The ^1 H nuclear magnetic resonance （^1 H NMR） fingerprints of fractionated non-polar extracts （control substance for a plant drug （CSPD） A） from Rhizoma chuanxiong, the rhizomes of Ligusticum chuanxiong Hort., ...The ^1 H nuclear magnetic resonance （^1 H NMR） fingerprints of fractionated non-polar extracts （control substance for a plant drug （CSPD） A） from Rhizoma chuanxiong, the rhizomes of Ligusticum chuanxiong Hort., of seven specimens from different sources were measured on Fourier Transform （FT）-NMR spectrometer and assigned by comparing them with the ^1 H NMR spectra of the isolated pure compounds. The ^1 H NMR fingerprints showed exclusively characteristic resonance signals of the major special constituents of the plant. Although the differences in the relative intensity of the ^1H NMR signals due to a discrepancy in the ratio of the major constituents among these samples could be confirmed by high performance liquid chromatography analysis, the general features of the ^1H NMR fingerprint established for an authentic sample of the rhizomes of L. chuanxiong e. hibited exclusive data from those special compounds and can be used for authenticating L. Chuanxiong species.展开更多
本研究采用定量核磁共振(nuclear magnetic resonance,NMR)与高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)技术分析大地95油菜蕾薹期不同部位(茎、叶、花苞)小分子营养物的组...本研究采用定量核磁共振(nuclear magnetic resonance,NMR)与高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)技术分析大地95油菜蕾薹期不同部位(茎、叶、花苞)小分子营养物的组成差异。结果表明,通过1H-NMR与HPLC-MS/MS分析在大地95菜薹茎、叶、花苞中共定性定量得到53种小分子化合物,其中具有显著差异的物质有亮氨酸、异亮氨酸、缬氨酸、γ-氨基丁酸、丙氨酸、脯氨酸、苯丙氨酸、乳酸、柠檬酸、琥珀酰胺、β-D-葡萄糖、α-D-葡萄糖、蔗糖、果糖、胆碱、甜菜碱、延胡索酸、黄芩素、阿魏酸、山柰酚、芥子碱、反式肉桂酸、橙皮素。糖类物质在油菜茎部的含量最高;而胆碱、琥珀酰胺、多数氨基酸、有机酸以及酚酸类物质主要在花苞中积累,叶部的优势代谢物以黄岑素、芥子碱和柠檬酸为主。通过分析代谢通路发现这些差异代谢物主要涉及植物的柠檬酸盐循环,黄酮和黄酮醇的生物合成,苯丙氨酸代谢,氨酰基-tRNA生物合成,缬氨酸、亮氨酸和异亮氨酸的生物合成,糖酵解/糖异生,苯丙氨酸、酪氨酸和色氨酸的生物合成等。本研究结果可为全面评估蕾薹期油菜的营养价值提供数据参考,并为选育营养丰富的油菜品种提供科学依据。展开更多
建立了杜仲中京尼平甙酸的硅胶柱色谱分离纯化及反相高效液相色谱/液相色谱-电喷雾质谱/核磁共振(RP-HPLC/LC-E S I-M S/NMR)鉴定方法。杜仲皮经粉碎后,用70%乙醇提取,提取液经减压蒸馏至干,再用甲醇溶解,然后吸附于硅胶上,并以不同体...建立了杜仲中京尼平甙酸的硅胶柱色谱分离纯化及反相高效液相色谱/液相色谱-电喷雾质谱/核磁共振(RP-HPLC/LC-E S I-M S/NMR)鉴定方法。杜仲皮经粉碎后,用70%乙醇提取,提取液经减压蒸馏至干,再用甲醇溶解,然后吸附于硅胶上,并以不同体积比的氯仿-甲醇混合液按洗脱剂的极性由小到大进行洗脱,以RP-HPLC法检测洗脱液中物质的种类和含量。结果表明:洗脱剂为氯仿-甲醇(体积比为8∶1)的洗脱液经分析为单一组分,其保留时间为5.142m in;以对照品京尼平甙酸添加法测定,其峰高增加;相关紫外光谱和红外光谱检测结果与京尼平甙酸对照品基本一致;结合LC-E S I-M S、1H-NMR和13C-NMR等测定,确定该洗脱组分为京尼平甙酸。展开更多
基金Supported by the National Natural Science Foundation of China (30630073)the Science Foundation of the State Administration of Traditional ChineseMedicine, China (02-03ZP09)
文摘The ^1 H nuclear magnetic resonance （^1 H NMR） fingerprints of fractionated non-polar extracts （control substance for a plant drug （CSPD） A） from Rhizoma chuanxiong, the rhizomes of Ligusticum chuanxiong Hort., of seven specimens from different sources were measured on Fourier Transform （FT）-NMR spectrometer and assigned by comparing them with the ^1 H NMR spectra of the isolated pure compounds. The ^1 H NMR fingerprints showed exclusively characteristic resonance signals of the major special constituents of the plant. Although the differences in the relative intensity of the ^1H NMR signals due to a discrepancy in the ratio of the major constituents among these samples could be confirmed by high performance liquid chromatography analysis, the general features of the ^1H NMR fingerprint established for an authentic sample of the rhizomes of L. chuanxiong e. hibited exclusive data from those special compounds and can be used for authenticating L. Chuanxiong species.
文摘本研究采用定量核磁共振(nuclear magnetic resonance,NMR)与高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)技术分析大地95油菜蕾薹期不同部位(茎、叶、花苞)小分子营养物的组成差异。结果表明,通过1H-NMR与HPLC-MS/MS分析在大地95菜薹茎、叶、花苞中共定性定量得到53种小分子化合物,其中具有显著差异的物质有亮氨酸、异亮氨酸、缬氨酸、γ-氨基丁酸、丙氨酸、脯氨酸、苯丙氨酸、乳酸、柠檬酸、琥珀酰胺、β-D-葡萄糖、α-D-葡萄糖、蔗糖、果糖、胆碱、甜菜碱、延胡索酸、黄芩素、阿魏酸、山柰酚、芥子碱、反式肉桂酸、橙皮素。糖类物质在油菜茎部的含量最高;而胆碱、琥珀酰胺、多数氨基酸、有机酸以及酚酸类物质主要在花苞中积累,叶部的优势代谢物以黄岑素、芥子碱和柠檬酸为主。通过分析代谢通路发现这些差异代谢物主要涉及植物的柠檬酸盐循环,黄酮和黄酮醇的生物合成,苯丙氨酸代谢,氨酰基-tRNA生物合成,缬氨酸、亮氨酸和异亮氨酸的生物合成,糖酵解/糖异生,苯丙氨酸、酪氨酸和色氨酸的生物合成等。本研究结果可为全面评估蕾薹期油菜的营养价值提供数据参考,并为选育营养丰富的油菜品种提供科学依据。
文摘建立了杜仲中京尼平甙酸的硅胶柱色谱分离纯化及反相高效液相色谱/液相色谱-电喷雾质谱/核磁共振(RP-HPLC/LC-E S I-M S/NMR)鉴定方法。杜仲皮经粉碎后,用70%乙醇提取,提取液经减压蒸馏至干,再用甲醇溶解,然后吸附于硅胶上,并以不同体积比的氯仿-甲醇混合液按洗脱剂的极性由小到大进行洗脱,以RP-HPLC法检测洗脱液中物质的种类和含量。结果表明:洗脱剂为氯仿-甲醇(体积比为8∶1)的洗脱液经分析为单一组分,其保留时间为5.142m in;以对照品京尼平甙酸添加法测定,其峰高增加;相关紫外光谱和红外光谱检测结果与京尼平甙酸对照品基本一致;结合LC-E S I-M S、1H-NMR和13C-NMR等测定,确定该洗脱组分为京尼平甙酸。
