Herein, a strategy is proposed for the simultaneous determination of primary coumarins in Peucedani Radix(Chinese name: Qianhu). The methodology consists of three consecutive steps: 1) Semi-preparative LC in combinati...Herein, a strategy is proposed for the simultaneous determination of primary coumarins in Peucedani Radix(Chinese name: Qianhu). The methodology consists of three consecutive steps: 1) Semi-preparative LC in combination with a home-made automated fraction collection module to fragment the universal metabolome standard into ten fractions(Frs. I–X); 2) LC–accurate MS/MS and quantitative1 H NMR spectroscopy conducted in parallel to acquire the qualitative and quantitative data of each fraction; 3) Robust identification and quantification of components by use of LC coupled to multiple reaction monitoring. In this final step, the most significant fractions(Frs. III–X) were pooled to serve as the pseudo-mixed standard solution. Meticulous online parameter optimization was performed to obtain the optimal parameters, including ion transitions and collision energies. Concerns were particularly paid onto pursuing the parameters being capable of monitoring regiospecific isomers, notably praeruptorin E vs. 3′-isovaleryl-4′-angeloylkhellactone. The quantitative performance of the method was validated according to diverse assays. Eleven primary coumarins(1–11) were unambiguously identified and absolutely quantified, even though no external reference compound was used. Above all, the integrated strategy not only provides a feasible pipeline for the quality assessment of Peucedani Radix, but more importantly, shows the potential for authentic compound-free quantitative evaluation of traditional Chinese medicines.展开更多
为探究白花前胡和紫花前胡中代谢物的种类及相对含量,借助于广泛靶向代谢组学的方法,利用UPLC-MS技术对白花前胡和紫花前胡成分进行分析、鉴定,确定主要差异代谢产物,并对其进行相对定量分析;从整体角度出发,结合多元统计分析,对二者中...为探究白花前胡和紫花前胡中代谢物的种类及相对含量,借助于广泛靶向代谢组学的方法,利用UPLC-MS技术对白花前胡和紫花前胡成分进行分析、鉴定,确定主要差异代谢产物,并对其进行相对定量分析;从整体角度出发,结合多元统计分析,对二者中主要差异性成分进行系统鉴定,并对差异代谢物进行KEGG通路富集分析。从白花前胡和紫花前胡中共鉴定出12类1556个代谢产物,主要差异代谢物12类共1085种,其中酚酸类、黄酮类、木脂素及香豆素类、生物碱类和脂类等化合物差异较大,分别占比为19.2%、15.9%、10.1%、9.4%和9.2%;其中421种成分上调,664种成分下调。差异代谢产物以biosynthesis of phenylpropanoids(ko01061)、linoleic acidmetabolism(ko00591)、pentose phosphate pathway(ko00030)、biosynthesis of secondarymetabolites(ko01110)、phosphotransferase system(ko02060)、phenylalanine和Tyrosine and tryptophan biosynthesis(ko00400)等6条通路富集显著,主要为酚酸类、脂肪酸类等成分的关键代谢通路。研究表明,白花前胡和紫花前胡化学成分差异较大,2020版《中国药典》将其单列为不同的药材,具有一定的先进性。本研究可为白花前胡和紫花前胡的标准修订及品质评价提供参考。展开更多
基金financially supported by National Science Fund of China (Nos. 81773875,81403073 and 81530097)Quality Guarantee System of Chinese Herbal Medicines (No. 201507002)+1 种基金foundation from Beijing University of Chinese Medicine (No. 2016-JYB-XJQ004)the Macao Science and Technology Development Fund (007/2014/AMJ)
文摘Herein, a strategy is proposed for the simultaneous determination of primary coumarins in Peucedani Radix(Chinese name: Qianhu). The methodology consists of three consecutive steps: 1) Semi-preparative LC in combination with a home-made automated fraction collection module to fragment the universal metabolome standard into ten fractions(Frs. I–X); 2) LC–accurate MS/MS and quantitative1 H NMR spectroscopy conducted in parallel to acquire the qualitative and quantitative data of each fraction; 3) Robust identification and quantification of components by use of LC coupled to multiple reaction monitoring. In this final step, the most significant fractions(Frs. III–X) were pooled to serve as the pseudo-mixed standard solution. Meticulous online parameter optimization was performed to obtain the optimal parameters, including ion transitions and collision energies. Concerns were particularly paid onto pursuing the parameters being capable of monitoring regiospecific isomers, notably praeruptorin E vs. 3′-isovaleryl-4′-angeloylkhellactone. The quantitative performance of the method was validated according to diverse assays. Eleven primary coumarins(1–11) were unambiguously identified and absolutely quantified, even though no external reference compound was used. Above all, the integrated strategy not only provides a feasible pipeline for the quality assessment of Peucedani Radix, but more importantly, shows the potential for authentic compound-free quantitative evaluation of traditional Chinese medicines.
文摘为探究白花前胡和紫花前胡中代谢物的种类及相对含量,借助于广泛靶向代谢组学的方法,利用UPLC-MS技术对白花前胡和紫花前胡成分进行分析、鉴定,确定主要差异代谢产物,并对其进行相对定量分析;从整体角度出发,结合多元统计分析,对二者中主要差异性成分进行系统鉴定,并对差异代谢物进行KEGG通路富集分析。从白花前胡和紫花前胡中共鉴定出12类1556个代谢产物,主要差异代谢物12类共1085种,其中酚酸类、黄酮类、木脂素及香豆素类、生物碱类和脂类等化合物差异较大,分别占比为19.2%、15.9%、10.1%、9.4%和9.2%;其中421种成分上调,664种成分下调。差异代谢产物以biosynthesis of phenylpropanoids(ko01061)、linoleic acidmetabolism(ko00591)、pentose phosphate pathway(ko00030)、biosynthesis of secondarymetabolites(ko01110)、phosphotransferase system(ko02060)、phenylalanine和Tyrosine and tryptophan biosynthesis(ko00400)等6条通路富集显著,主要为酚酸类、脂肪酸类等成分的关键代谢通路。研究表明,白花前胡和紫花前胡化学成分差异较大,2020版《中国药典》将其单列为不同的药材,具有一定的先进性。本研究可为白花前胡和紫花前胡的标准修订及品质评价提供参考。
文摘针对轻质、异形不规则的宁前胡种子存在流动性差、易破损等难题,基于宁前胡的种子物性参数和种植农艺要求,设计了一种马蹄形轮式“条播”排种器。通过充种过程的分析,得知马蹄形型孔可提高种子流动性、减少种子损伤。利用Rocky Dem离散元仿真软件进行单因素试验,由Particles Energy Spectra模块分析种子与排种轮的碰撞能量预测种子破损情况。以排种轮转速和导种槽倾角为试验因素进行二次回归正交旋转组合试验,并利用回归模型进行参数优化。结果表明:当排种轮转速为31.75 r/min、导种槽倾角为31.05°时,排种性能最优,排种均匀性变异系数为11.37%、排量稳定性变异系数为1.02%。通过台架试验验证了不同型孔圆角半径对种子破损情况的变化趋势与仿真试验结果一致,证明了该方法的可行性。马蹄形轮式宁前胡“条播”排种器田间试验与台架试验结果基本一致,能满足宁前胡种植农艺要求。
