没药热解特性与炮制相关性研究

Study on Correlation between Pyrolysis Characteristics and Processing of Myrrh

目的建立基于热分析技术的优质没药鉴别的燃烧热解特征参数;并依据没药及其相关配比物的程序升温和恒温的热解特性、热解特性与炮制的相关性,探究没药文火炮制的火力和火候大小。方法应用热重-微熵热重(TG-DTG)技术,依据没药的不同品质等级,建立没药品质鉴别热解特性参数,并对没药及其相关配比物进行程序升温及恒温的热解特性研究。结果没药生品于286.20℃±10.32℃及460.72℃±11.09℃附近的强度为(3.13±0.13)%·min-1及(4.68±0.63)%·min-1的热解燃烧速率峰为品质鉴定没药燃烧热解特征峰,于412.9℃±86.4℃处现热失重速率峰可能与所含杂质有关。根据没药燃烧热解特性,量化本品文火炮制(醋没药、清炒没药)的具体温度为145.17℃±2.72℃;按照没药醋制品及挥发油醋配比物、总酸醋配比物燃烧热解特性可知,醋的加入以反比例降低挥发油热解最大热失重速率温度,并以反比例缩短挥发油热解所需时长,致使挥发油加速热解,从而易于失去,而且以正比例减少总酸热解,致使总酸量得以保留,本品的具体炮制火力和火候分别为炮制温度达到145.17℃±2.72℃后加热(5.67±0.98)min。动力学研究可得没药及其醋配比物都具有良好的线性关系,其中没药R2范围为0.887±0.051,醋配比物R2范围为0.929±0.019,证明Page模型用于中药材文火炮制验证的可行性。结论本研究运用热分析技术建立了用于鉴别优质没药的燃烧热解特征参数,为没药品质鉴别提供了科学性和合理性,并结合炮制辅料,推导、量化清炒、醋炙炮制工艺(起始及终点温度,加热时间),阐释没药清炒和醋炙科学内涵。

Objective Based on the experimental data of thermal analysis,the characteristic parameters of combustion pyrolysis of myrrh were obtained,and the internal evaluation system of myrrh was established.To Investigate the pyrolysis characteristics of myrrh and its relevant mixture.Methods The pyrolysis properties of myrrh and its relevant mixture were studied by thermogravimetry and thermogravimetric TG-DTG technique.Results According to the characteristics of burning pyrolysis of myrrh,the pyrolysis rate peaks of myrrh at 286.20℃±10.32℃and 460.72℃±11.09℃were(3.13±0.13)%·min-1 and(4.68±0.63)%·min-1 respectively were the pyrolysis characteristics of myrrh,at 412.9℃±86.4℃appeared the thermogravimetric rate peak may be related to the impurities contained in it.The specific temperature of this product was 145.17℃±2.72℃.The addition of vinegar reduces the temperature of the maximum thermogravimetric rate of the pyrolysis of the volatile oil in reverse proportion,which causes the volatile oil to be easily lost,and shortens the time required for the pyrolysis of the volatile oil in a reverse proportion,which results in the accelerated pyrolysis of the essential oil,and decreases the total acid pyrolysis in a positive proportion.As a result,the total acid content is preserved.The specific processing temperature and time of this product are 145.17℃±2.72℃and 12.37±1.60 min.It was found that there was a good linear relationship between myrrh and its vinegar ratio.The range of R2 of myrrh and vinegar was 0.887±0.051 and 0.929±0.019,respectively,which proved the feasibility of using Page model to verify the processing of Chinese medicinal materials.Conclusion The characteristic parameters of combustion pyrolysis used to identify high quality myrrh were established by using thermal analysis technique,which provided scientific and reasonable quality identification of myrrh.It lays a theoretical foundation for specific application and related research,combined with processing excipients and this paper deduces and quantifies the processing technology.