D-苦杏仁苷在该环节的转移率低。D-苦杏仁苷在碱性环境下不稳定,易发生异构化;液料比、提取时间对D-苦杏仁苷的提取率均有明显影响。该研究基于特征图谱和D-苦杏仁苷在各环节之间的量值传递,明确燀桃仁配方颗粒生产过程的关键环节,为企业生产和质量控制提供一定的理论依据。

This study aimed to establish characteristic chromatogram and content determination method for Chan Taoren formula granules,evaluate the production processes of Chan Taoren formula granules based on the correlation of characteristic chromatogram and the transfer rate of D-amygdalin,and clarify the key control points.The optimized analytical method was carried out on a Waters CORTECS C18 column(4.6 mm×150 mm,2.7μm)with acetonitrile-0.1%phosphoric acid aqueous solution as the mobile phase at a flow rate of 0.6 m L·min-1.The detection wavelength was 207 nm,and the column temperature was 20℃.As compared with the standard decoction of Chan Taoren,there were five characteristic peaks in the decoction pieces,extracts,concentrates,spray-dried powders and formula granules,basically consistent in relative retention time and peak pattern;in addition,the transfer rate of D-amygdalin from Chan Taoren pieces to the formula granules was within the transfer rate range of standard decoction.The average transfer rate of D-amygdalin was 56.65%,72.85%,94.58%and 99.29%respectively in the extraction,concentration,spray drying and granulation processes.Therefore,the factors affecting D-amygdalin in the extraction process were further studied.The results showed that D-amygdalin was easily converted to L-amygdalin in the water extraction process,leading to a low transfer rate of D-amygdalin in this process.D-amygdalin was unstable under alkaline conditions and prone to isomerization.Both liquid to solid ratio and extraction time had significant effects on the extraction rate of D-amygdalin.In this study,the key links in the production process of Chan Taoren formula granules was clarified based on the characteristic chromatogram and the quantity transmission of D-amygdalin,which provided a theoretical basis for production and quality control.