经典方剂大青龙汤物质基准量值传递分析

Analysis on transfer of reference value of classic prescription Daqinglong decoction

目的:建立大青龙汤物质基准指纹图谱,测定其6个指标成分的含量及其转移率,研究大青龙汤物质基准量值传递规律,为大青龙汤复方制剂和质量标准研究奠定基础。方法:制备15批大青龙汤物质基准,测定出膏率;建立HPLC法,采用Dikma Platisil C18(250 mm×4.6 mm,5μm)色谱柱,以0.15%磷酸水(A)-乙腈(B)为流动相,梯度洗脱,体积流量1 mL·min^(-1),柱温25℃,检测波长207 nm,进样体积10μL,测定物质基准麻黄碱、伪麻黄碱、苦杏仁苷、肉桂酸的含量;以0.05%磷酸水(A)-乙腈(B)为流动相,梯度洗脱,检测波长237 nm,测定物质基准甘草苷、甘草酸的含量,计算其转移率,开展饮片到物质基准量值传递分析。结果:15批大青龙汤物质基准指纹图谱相似度≥0.921,图谱标定了15个共有峰,其中8个来自麻黄,3个来自桂枝,2个来自炒甘草,2个来自燀苦杏仁;指标性成分麻黄碱、伪麻黄碱、苦杏仁苷、甘草苷、肉桂酸、甘草酸的质量分数分别为0.94%~1.30%、0.56%~1.02%、0.70%~1.25%、0.18%~0.32%、0.05%~0.10%、0.46%~1.23%,转移率分别为41.67%~59.47%、42.66%~59.74%、17.59%~36.34%、21.48%~44.75%、31.06%~48.89%、12.95%~25.15%,物质基准出膏率为11.98%~13.38%。结论:指纹图谱结合出膏率和指标成分含量测定对大青龙汤物质基准进行量值传递研究,初步建立了科学稳定的物质基准质量评价方法,为后期复方制剂的研究提供参考。

Objective:To establish the substances benchmarks fingerprint of Daqinglong decoction and determine the content and transfer rate of 6 index components,and study the transfer rule of Daqinglong decoction substances benchmarks value,which laid the foundation for the study of Daqinglong decoction compound preparation and quality standard.Methods:Fifteen batches of substances benchmarks of Daqinglong decoction were prepared,and the paste rate was determined.To determine the contents of ephedrine,pseudoephedrine,amygdalin,and cinnamic acid,HPLC method was performed on a Dikma Platisil C_(18)column(250 mm×4.6 mm,5μm).And 0.15%phosphoric acid water(A)and acetonitrile(B)were used as mobile phases with gradient elution at a flow rate of 1 mL·min^(-1).The column temperature was 25℃,the detection wavelength was 207 nm,and the injection volume was 10μL.To determine the contents of liquiritin and glycyrrhizic acid,0.05%phosphoric acid water(A)and acetonitrile(B)were used as mobile phases with gradient elution.The detection wavelength was 237 nm.The transfer rate was calculated,and the transfer analysis from the decoction pieces to the substances benchmarks was carried out.Results:The fingerprint similarities of 15 batches of Daqinglong decoction substances were≥0.921.Fifteen common peaks were identified,including 8 from Ephedrae Herba,3 from Cinnamomi Ramulus,2 from Glycyrrhizae Radix et Rhizoma(fried),and 2 from Armeniacae Semen Amarum(here).The contents of ephedrine,pseudoephedrine,amygdalin,liquiritin,cinnamic acid and glycyrrhizic acid were 0.94%-1.30%,0.56%-1.02%,0.70%-1.25%,0.18%-0.32%,0.05%-0.10%and 0.46%-1.23%,respectively.The transfer rates were 41.67%-59.47%,42.66%-59.74%,17.59%-36.34%,21.48%-44.75%,31.06%-48.89%and 12.95%-25.15%,respectively.The paste yields of substances benchmarks were 11.98%-13.38%.Conclusion:The fingerprint combined with the determination of paste rates and index component contents are used to study the quantitative value transfer of Daqinglong decoction substance benchmarks,and initially establish a scientific and stable substance benchmarks quality evaluation method,which can provide reference for the future research on compound preparation.