公开(公告)号：US20100315083A1

公开(公告)日：2010-12-16

申请号：US12445792

申请日：2007-10-19

申请人： Guido F. Pauli ,  Birgit Jaki ,  David Lankin

发明人： Guido F. Pauli ,  Birgit Jaki ,  David Lankin

IPC分类号： G01R33/48

CPC分类号： G01N24/08 ,  G01R33/46

摘要： Provided herein are various methods and systems for analyzing natural products by quantitative proton nuclear magnetic resonance (qHNMR). A method is provided for quantitative and qualitative determination of a natural product by 1HNMR and decoupling 13C nuclei from the protons in the sample containing the natural product. The resultant spectrum wherein the decoupling provides a cleaner spectrum is used to provide both structural and quantitative information about species within the sample. In an aspect, the decoupling is provided by globally optimized alternating-phase rectangular pulses (GARP). The methods presented herein are optionally used to detect impurities in a reference material and verify the purity level of a reference material.

摘要翻译： 本文提供了通过定量质子核磁共振（qHNMR）分析天然产物的各种方法和系统。 提供了一种通过1HNMR定量和定性测定天然产物的方法，并将含有天然产物的样品中的13C核与质子脱离。 其中解耦提供更清洁光谱的所得光谱用于提供关于样品内物种的结构和定量信息。 在一个方面，解耦由全局优化的交变相位矩形脉冲（GARP）提供。 本文提供的方法任选地用于检测参考材料中的杂质并验证参考材料的纯度水平。

公开(公告)号：US08062898B2

公开(公告)日：2011-11-22

申请号：US11876545

申请日：2007-10-22

申请人： Guido F. Pauli ,  John Brent Friesen

发明人： Guido F. Pauli ,  John Brent Friesen

IPC分类号： G01N30/00

CPC分类号： G01N30/42 ,  G01N30/8658 ,  G01N30/34

摘要： Application of a reference mixture of natural products for systematic analysis and comparison of the properties of biphasic solvent systems in counter-current/partition chromatography. Because the reference mixture is comprised of compounds with varying polarities, functional groups, and structural features it provides a rational method for mapping the optimal resolution polarity range of a particular solvent system. The mapping of optimal resolution polarity ranges of solvent systems provided for the description of the overall optimal resolution polarity range of a solvent system family, comprised of the same solvents in different proportions. By comparing the reference mixture performance in the individual members of a solvent system family, the solvent system that best functions as the representative of, or portal to, the solvent system families is determined. Use of the reference mixture also afforded a method to compare the overall optimal resolution polarity ranges of solvent system families. Based on performance of reference mixture chromatograms, the CCC properties of solvent systems, can be compared and their CCC potential examined. The methods of the invention employing the reference mixture provides was used to identify a quaternary solvent system, hexane/t-butylmethylether/acetonitrile/water (HterAcWat), which was found to be useful for CCC of mixtures containing natural products.

摘要翻译： 应用天然产物的参考混合物进行系统分析，并对比逆流/分配色谱中双相溶剂体系的性质。 由于参考混合物由具有不同极性，官能团和结构特征的化合物组成，因此提供了一种合理的方法，用于绘制特定溶剂系统的最佳分辨率极性范围。 溶剂系统的最佳分辨率极性范围的映射，用于描述溶剂系统族的总体最佳分辨率极性范围，由不同比例的相同溶剂组成。 通过比较溶剂系统族的各个成员的参考混合物性能，确定最适合作为溶剂系统族的代表或入口的溶剂体系。 参考混合物的使用也提供了一种比较溶剂系统族的总体最佳分辨率极性范围的方法。 基于参比混合色谱的性能，可以比较溶剂体系的CCC性质，并对其CCC电位进行检测。 使用参考混合物提供的本发明的方法用于鉴定四元溶剂体系，己烷/叔丁基甲基醚/乙腈/水（HterAcWat），其被发现可用于含有天然产物的混合物的CCC。

公开(公告)号：US08175817B2

公开(公告)日：2012-05-08

申请号：US11961026

申请日：2007-12-20

申请人： Guido F. Pauli ,  J. Brent Friesen

发明人： Guido F. Pauli ,  J. Brent Friesen

IPC分类号： G06F17/14 ,  G01N31/00

CPC分类号： G01N30/8675 ,  G01N30/42 ,  G01N30/8658 ,  G01N30/8665

摘要： Various methods for visualization of output from a liquid-liquid chromatographic instrument are provided. One or more analytes detected by a liquid-liquid chromatographic instrument are visualized by providing a data set comprising a plurality of data points corresponding to one or more analytes detected by the instrument, wherein the data points comprise at least one parameter related to a K-value or a parameter from which a K-value can be determined. A K-value is calculated for at least a portion of the data set, and at least a portion of those K-values transformed by a reciprocal transformation to generate output data having a transformed K-value, wherein the transformed K-value is a real number for all K undergoing the transformation, thereby ensuring that all analytes detected by the instrument are plotted in a single chromatogram. The output data is provided to a user. The output data may be used for instrument performance testing, design, calibration, or for selecting suitable solvent systems to detect analytes of interest.

摘要翻译： 提供了用于液体色谱仪输出可视化的各种方法。 通过提供包括对应于由仪器检测到的一种或多种分析物的多个数据点的数据集来显现由液 - 液色谱仪检测到的一种或多种分析物，其中数据点包括与K- 值或可以从其确定K值的参数。 对于数据集的至少一部分计算K值，并且通过互逆变换变换的那些K值的至少一部分以生成具有变换的K值的输出数据，其中变换的K值是 所有K进行转化的实数，从而确保仪器检测到的所有分析物都绘制在单个色谱图中。 将输出数据提供给用户。 输出数据可用于仪器性能测试，设计，校准或选择合适的溶剂系统以检测感兴趣的分析物。

公开(公告)号：US20080201085A1

公开(公告)日：2008-08-21

申请号：US11961026

申请日：2007-12-20

申请人： Guido F. Pauli ,  J. Brent Friesen

发明人： Guido F. Pauli ,  J. Brent Friesen

IPC分类号： G06F17/14 ,  G01N31/00

CPC分类号： G01N30/8675 ,  G01N30/42 ,  G01N30/8658 ,  G01N30/8665

摘要： Various methods for visualization of output from a liquid-liquid chromatographic instrument are provided. One or more analytes detected by a liquid-liquid chromatographic instrument are visualized by providing a data set comprising a plurality of data points corresponding to one or more analytes detected by the instrument, wherein the data points comprise at least one parameter related to a K-value or a parameter from which a K-value can be determined. A K-value is calculated for at least a portion of the data set, and at least a portion of those K-values transformed by a reciprocal transformation to generate output data having a transformed K-value, wherein the transformed K-value is a real number for all K undergoing the transformation, thereby ensuring that all analytes detected by the instrument are plotted in a single chromatogram. The output data is provided to a user. The output data may be used for instrument performance testing, design, calibration, or for selecting suitable solvent systems to detect analytes of interest.

摘要翻译： 提供了用于液体色谱仪输出可视化的各种方法。 通过提供包括对应于由仪器检测到的一种或多种分析物的多个数据点的数据集来显现由液 - 液色谱仪检测到的一种或多种分析物，其中数据点包括与K- 值或可以从其确定K值的参数。 对于数据集的至少一部分计算K值，并且通过互逆变换变换的那些K值的至少一部分以生成具有变换的K值的输出数据，其中变换的K值是 所有K进行转化的实数，从而确保仪器检测到的所有分析物都绘制在单个色谱图中。 将输出数据提供给用户。 输出数据可用于仪器性能测试，设计，校准或选择合适的溶剂系统以检测感兴趣的分析物。

公开(公告)号：US20080127720A1

公开(公告)日：2008-06-05

申请号：US11876545

申请日：2007-10-22

申请人： Guido F. Pauli ,  John Brent Friesen

发明人： Guido F. Pauli ,  John Brent Friesen

IPC分类号： G01N30/00 ,  G01N37/00 ,  G01N30/90

CPC分类号： G01N30/42 ,  G01N30/8658 ,  G01N30/34

摘要： Application of a reference mixture of natural products for systematic analysis and comparison of the properties of biphasic solvent systems in counter-current/partition chromatography. Because the reference mixture is comprised of compounds with varying polarities, functional groups, and structural features it provides a rational method for mapping the optimal resolution polarity range of a particular solvent system. The mapping of optimal resolution polarity ranges of solvent systems provided for the description of the overall optimal resolution polarity range of a solvent system family, comprised of the same solvents in different proportions. By comparing the reference mixture performance in the individual members of a solvent system family, the solvent system that best functions as the representative of, or portal to, the solvent system families is determined. Use of the reference mixture also afforded a method to compare the overall optimal resolution polarity ranges of solvent system families. Based on performance of reference mixture chromatograms, the CCC properties of solvent systems, can be compared and their CCC potential examined. The methods of the invention employing the reference mixture provides was used to identify a quaternary solvent system, hexane/t-butylmethylether/acetonitrile/water (HterAcWat), which was found to be useful for CCC of mixtures containing natural products.

摘要翻译： 应用天然产物的参考混合物进行系统分析，并对比逆流/分配色谱中双相溶剂体系的性质。 由于参考混合物由具有不同极性，官能团和结构特征的化合物组成，因此提供了一种合理的方法，用于绘制特定溶剂系统的最佳分辨率极性范围。 溶剂系统的最佳分辨率极性范围的映射，用于描述溶剂系统族的总体最佳分辨率极性范围，由不同比例的相同溶剂组成。 通过比较溶剂系统族的各个成员的参考混合物性能，确定最适合作为溶剂系统族的代表或入口的溶剂体系。 参考混合物的使用也提供了一种比较溶剂系统族的总体最佳分辨率极性范围的方法。 基于参比混合色谱的性能，可以比较溶剂体系的CCC性质，并对其CCC电位进行检测。 使用参考混合物提供的本发明的方法用于鉴定四元溶剂体系，己烷/叔丁基甲基醚/乙腈/水（HterAcWat），其被发现可用于含有天然产物的混合物的CCC。