[关键词]
[摘要]
目的 建立5产地15批次龙胆饮片标准汤剂质量评价方法,并以出膏率、指标成分量及转移率、指纹图谱为指征进行研究。方法 以水为溶剂,参照传统煎药工艺制备标准汤剂,采用UPLC-DAD法测定龙胆苦苷量,计算转移率、出膏率,采用UPLC/Q-TOF-MS/MS法进行指纹图谱研究并确认共有峰。结果 15批次龙胆样品制成的标准汤剂中龙胆苦苷量为1.57~2.81 mg/mL,龙胆苦苷转移率在50.71%~67.70%,平均转移率为59.20%,标准偏差(RE)为7.31%。出膏率为15.72%~25.52%,平均出膏率为19.20%,RE为2.85%。指纹图谱共有峰10个,确认10个,分别为紫丁香酸葡萄糖苷、1-(4-羟基-3-甲氧基)-苯基-1,2,3-丙三醇或异构体、马钱酸、四乙酰开联番木鳖苷、龙胆苦苷、naptho(2,3-c)furan-1(3H)-one-9-(acetyloxy)-6-methoxy-8-[(2,3,4-tri-O-acetyl-6-O-(2,3,4-tri-O-acetyl-β-D-xylopyranosyl)-β-D-glucopyranosyl)oxy]或异构体、C46H54O28(未知化合物)、C46H54O27(未知化合物)、macrophylloside B、isomacrophylloside。结论 15批次龙胆饮片标准汤剂制备工艺符合传统汤剂制法,样品来源具有代表性,样品批次符合指纹图谱研究要求,质量评价内容涵盖面广,所得数据具有代表性,可用于龙胆饮片标准汤剂的制备及质量评价,可以为配方颗粒标准的制定及工业化生产提供基础数据支撑。
[Key word]
[Abstract]
Objective To evaluate the extraction ratio, content determination, transfer ratio, and feature maps or fingerprints by establishing 15 batches of standard decoction of Gentiana Radix from five different places. Methods The Gentiana Radix was dissolved in water based on the traditional decoction process, the content of gentiopicroside was determined by UPLC-DAD, the transfer ratio, the extraction ratio, the fingerprints and the common peaks were evaluated by UPLC/Q-TOF-MS/MS. Results The determination of gentiopicroside of 15 batches of standard decoction was in the range of 1.57-2.81 mg/mL, the transfer ratio of gentiopicroside was in the range of 50.71%-67.70%, the average transfer ratio was 59.20%, and the standard deviation was 7.31%. The extraction ratio was in the range of 15.72%-25.52%, the average extraction ratio was 19.20% and the standard deviation was about 2.85%. Ten peaks of fingerprint were confirmed in this research, such as lilac glucoside, 1-(4-hydroxy-3-methoxy)-phenyl-1,2,3-glycerol or isomer, loganate, secologanoside, gentiopicroside, naptho(2,3-c)furan-1(3H)-one-9-(acetyloxy)-6-methoxy-8-[(2,3,4-tri-O-acetyl-6-O-(2,3,4-tri-oacetyl-β-D-xylopyranosyl)-β-D-glucopyranosyl)oxy] or isomer, C46H54O28 (unknown compound), C46H54O27 (unknown compound), macrophylloside B, and isomacrophylloside. Conclusion The preparation method in this paper conforms to the traditional decoction method, the analyzed samples had representiveness, the batches fit the fingerprint research requirements, the content of quality evaluation covers a wide range and the data obtained are representative. It can be used for the standard preparation and quality evaluation of traditional Chinese medicine and providing basic data for the quality and the industrialization of dispensing granules.
[中图分类号]
[基金项目]
中国中医科学院中药研究所、上海市药材有限公司、日本国株式会社津村科研合作项目——标准汤剂、中药配方颗粒国家标准和药材DNA条形码鉴定体系研究(H2016021-06)