粒径对多类中药材NIR频谱区的检测研究(1)
[摘要]采用近红外(NIR)光谱漫反射分析技术，提出基于频谱特征，分析粉末粒径对多类中药材近红外漫反射光谱检测影响。以多类中药材为载体，将其粉碎过60，80，100，120目筛，采集近红外光谱。以柴葛根、柴胡、山药为载体考察中药材装样过程所引入误差。结果表明近红外光谱不同波段受粒径的影响不同，在组合频区和一级倍频区的近红外光谱强度与粒径成正比，而且随着波长增大，受粒径的影响越大。而在二级倍频区，近红外光谱强度与粒径成正比。对于装样误差的考察结果表明，当粉碎目数大于60目时，装样误差较小。阐明了合适的粉碎粒径，保证中药近红外漫反射光谱分析技术的准确性。
[关键词]中药材;近红外漫反射;粒径;装样误差;频谱特征
Detection analysis of particle size effects in overtone and combination
region of NIR based on multi-types of Chinese material medica
, 百拇医药
WU Zhi-sheng1，2，3， DU Min1，2，3， PAN Xiao-ning1，2，3， SHI Xin-yuan1，2，3*， QIAO Yan-jiang1，2，3*
(1.Beijing University of Chinese Medicine， 100102， China;
2.Key Laboratory of TCM-information Engineering of State Administration of Traditional Chinese Medicine， Beijing 100102， China;
3.Beijing Key Laboratory for Basic and Development Research on Chinese Medicine， Beijing 100102， China)
, 百拇医药
[Abstract]Near-infrared (NIR) diffuse reflectance spectroscopy was used to analyze the impact of multi-class particle size of Chinese material medica(CMM) based on the spectral characteristics in overtone and combination region. Several types of CMM(60， 80， 100，120 mesh) were subjected to NIR spectra analysis. Spectral reproducibility was examined after sample repackage. The result showed that the effects of particle size on the NIR spectra were different according to different bands， in the combination region and first combination-overtone region. Spectroscopy intensity was proportional to the particle size and influence of particle size was greater as the wavelength increased. While in the second combination-overtone region， it was inversely proportional to particle size. To the sampling loading error， the result indicated that when the mesh number was larger than 60 mesh， the error was small. The appropriate particle size was clarified to guarantee the accuracy and reliability of NIR diffuse reflectance spectroscopy in CMM.
, 百拇医药
[Key words]Chinese material medica; NIR diffuse spectroscopy; particle size; repackage; spectral characteristic
doi：10.4268/cjcmm20150223
近红外漫反射光谱法由于分析速度快、无破坏性、灵活性及无需或很少进行样品处理等优点而广泛应用于固体样品的质量分析，涉及制药、农业、烟草、食品和水果等诸多领域。在中药领域，近红外漫反射光谱法主要应用于中药原料药的质量控制、生产过程控制及制剂的质量控制[1-4]。
对于中药原料药的质量分析包括指标成分的定量分析和特定属性的鉴别。由于中药材多为不规则、质地不均匀样本，因此为尽量使样品均匀以减少误差，在分析中大多需要进行粉碎处理。对于固体粉末样本而言，样品的粒径不同时，样品的重装样的光谱重复性及所产生的噪音水平不同。而且不同粒径样品颗粒间的紧密度及表面积不同，这会严重影响近红外光在样品中的反射及吸收情况，并进而影响近红外光谱的形状。
同时样品颗粒度的这种差异会引起严重的光散射及光程差异[5-6]。目前用于消除物理因素差异的数学方法主要有多元散射校正(multiplicativescattercorrection，MSC)[7]，标准正则变换(standardnormalvariate，SNV)，扩展多元散射校正(extendedmultiplicativescattercorrection，EMSC)，正交信号校正(orthogonalsignalcorrection，OSC)[8]以及opticalpathlengthestimationandcorrection(OPLEC)[9]。数学处理方法虽能一定程度上消除这种影响，但并不能完全消除。, 百拇医药(吴志生 杜敏 潘晓宁 史新元 乔延江)
[关键词]中药材;近红外漫反射;粒径;装样误差;频谱特征
Detection analysis of particle size effects in overtone and combination
region of NIR based on multi-types of Chinese material medica
, 百拇医药
WU Zhi-sheng1，2，3， DU Min1，2，3， PAN Xiao-ning1，2，3， SHI Xin-yuan1，2，3*， QIAO Yan-jiang1，2，3*
(1.Beijing University of Chinese Medicine， 100102， China;
2.Key Laboratory of TCM-information Engineering of State Administration of Traditional Chinese Medicine， Beijing 100102， China;
3.Beijing Key Laboratory for Basic and Development Research on Chinese Medicine， Beijing 100102， China)
, 百拇医药
[Abstract]Near-infrared (NIR) diffuse reflectance spectroscopy was used to analyze the impact of multi-class particle size of Chinese material medica(CMM) based on the spectral characteristics in overtone and combination region. Several types of CMM(60， 80， 100，120 mesh) were subjected to NIR spectra analysis. Spectral reproducibility was examined after sample repackage. The result showed that the effects of particle size on the NIR spectra were different according to different bands， in the combination region and first combination-overtone region. Spectroscopy intensity was proportional to the particle size and influence of particle size was greater as the wavelength increased. While in the second combination-overtone region， it was inversely proportional to particle size. To the sampling loading error， the result indicated that when the mesh number was larger than 60 mesh， the error was small. The appropriate particle size was clarified to guarantee the accuracy and reliability of NIR diffuse reflectance spectroscopy in CMM.
, 百拇医药
[Key words]Chinese material medica; NIR diffuse spectroscopy; particle size; repackage; spectral characteristic
doi：10.4268/cjcmm20150223
近红外漫反射光谱法由于分析速度快、无破坏性、灵活性及无需或很少进行样品处理等优点而广泛应用于固体样品的质量分析，涉及制药、农业、烟草、食品和水果等诸多领域。在中药领域，近红外漫反射光谱法主要应用于中药原料药的质量控制、生产过程控制及制剂的质量控制[1-4]。
对于中药原料药的质量分析包括指标成分的定量分析和特定属性的鉴别。由于中药材多为不规则、质地不均匀样本，因此为尽量使样品均匀以减少误差，在分析中大多需要进行粉碎处理。对于固体粉末样本而言，样品的粒径不同时，样品的重装样的光谱重复性及所产生的噪音水平不同。而且不同粒径样品颗粒间的紧密度及表面积不同，这会严重影响近红外光在样品中的反射及吸收情况，并进而影响近红外光谱的形状。
同时样品颗粒度的这种差异会引起严重的光散射及光程差异[5-6]。目前用于消除物理因素差异的数学方法主要有多元散射校正(multiplicativescattercorrection，MSC)[7]，标准正则变换(standardnormalvariate，SNV)，扩展多元散射校正(extendedmultiplicativescattercorrection，EMSC)，正交信号校正(orthogonalsignalcorrection，OSC)[8]以及opticalpathlengthestimationandcorrection(OPLEC)[9]。数学处理方法虽能一定程度上消除这种影响，但并不能完全消除。, 百拇医药(吴志生 杜敏 潘晓宁 史新元 乔延江)