机构地区:[1]辽宁中医药大学药学院,辽宁大连116600 [2]辽宁省组分中药工程技术研究中心辽宁省现代中药研究工程实验室,辽宁大连116600
出 处:《中国实验方剂学杂志》2016年第5期101-104,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:国家自然科学基金项目(81241111);辽宁省高等学校优秀人才支持计划项目(LR2013044)
摘 要:目的:对气滞胃痛颗粒复方中挥发性指标成分柠檬烯进行含量测定,完善气滞胃痛颗粒复方中挥发性成分的质量控制标准。方法:采用高效液相色谱法,考察了无糖型气滞胃痛颗粒中柠檬烯的最佳前处理工艺,并对此方法进行了方法学考察,与此同时定量检测10批气滞胃痛颗粒的柠檬烯含量,确定其含量限度。检测气滞胃痛颗粒红外光谱,并应用灰色关联理论分析与柠檬烯含量相关的谱峰。结果:实验所得的柠檬烯的最佳前处理方法为取无糖型气滞胃痛颗粒2.5 g,加甲醇50 m L,超声处理(功率250 W,频率40 k Hz)30 min,经方法学考察确定,柠檬烯线性范围为0.17~1.68μg(r=0.999 8),平均加样回收率为99.77%,最终确定每袋无糖型气滞胃痛颗粒中柠檬烯含量应不低于1.00 mg。灰色关联分析共得到3个与柠檬烯含量相关的谱峰。结论:该方法操作简便、科学合理,可作为气滞胃痛颗粒中柠檬烯的含量测定方法,该研究对气滞胃痛颗粒的质量评价具有重大意义。结合灰色理论数据分析方法,构建了粗略检验气滞胃痛颗粒中柠檬烯含量的红外光谱分析法,为气滞胃痛颗粒中柠檬烯含量的快速鉴别提供了一种有效、简便和直观的方法,为全面、综合评价中药成方制剂气滞胃痛颗粒的质量提供了有力补充。Objective: To determine the content of volatile index component limonene in Qizhi Weitong granules, and improve the quality control standard of volatile components in Qizhi Weitong granules compound. Method: In this study, high performance liquid chromatography (HPLC) was used to investigate the optimum pretreatment process of limonene in sugarless Qizhi Weitong granules, and a methodological study was done for this method.At the same time, content of limonene in 10 batches of Qizhi Weitong granules was detected and their content limits were determined, and to establish a rapid identification by infrared spectroscopy easy way limonene content. Result: The obtained optimum pretreatment method for limonene was as follows: take sugarless Qizhi Weitong granules 2.5 g, add methanol 50 mL, and with ultrasonic treatment (power 250 W, frequency 40 kHz) for 30 min. Methodological study identified a linear range of limonene between 0.17-1.68 μg (r=0.999 8), and the average recovery rate was 99.77%, and the content limit of limonene in Qizhi Weitong granules was determined as not less than 1.00 mg. Gray correlation analysis were obtained 3 and limonene content related peaks. Conclusion: The method is simple, scientific and reasonable, and can be used as a method for the determination of limonene content in Qizhi Weitong granules. The present study has great significance for quality evaluation of Qizhi Weitong granules, and provides great supplementary for the full and comprehensive evaluation of traditional Chinese medicine prescriptions. The study combined data analysis of gray theory, construction of the coarse particle inspection Qizhiweitong limonene content of infrared spectroscopy, for the rapid identification of stomach Qi stagnation particles limonene provides an effective, simple and intuitive way, for the full, comprehensive evaluation of traditional Chinese medicine prescription preparations Qizhiweitong the quality of the particles provide a strong complement.
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