[关键词]
[摘要]
目的 建立经典名方桂枝甘草汤(Guizhi Gancao Decoction,GGD)基准样品的HPLC指纹图谱及指标性成分含量测定方法,研究GGD基准样品量质传递规律。方法 根据《伤寒论》记载方法制备15批GGD基准样品,建立15批GGD基准样品的HPLC指纹图谱,明确指纹图谱中共有峰归属和相似度范围,并对出膏率范围、指标性成分含量范围及转移率范围等量质传递指标进行分析,初步建立了GGD基准样品的质量控制体系。结果 15批GGD基准样品共标定了40个共有峰,且相似度良好(>0.99)。基准样品中原儿茶酸、甘草苷、香豆素、肉桂醇、甘草素、肉桂酸、肉桂醛、甘草酸的质量分数分别为0.080~0.087、0.863~1.055、0.431~0.560、0.167~0.227、0.087~0.127、0.423~0.492、0.160~0.199、2.437~2.904 mg/g。饮片至水煎液中8个指标性成分的转移率分别为44.35%~54.84%、40.56%~44.44%、48.82%~56.00%、22.84%~52.61%、25.70%~30.02%、33.75%~37.83%、23.42%~28.98%、62.09%~65.13%。水煎液至基准样品中8个指标性成分的转移率分别67.99%~84.39%、62.15%~67.93%、59.42%~74.22%、76.20%~85.64%、51.31%~60.73%、78.80%~85.17%、16.27%~22.19%、71.82%~76.58%。整体上,成分在饮片到水煎液阶段转移率偏低,而在后续浓缩与冻干过程中多数成分转移率提升,仅肉桂醛在冻干过程中损失显著。GGD基准样品干膏率传递稳定,平均转移率为77.71%。结论 通过GGD基准样品的HPLC指纹图谱与有效成分的量质传递规律,初步构建了指标成分的质量控制体系,为GGD经典名方制剂的标准化与质量一致性评价提供了科学依据。
[Key word]
[Abstract]
Objective The HPLC fingerprint and the content determination method of the benchmark sample of Guizhi Gancao Decoction (GGD, 桂枝甘草汤) were established to study the rule of quantity-quality transmitting of GGD benchmark samples. Methods According to the method recorded in “Treatise on Febrile Diseases”, 15 batches of GGD benchmark samples were prepared and the HPLC fingerprint of 15 batches of benchmark samples was established. The peak attribution and similarity range in the fingerprint were clarified, and the quantity-quality transfer indexes such as the range of extract yield, the content range of index components and the range of transfer rate were analyzed. The quality control system for GGD benchmark samples was preliminarily established. Results A total of 40 common peaks were identified in the 15 batches of GGD benchmark samples, which with good similarity (> 0.99). The contents of protocatechuic acid, liquiritin, coumarin, cinnamyl alcohol, liquiritigenin, cinnamic acid, cinnamaldehyde, and glycyrrhizic acid in the benchmark sample were 0.080—0.087, 0.863—1.055, 0.431—0.560, 0.167—0.227, 0.087—0.127, 0.423—0.492, 0.160—0.199, and 2.437—2.904 mg/g, respectively. The transfer rates of the eight index components from decoction pieces to water decoction were 44.35%—54.84%, 40.56%—44.44%, 48.82%—56.00%, 22.84%—52.61%, 25.70%—30.02%, 33.75%—37.83%, 23.42%—28.98%, and 62.09%—65.13%, respectively. The transfer rates from the water decoction to the reference sample were 67.99%—84.39%, 62.15%—67.93%, 59.42%—74.22%, 76.20%—85.64%, 51.31%—60.73%, 78.80%—85.17%, 16.27%—22.19%, and 71.82%—76.58%, respectively. Overall, the transfer rates of components from decoction pieces to water decoction were relatively low, while the transfer rates of most components increased during the subsequent concentration and freeze-drying processes. Only cinnamaldehyde showed a significant loss during freeze-drying. The dry paste yield of the reference sample was stable, with an average transfer rate of 77.71 %. Conclusion Through the HPLC fingerprint of GGD benchmark samples and the quantity-quality transfer patterns of its active components, a preliminary quality control system based on index components was established. This provides a scientific basis for the standardization and quality consistency evaluation of GGD classical prescription preparations.
[中图分类号]
R283.6
[基金项目]
国家级大学生创新创业训练计划项目(202410716036);陕西省中医药管理局中医药科研项目(SZY-KJCYC-2025-JC-043);陕西省教育厅重点科学研究计划项目——高校工程研究中心类(25JR059);陕西中医药大学科技创新人才体系建设计划项目(2024-CXTD-03);教育部代谢性心血管疾病医药基础研究创新中心开放课题基金资助(xnykdxcxzx-2024-06)