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
A quantitative structure-spectrum relationship (QSSR) model was developed to simulate 13C nuclear magnetic resonance (NMR) spectra of carbinol carbon atoms for 55 alcohols. The proposed model,using multiple linear reg...A quantitative structure-spectrum relationship (QSSR) model was developed to simulate 13C nuclear magnetic resonance (NMR) spectra of carbinol carbon atoms for 55 alcohols. The proposed model,using multiple linear regression,contained four descriptors solely extracted from the molecular structure of compounds. The statistical results of the final model show that R2= 0.982 4 and S=0.869 8 (where R is the correlation coefficient and S is the standard deviation). To test its predictive ability,the model was further used to predict the 13C NMR spectra of the carbinol carbon atoms of other nine compounds which were not included in the developed model. The average relative errors are 0.94% and 1.70%,respectively,for the training set and the predictive set. The model is statistically significant and shows good stability for data variation as tested by the leave-one-out (LOO) cross-validation. The comparison with other approaches also reveals good performance of this method.展开更多
The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) in combination with solid p...The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) in combination with solid phase extraction(SPE). As the capsule’s main active component, chlorogenic acid comes from the extraction of Chinese herb medicine Flos Lonicerae. The chlorogenic acid in capsule was ultrasonically extracted at room temperature using pure water as solvent. The extracting solution was enriched and cleaned using HC-C18 SPE cartridge. The effect of ultrasonic extraction, sample pretreatment conditions via SPE and q NMR experimental conditions were investigated. The q NMR experiment conditions were selected using deuterated DMSO as solvent, calibrated 1,4-phthalaldehyde as internal standard, and P1(pulse width) = 14.4 μs, d1(pulse delay time) = 1 s, NS(number of scan) = 512. The 1 H NMR peaks of δ 6.138–6.182(H-8’, d, 1 H) of chlorogenic acid was chosen as the quantitative peaks. Method validation was performed, including precision(the intra-day RSD = 1.2% and the inter-day RSD = 1.5%), linearity(correlation coefficient r>0.9999), LOD(0.0017 mg/g) and LOQ(0.079 mg/g). The recovery of the SPE-q NMR was within the range of 100.2%–103.2%. The result showed that the method was stable, accurate and reliabile. Determined by the method, the chlorogenic acid in a real Shuanghuanglian capsule was within the range of 9.68–10.35 mg/g.展开更多
利用六西格玛设计(design for six Sigma,DFSS)方法,通过定量核磁共振碳谱(quantitative carbon nuclear magnetic resonance spectroscopy,^(13)C qNMR)对由11种已知烃类化合物组成的模型油品进行了芳香碳摩尔百分比[C(ar)%,简称芳碳率...利用六西格玛设计(design for six Sigma,DFSS)方法,通过定量核磁共振碳谱(quantitative carbon nuclear magnetic resonance spectroscopy,^(13)C qNMR)对由11种已知烃类化合物组成的模型油品进行了芳香碳摩尔百分比[C(ar)%,简称芳碳率]测定的系统研究,建立了C(ar)%与样品浓度Conc.、弛豫试剂浓度[Cr(acac)_3]和循环延迟D13个参数之间的数学模型,据此模型得到了优化的参数设置:Conc.为180mg/mL,[Cr(acac)_3]为12 mg/mL,D1为10.5 s.按此设置进行了8组验证实验,其结果重现性较好,相对标准偏差(relative standard deviation,RSD)为0.61%;准确性较高,达到99.0%~100.6%.该方法也可用于其它分析测试方法的系统研究,且实验结果对现行油品芳碳率测定标准中相关参数,如[Cr(acac)_3]和D1的设置能够提出补充性建议.展开更多
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。
基金Projects(20775010, 21075011) supported by the National Natural Science Foundation of ChinaProject(2008AA05Z405) supported by the National High-tech Research and Development Program of China+2 种基金Project(09JJ3016) supported by the Natural Science Foundation of Hunan Province, ChinaProject(09C066) supported by the Scientific Research Fund of Hunan Provincial Education Department, ChinaProject(2010CL01) supported by the Foundation of Hunan Provincial Key Laboratory of Materials Protection for Electric Power and Transportation, China
文摘A quantitative structure-spectrum relationship (QSSR) model was developed to simulate 13C nuclear magnetic resonance (NMR) spectra of carbinol carbon atoms for 55 alcohols. The proposed model,using multiple linear regression,contained four descriptors solely extracted from the molecular structure of compounds. The statistical results of the final model show that R2= 0.982 4 and S=0.869 8 (where R is the correlation coefficient and S is the standard deviation). To test its predictive ability,the model was further used to predict the 13C NMR spectra of the carbinol carbon atoms of other nine compounds which were not included in the developed model. The average relative errors are 0.94% and 1.70%,respectively,for the training set and the predictive set. The model is statistically significant and shows good stability for data variation as tested by the leave-one-out (LOO) cross-validation. The comparison with other approaches also reveals good performance of this method.
基金National Natural Science Foundation of China(Grant No.31671928)Natural Science Foundation of Shanghai(Grant No.15ZR1440800).
文摘The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) in combination with solid phase extraction(SPE). As the capsule’s main active component, chlorogenic acid comes from the extraction of Chinese herb medicine Flos Lonicerae. The chlorogenic acid in capsule was ultrasonically extracted at room temperature using pure water as solvent. The extracting solution was enriched and cleaned using HC-C18 SPE cartridge. The effect of ultrasonic extraction, sample pretreatment conditions via SPE and q NMR experimental conditions were investigated. The q NMR experiment conditions were selected using deuterated DMSO as solvent, calibrated 1,4-phthalaldehyde as internal standard, and P1(pulse width) = 14.4 μs, d1(pulse delay time) = 1 s, NS(number of scan) = 512. The 1 H NMR peaks of δ 6.138–6.182(H-8’, d, 1 H) of chlorogenic acid was chosen as the quantitative peaks. Method validation was performed, including precision(the intra-day RSD = 1.2% and the inter-day RSD = 1.5%), linearity(correlation coefficient r>0.9999), LOD(0.0017 mg/g) and LOQ(0.079 mg/g). The recovery of the SPE-q NMR was within the range of 100.2%–103.2%. The result showed that the method was stable, accurate and reliabile. Determined by the method, the chlorogenic acid in a real Shuanghuanglian capsule was within the range of 9.68–10.35 mg/g.
文摘利用六西格玛设计(design for six Sigma,DFSS)方法,通过定量核磁共振碳谱(quantitative carbon nuclear magnetic resonance spectroscopy,^(13)C qNMR)对由11种已知烃类化合物组成的模型油品进行了芳香碳摩尔百分比[C(ar)%,简称芳碳率]测定的系统研究,建立了C(ar)%与样品浓度Conc.、弛豫试剂浓度[Cr(acac)_3]和循环延迟D13个参数之间的数学模型,据此模型得到了优化的参数设置:Conc.为180mg/mL,[Cr(acac)_3]为12 mg/mL,D1为10.5 s.按此设置进行了8组验证实验,其结果重现性较好,相对标准偏差(relative standard deviation,RSD)为0.61%;准确性较高,达到99.0%~100.6%.该方法也可用于其它分析测试方法的系统研究,且实验结果对现行油品芳碳率测定标准中相关参数,如[Cr(acac)_3]和D1的设置能够提出补充性建议.
