目的根据白术Atractylodis Macrocephalae Rhizoma指纹图谱形状特征,建立一种快速精准辨识不同产地与炮制品的方法。方法建立45批不同产地与炮制法的白术UPLC指纹图谱库,运用总量统计矩及相似度法、正交偏最小二乘-判别分析(orthogonal ...目的根据白术Atractylodis Macrocephalae Rhizoma指纹图谱形状特征,建立一种快速精准辨识不同产地与炮制品的方法。方法建立45批不同产地与炮制法的白术UPLC指纹图谱库,运用总量统计矩及相似度法、正交偏最小二乘-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)法辨析此指纹图谱的形状特点,捕获其特征指纹图谱及特征峰。结果生品、麸炒、土炒白术UPLC指纹图谱的共有峰16个;安徽与湖南、安徽与浙江、湖南与浙江产地的生白术的总量统计矩相似度分别为0.774~0.982、0.799~0.969、0.788~0.886;3产地的生品与麸炒、生品与土炒、麸炒与土炒白术的总量统计矩相似度中最大值为0.990, 最小值为0.774。再结合OPLS-DA法中变量重要性投影(variable importance for the projection,VIP)分析获得其中1~3、6、16号为区分贡献度最大的5个标志峰,确认6号峰为白术内酯II。结论这5个标志峰对应物质可认定白术的潜在质量标志物(Q-Marker),为白术的产地、炮制法的精准识别及其质量控制与评价提供理论与实验依据,同时也为中药指纹图谱辨形论质做了积极探索。展开更多
Three lanthanide complexes [LnL_(3)(H_(2)O)]PMo_(12)O_(40)·CH_(3)CN(Ln = Dy^(3+) for 1, Ln = Ho^(3+) for 2, Ln = Lu^(3+) for 3, L = tetraethyl ethylenediphosphonate) have been synthesized, and characterized by si...Three lanthanide complexes [LnL_(3)(H_(2)O)]PMo_(12)O_(40)·CH_(3)CN(Ln = Dy^(3+) for 1, Ln = Ho^(3+) for 2, Ln = Lu^(3+) for 3, L = tetraethyl ethylenediphosphonate) have been synthesized, and characterized by single-crystal X-ray diffraction, elemental analysis, IR, PXRD, thermogravimetric analysis and terahertz time-domain spectroscopy(THz-TDS). Structural analysis results show that they have the same coordination mode and similar steric structures. Complexes 1~3 all crystallize in the monoclinic crystal system with space group P2_(1/c). The centered Ln(Ⅲ) obtained a seven-coordinated mononuclear structure by linking with three tetraethyl ethylenediphosphonates and one water molecule, resulting in a three-dimensional supramolecular structure through hydrogen bonding. The three complexes have good adsorption properties for rhodamine B(RhB) in powder state. Moreover, terahertz time-domain spectroscopy(THz-TDS) was applied to represent the structures of complexes and ligands, which will provide useful information for establishing bridge between THz and complex structure in coordination chemistry.展开更多
文摘目的根据白术Atractylodis Macrocephalae Rhizoma指纹图谱形状特征,建立一种快速精准辨识不同产地与炮制品的方法。方法建立45批不同产地与炮制法的白术UPLC指纹图谱库,运用总量统计矩及相似度法、正交偏最小二乘-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)法辨析此指纹图谱的形状特点,捕获其特征指纹图谱及特征峰。结果生品、麸炒、土炒白术UPLC指纹图谱的共有峰16个;安徽与湖南、安徽与浙江、湖南与浙江产地的生白术的总量统计矩相似度分别为0.774~0.982、0.799~0.969、0.788~0.886;3产地的生品与麸炒、生品与土炒、麸炒与土炒白术的总量统计矩相似度中最大值为0.990, 最小值为0.774。再结合OPLS-DA法中变量重要性投影(variable importance for the projection,VIP)分析获得其中1~3、6、16号为区分贡献度最大的5个标志峰,确认6号峰为白术内酯II。结论这5个标志峰对应物质可认定白术的潜在质量标志物(Q-Marker),为白术的产地、炮制法的精准识别及其质量控制与评价提供理论与实验依据,同时也为中药指纹图谱辨形论质做了积极探索。
基金supported by the National Natural Science Foundation of China(Nos.21171119 and 11574408)the Beijing Municipal Natural Science Foundation(Nos.2172017 and 2172012)。
文摘Three lanthanide complexes [LnL_(3)(H_(2)O)]PMo_(12)O_(40)·CH_(3)CN(Ln = Dy^(3+) for 1, Ln = Ho^(3+) for 2, Ln = Lu^(3+) for 3, L = tetraethyl ethylenediphosphonate) have been synthesized, and characterized by single-crystal X-ray diffraction, elemental analysis, IR, PXRD, thermogravimetric analysis and terahertz time-domain spectroscopy(THz-TDS). Structural analysis results show that they have the same coordination mode and similar steric structures. Complexes 1~3 all crystallize in the monoclinic crystal system with space group P2_(1/c). The centered Ln(Ⅲ) obtained a seven-coordinated mononuclear structure by linking with three tetraethyl ethylenediphosphonates and one water molecule, resulting in a three-dimensional supramolecular structure through hydrogen bonding. The three complexes have good adsorption properties for rhodamine B(RhB) in powder state. Moreover, terahertz time-domain spectroscopy(THz-TDS) was applied to represent the structures of complexes and ligands, which will provide useful information for establishing bridge between THz and complex structure in coordination chemistry.
