含挥发油饮片砂仁标准汤剂的质量评价方法研究
投稿时间:2024-04-28  修订日期:2024-06-20   点此下载全文
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作者中文名作者英文名单位中文名单位英文名E-Mail
唐双燕* TANG Shuangyan 华润三九现代中药制药有限公司 China Resources Sanjiu Modern Chinese Medicine Pharmaceutical Co,LTD tangshuangyan@999.com.cn 
魏家保 WEI Jiabao 华润三九现代中药制药有限公司 China Resources Sanjiu Modern Chinese Medicine Pharmaceutical Co,LTD WEIJIABAO8@999.com.cn 
基金项目:深圳市科技计划项目(JSGG20191129093418578)
中文摘要:目的 通过分析砂仁饮片标准汤剂出膏率、含量和转移率以及特征图谱,建立其质量评价方法。方法 按要求制备15批砂仁标准汤剂,测定出膏率、乙酸龙脑酯和挥发油含量,并计算转移率。同时采用CORTECS T3色谱柱(2.1 mm × 100 mm,1.6 μm),乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱,检测波长为260 nm,流速为0.35 mL·min–1,柱温为30 ℃,建立标准汤剂特征图谱分析方法。结果:通过对制备的15批砂仁标准汤剂进行出膏率、含量、特征图谱测定,得到出膏率为12.3~17.6%,乙酸龙脑酯转移率为3.9~10.5%,挥发油转移率为5.6~15.6%。在最佳色谱条件下,采集到的砂仁标准汤剂特征图谱,实现了多种化学成分类型的展现,共标定11个特征峰,采用LC/MS/MS和对照品确认其中7个,其中峰1为原儿茶酸、峰4为香草酸、峰5为儿茶素、峰7为原花青素B2、峰8为表儿茶素、峰10为异槲皮苷、峰11为槲皮苷,采用中药色谱指纹图谱相似度评价系统,得到15批砂仁标准汤剂的相似度评价结果为0.984~0.999。聚为2类,2种主成分统计的累积方差贡献率达81.579%。结论:本研究所建立的含量测定及特征图谱方法适用性与准确度好,能较全面地反映砂仁饮片标准汤剂内在质量,可为砂仁配方颗粒制备提供参考依据。
中文关键词:阳春砂  标准汤剂  乙酸龙脑酯  挥发油  特征图谱
 
Study on the Quality Evaluation of Standard Decoction of Amomum villosum Containing Volatile Oil
Abstract:Objective The quality evaluation method was established by analyzing the extraction rate, content, transfer rate and characteristic spectrum of standard decoction for Amomi Fructus decoction pieces. Methods 15 batches of standard decoction were prepared according to the requirements, the extraction rate and content of bornyl acetate and volatile oil were determined, and the transfer rate was calculated. Simultaneously, the chromatography was performed on A CORTECS T3 column (2.1 mm × 100 mm, 1.6 μm) with acetonitrile (A) -0.1% phosphoric acid aqueous solution (B) as the mobile phase by gradient elution. The detection wavelength was set at 260 nm, the flow rate was 0.35 mL· min-1, and the column temperature was 30 ℃. To establish a standard decoction characteristic spectrum analysis method. Results The extraction rate, content and characteristic spectrum of 15 batches of Amomi Fructus standard decoction were determined. Which showed that the extraction rate was 12.3~17.6%, the transfer rate of bornyl acetate was 3.9~10.5%, and the transfer rate of volatile oil was 5.6~15.6%. The characteristic spectrum of Amomi Fructus standard decoction was collected under the optimal chromatographic conditions, and a variety of chemical composition types were displayed. A total of 11 characteristic peaks were marked, and 7 of them were identified by LC/MS/MS and reference substances. Peak 1 is Protocatechuic Acid, peak 4 is Vanillic Acid, peak 5 is Catechin, peak 7 is Procyanidin B2, peak 8 is Epicatechin, peak 10 is Isoquercetin and peak 11 is Quercetin. The similarity evaluation results of 15 batches of Amomi Fructus standard decoction were 0.984 ~ 0.999 by using the traditional Chinese medicine chromatographic fingerprint similarity evaluation system. The cumulative variance contribution of the two principal components is 81.579%. Conclusion The method of content determination and characteristic atlas established in this study has good applicability and accuracy, and can reflect the intrinsic quality of standard decoction of Amomi Fructus decoction pieces comprehensively, also can provide reference for preparation of Amomi Fructus formula granules.
keywords:Amomi Fructus  Standard decoction  Bornyl acetate  volatile oil  Characteristic map
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