The availability of liquid chromatography ultraviolet nuclear magnetic resonance mass spectrometry (LC UV NMR MS)integrated systems is providing greater information content and confidence for a variety of sample types...The availability of liquid chromatography ultraviolet nuclear magnetic resonance mass spectrometry (LC UV NMR MS)integrated systems is providing greater information content and confidence for a variety of sample types, such asdrug metabolites, natural products, impurities, and degradants. A wide range of experimental strategies can be pur sued,highlighting the flexibility and performance possible with this multihyphenated technique.展开更多
目的应用质谱核磁共振（1H-nuclear magnetic resonance,1H-NMR）代谢组技术研究维吾尔族原发性高血压（高血压）患者和健康正常人血清中代谢物,筛选维吾尔族高血压患者特征代谢物,并从代谢途径探讨高血压发病机制。方法 256例维吾尔族...目的应用质谱核磁共振（1H-nuclear magnetic resonance,1H-NMR）代谢组技术研究维吾尔族原发性高血压（高血压）患者和健康正常人血清中代谢物,筛选维吾尔族高血压患者特征代谢物,并从代谢途径探讨高血压发病机制。方法 256例维吾尔族观察对象进入研究范围（高血压组为157,正常组为99例）,均来自新疆医科大学高血压研究组2009~2012年在新疆和田策勒县的维吾尔族人群流行病学调查,其中维吾尔族要求三代血亲为本民族血统。高血压组和正常对照组血清标本采用Inova600型核磁共振波谱仪分别进行1H-NMR实验,采集NMR谱图后进行数据预处理。鉴定高血压患者和健康者血清中差异性代谢成分,根据差异性代谢物信息构建与高血压相关的代谢途径网络。结果两组年龄、体质量、身高和血清三酰甘油、低密度脂蛋白胆固醇浓度比较,差异无统计意义（P〉0.05）;两组空腹血糖、收缩压、舒张压和血清高密度脂蛋白胆固醇、总胆固醇浓度比较,差异有统计学意义（P〈0.05）。正交偏最小二乘判别分析（orthogonal partial least squares discriminant analysis,OPLS-DA）结果显示主成分积分值集中分布于椭圆形散点图（95%置信区间内）的4个区域,从得分图和3D空间分布图中可以明确两组的分布区域完全分开,高血压组与正常组血清在代谢成分上有明显差异,鉴定出12种差异性代谢物。高血压组与正常组比较,血清中多种氨基酸浓度显著降低,包括缬氨酸、丙氨酸、丙酮酸、肌醇、酪氨酸、甲基组氨酸等,差异有统计学意义（P〈0.05）。高血压组者血清中血清极低密度脂蛋白胆固醇、低密度脂蛋白胆固醇、乳酸、丙酮较正常组增加,差异有统计学意义（P〈0.05）。结论 1H-NMR代谢组技术结合OPLS-DA模式识别方法是高通量筛选高血压患者血清中代谢物差异表达的有效研究手段。使用OPLSDA对NMR谱数据进行模式识别分析,可以区分高血压患者和健康正常人代谢物的差异。维吾尔族高血压患者体内的代谢表型发生了显著变异,12种特征代谢物有可能是高血压的血清潜在生物标记物。展开更多
Objective： To evaluate the clinical application of proton magnetic resonance spectroscopy （1HMRS） in patients with radiotherapy treated intracranial tumors. Methods： Forty patients with intracranial tumors underwe...Objective： To evaluate the clinical application of proton magnetic resonance spectroscopy （1HMRS） in patients with radiotherapy treated intracranial tumors. Methods： Forty patients with intracranial tumors underwent multivoxel 1HMRS examination before and after radiotherapy. The concentrations of N-acetyl aspartate （NAA）, choline （Cho） and creatine （Cr） were obtained both in the tumors and the contralateral normal brain regions, The ratios of NANCr, Cho/Cr and Cho/NAA were calculated at the same time and follow-up one year. Results： （1） After radiotherapy, tumors inhibited by radiation had decreased Cho, NAA and Cr on proton MRS. Some cases showed necrotic wave. （2） During the one year follow-up, local tumor recurred in 8 cases and their Cho and Cho/NAA increased high again. Other cases without recurrence, HMRS showed no change. Conclusion： Multivoxel proton MR spectroscopy is available for study of tumor metabolites after radiotherapy and it is a valuable method in the evaluation of radiotherapy treated tumors,展开更多
Objective： To explore water soluble metabolite features of brain tumor specimens with HRMAS-^1HMRS and its potential clinical value. Methods： There were thirty cases of pathologically proven brain tumor, including 6...Objective： To explore water soluble metabolite features of brain tumor specimens with HRMAS-^1HMRS and its potential clinical value. Methods： There were thirty cases of pathologically proven brain tumor, including 6 Ⅰ-Ⅱ grade astrocytomas, 7 Ⅲ grade anaplastic astrocytomas, 10 IV grade glioblastomas and 7 meningiomas. Used Varian Company 600 MHz spectrometer with the Nano-probe for acquisition HRMASJHMRS, which was postprocessed with jMRUI 3.2 version software. These metabolic probability and their ratios to Cr were summed. Results： （1） HRMAS-^1HMRS could resolve NAA, PCr/Cr, GPC ± PCho ± Cho, Glu/GIn, Gly, Tau, Ala, Lac, ml and so on. All samples showed Lac, 6 samples showed unknown single peak at 3.72 ppm or 3.90 ppm. （2） The mean Cho/Cr of 6 Ⅰ-ⅡI grade astrocytomas was 2.42 ± 1.01 （P = 0.003, compared with glioblastoma）. The mean Cho/Cr of 7 anaplastic astrocytomas was 3.48 ± 0.59 （P = 0.01, compared with glioblastoma）. The Cho/Cr of 10 glioblastomas broadly ranged from 0.9 to 11.3 （mean 5.40 ± 1.23）. From Ⅰ-Ⅱ grade astrocytoma to glioblastoma, Ala/Cr, Tau/Cr and Gly/Cr trends were increased; the mean Ala/Cr of glioma was 0.31 ± 0.13. （3） Meningiomas showed higher Ala and Cho. Their Cr was lower than that of gliomas. 4/7 cases had no NAA, 3/7 patients had lower NAA. Mean Cho/Cr was 3.56 ± 1.01, Ala/Cr was 0.53 ±0.28 （P = 0.006, compared with glioma）. Conclusion： HRMAS-^1HMRS can show further details in vivo MRS, resolve in vivo spectroscopic metabolite of Cho compound and differentiate the extent of benign and malignant glioma. With the increase in the malignant degree of gliomas, Cho, ml, Ala, Tau and Gly will increase. HRMAS-^1HMRS is the only method of isotropic spectroscopy for pathological specimens.展开更多
Proton magnetic resonance spectroscopy (1H MRS) can provide specific biochemical information within breast lesions and the elevated composite choline concentration as a useful diagnostic tool has been used to distingu...Proton magnetic resonance spectroscopy (1H MRS) can provide specific biochemical information within breast lesions and the elevated composite choline concentration as a useful diagnostic tool has been used to distinguish malignant from benign breast lesions, early evaluate response to therapy and predict prognosis. However, several obstacles including poor spatial resolution, low signal-to-noise ratio (SNR), long acquisition time and the difficulty of "extra" lipid suppression may have a negative impact on the routine application of in vivo 1H MRS for human breast cancer. At present, optimization H MRS methodology for breast studies has been performed.展开更多
High-temperature coal tar was extracted with petroleum ether （PE） under ultrasonic irradiation and the extracts were analyzed with gas chromatograph/mass spectrometer. The acearylene fractions including acenaphthyle...High-temperature coal tar was extracted with petroleum ether （PE） under ultrasonic irradiation and the extracts were analyzed with gas chromatograph/mass spectrometer. The acearylene fractions including acenaphthylene, aceanthrylene and cyclopentapyrene were enriched together and named E, which was then transferred to a car- tridge in Isolera-One flash chromatography. Three groups of compounds were eluted out with ethyl acetate/PE mixed solvent （volume ratio 1：9） and named E1, E2 and E3 according to their main components. Acenaphthylene accounted for 78.2% in El, aceanthrylene 71.6% in E2 and cyclopentapyrene 75.9% in E3, respectively. The three groups of acearylenes were purified by Sephadex LH-20 column chromatography with ethanol/cyclohexane mixed solvent （vol- ume ratio 1：4）, and then confirmed with nuclear magnetic resonance spectrometer. This method indicates that flash chromatography has a good effect on separating the compounds with a similar structnre after extraction under ultrasonic irradiation.展开更多
The Mycobacterium tuberculosis protein Rv2302 has been characterized using nuclear magnetic resonance （NMR） and circular dichroism （CD） spectroscopy. While the biochemical function of Rv2302 is still unknown, rece...The Mycobacterium tuberculosis protein Rv2302 has been characterized using nuclear magnetic resonance （NMR） and circular dichroism （CD） spectroscopy. While the biochemical function of Rv2302 is still unknown, recent microarray analyses show that Rv2302 is upregulated in response to starvation and overexpression of heat shock proteins and, consequently, may play a role in the biochemical processes associated with these events. Rv2302 is a monomer in solution as shown by size exclusion chromatography and NMR spectroscopy. CD spectroscopy suggests that Rv2302 partially unfolds upon heating and that this unfolding is reversible. Using NMR-based methods, the solution structure of Rv2302 was determined. The protein contains a five-strand, antiparalle β-sheet core with one C-terminal α-helix （A61 to A75） nestled against its side. Hydrophobic interactions between residues in the α-helix and β-strands 3 and 4 hold the α-helix near the β-sheet core. The electrostatic potential on the solvent-accessible surface is primarily negative with the exception of a positive arginine pocket composed of residues R18, R70, and R74. Steady-state {^1H}-^15N heteronuclear nuclear Overhauser effects indicate that the protein＇s core is rigid on the picosecond timescale. The absence of amide cross-peaks for residues G 13 to H 19 in the ^1H-^15N heteronuclear single quantum correlation spectrum suggests that this region, a loop between β-strands 1 and 2, undergoes motion on the millisecond to microsecond timescale. Dali searches using the structure closest to the average structure do not identify any high similarities to any other known protein structure, suggesting that the structure of Rv2302 may represent a novel protein fold.展开更多
A range of new compounds such as N1,N4-bis（diphenylmethlene）benzene-l,4-diamine zirconium （IV） chloride [{（Ar）2NC6HsN（Ar）z}ZrCl4] （Ar = C6H5） complex counting the chelating amine and chloride in position tra...A range of new compounds such as N1,N4-bis（diphenylmethlene）benzene-l,4-diamine zirconium （IV） chloride [{（Ar）2NC6HsN（Ar）z}ZrCl4] （Ar = C6H5） complex counting the chelating amine and chloride in position trans have been prepared. Well-defined NI,N4-bis（diphenylmethlene）benzene-l,4-diamine zirconium （IV） chloride [{（Ar）2NC6H5N（Ar）2}ZrCl4] （Ar = C6H5） was obtained by stoichiometric addition of {（Ar）2NC6H5N（Ar）2} （Ar = C6H5） and {ZrC14} in ethanol at reflex temperature. IR, 1H NMR, electronic properties using hyperchem program study has been improved for this compound such as bond distance, and this compound was also defined as electric conductivity which proves to be useful for conductively compound.展开更多
文摘The availability of liquid chromatography ultraviolet nuclear magnetic resonance mass spectrometry (LC UV NMR MS)integrated systems is providing greater information content and confidence for a variety of sample types, such asdrug metabolites, natural products, impurities, and degradants. A wide range of experimental strategies can be pur sued,highlighting the flexibility and performance possible with this multihyphenated technique.
文摘目的应用质谱核磁共振（1H-nuclear magnetic resonance,1H-NMR）代谢组技术研究维吾尔族原发性高血压（高血压）患者和健康正常人血清中代谢物,筛选维吾尔族高血压患者特征代谢物,并从代谢途径探讨高血压发病机制。方法 256例维吾尔族观察对象进入研究范围（高血压组为157,正常组为99例）,均来自新疆医科大学高血压研究组2009~2012年在新疆和田策勒县的维吾尔族人群流行病学调查,其中维吾尔族要求三代血亲为本民族血统。高血压组和正常对照组血清标本采用Inova600型核磁共振波谱仪分别进行1H-NMR实验,采集NMR谱图后进行数据预处理。鉴定高血压患者和健康者血清中差异性代谢成分,根据差异性代谢物信息构建与高血压相关的代谢途径网络。结果两组年龄、体质量、身高和血清三酰甘油、低密度脂蛋白胆固醇浓度比较,差异无统计意义（P〉0.05）;两组空腹血糖、收缩压、舒张压和血清高密度脂蛋白胆固醇、总胆固醇浓度比较,差异有统计学意义（P〈0.05）。正交偏最小二乘判别分析（orthogonal partial least squares discriminant analysis,OPLS-DA）结果显示主成分积分值集中分布于椭圆形散点图（95%置信区间内）的4个区域,从得分图和3D空间分布图中可以明确两组的分布区域完全分开,高血压组与正常组血清在代谢成分上有明显差异,鉴定出12种差异性代谢物。高血压组与正常组比较,血清中多种氨基酸浓度显著降低,包括缬氨酸、丙氨酸、丙酮酸、肌醇、酪氨酸、甲基组氨酸等,差异有统计学意义（P〈0.05）。高血压组者血清中血清极低密度脂蛋白胆固醇、低密度脂蛋白胆固醇、乳酸、丙酮较正常组增加,差异有统计学意义（P〈0.05）。结论 1H-NMR代谢组技术结合OPLS-DA模式识别方法是高通量筛选高血压患者血清中代谢物差异表达的有效研究手段。使用OPLSDA对NMR谱数据进行模式识别分析,可以区分高血压患者和健康正常人代谢物的差异。维吾尔族高血压患者体内的代谢表型发生了显著变异,12种特征代谢物有可能是高血压的血清潜在生物标记物。
基金a grant from the Medical Foundation of Wu Jieping(No.32067000501).
文摘Objective： To evaluate the clinical application of proton magnetic resonance spectroscopy （1HMRS） in patients with radiotherapy treated intracranial tumors. Methods： Forty patients with intracranial tumors underwent multivoxel 1HMRS examination before and after radiotherapy. The concentrations of N-acetyl aspartate （NAA）, choline （Cho） and creatine （Cr） were obtained both in the tumors and the contralateral normal brain regions, The ratios of NANCr, Cho/Cr and Cho/NAA were calculated at the same time and follow-up one year. Results： （1） After radiotherapy, tumors inhibited by radiation had decreased Cho, NAA and Cr on proton MRS. Some cases showed necrotic wave. （2） During the one year follow-up, local tumor recurred in 8 cases and their Cho and Cho/NAA increased high again. Other cases without recurrence, HMRS showed no change. Conclusion： Multivoxel proton MR spectroscopy is available for study of tumor metabolites after radiotherapy and it is a valuable method in the evaluation of radiotherapy treated tumors,
文摘Objective： To explore water soluble metabolite features of brain tumor specimens with HRMAS-^1HMRS and its potential clinical value. Methods： There were thirty cases of pathologically proven brain tumor, including 6 Ⅰ-Ⅱ grade astrocytomas, 7 Ⅲ grade anaplastic astrocytomas, 10 IV grade glioblastomas and 7 meningiomas. Used Varian Company 600 MHz spectrometer with the Nano-probe for acquisition HRMASJHMRS, which was postprocessed with jMRUI 3.2 version software. These metabolic probability and their ratios to Cr were summed. Results： （1） HRMAS-^1HMRS could resolve NAA, PCr/Cr, GPC ± PCho ± Cho, Glu/GIn, Gly, Tau, Ala, Lac, ml and so on. All samples showed Lac, 6 samples showed unknown single peak at 3.72 ppm or 3.90 ppm. （2） The mean Cho/Cr of 6 Ⅰ-ⅡI grade astrocytomas was 2.42 ± 1.01 （P = 0.003, compared with glioblastoma）. The mean Cho/Cr of 7 anaplastic astrocytomas was 3.48 ± 0.59 （P = 0.01, compared with glioblastoma）. The Cho/Cr of 10 glioblastomas broadly ranged from 0.9 to 11.3 （mean 5.40 ± 1.23）. From Ⅰ-Ⅱ grade astrocytoma to glioblastoma, Ala/Cr, Tau/Cr and Gly/Cr trends were increased; the mean Ala/Cr of glioma was 0.31 ± 0.13. （3） Meningiomas showed higher Ala and Cho. Their Cr was lower than that of gliomas. 4/7 cases had no NAA, 3/7 patients had lower NAA. Mean Cho/Cr was 3.56 ± 1.01, Ala/Cr was 0.53 ±0.28 （P = 0.006, compared with glioma）. Conclusion： HRMAS-^1HMRS can show further details in vivo MRS, resolve in vivo spectroscopic metabolite of Cho compound and differentiate the extent of benign and malignant glioma. With the increase in the malignant degree of gliomas, Cho, ml, Ala, Tau and Gly will increase. HRMAS-^1HMRS is the only method of isotropic spectroscopy for pathological specimens.
文摘Proton magnetic resonance spectroscopy (1H MRS) can provide specific biochemical information within breast lesions and the elevated composite choline concentration as a useful diagnostic tool has been used to distinguish malignant from benign breast lesions, early evaluate response to therapy and predict prognosis. However, several obstacles including poor spatial resolution, low signal-to-noise ratio (SNR), long acquisition time and the difficulty of "extra" lipid suppression may have a negative impact on the routine application of in vivo 1H MRS for human breast cancer. At present, optimization H MRS methodology for breast studies has been performed.
基金Supported by National Natural Science Foundation of China for Innovative Research Group(No.50921002)the Program of the Universities in Jiangsu Province for Development of High-Tech Industries(No.JHB05-33)the Fundamental Research Funds for the Central Universities (China University of Mining and Technology,No.2010ZDP02B03)
文摘High-temperature coal tar was extracted with petroleum ether （PE） under ultrasonic irradiation and the extracts were analyzed with gas chromatograph/mass spectrometer. The acearylene fractions including acenaphthylene, aceanthrylene and cyclopentapyrene were enriched together and named E, which was then transferred to a car- tridge in Isolera-One flash chromatography. Three groups of compounds were eluted out with ethyl acetate/PE mixed solvent （volume ratio 1：9） and named E1, E2 and E3 according to their main components. Acenaphthylene accounted for 78.2% in El, aceanthrylene 71.6% in E2 and cyclopentapyrene 75.9% in E3, respectively. The three groups of acearylenes were purified by Sephadex LH-20 column chromatography with ethanol/cyclohexane mixed solvent （vol- ume ratio 1：4）, and then confirmed with nuclear magnetic resonance spectrometer. This method indicates that flash chromatography has a good effect on separating the compounds with a similar structnre after extraction under ultrasonic irradiation.
文摘The Mycobacterium tuberculosis protein Rv2302 has been characterized using nuclear magnetic resonance （NMR） and circular dichroism （CD） spectroscopy. While the biochemical function of Rv2302 is still unknown, recent microarray analyses show that Rv2302 is upregulated in response to starvation and overexpression of heat shock proteins and, consequently, may play a role in the biochemical processes associated with these events. Rv2302 is a monomer in solution as shown by size exclusion chromatography and NMR spectroscopy. CD spectroscopy suggests that Rv2302 partially unfolds upon heating and that this unfolding is reversible. Using NMR-based methods, the solution structure of Rv2302 was determined. The protein contains a five-strand, antiparalle β-sheet core with one C-terminal α-helix （A61 to A75） nestled against its side. Hydrophobic interactions between residues in the α-helix and β-strands 3 and 4 hold the α-helix near the β-sheet core. The electrostatic potential on the solvent-accessible surface is primarily negative with the exception of a positive arginine pocket composed of residues R18, R70, and R74. Steady-state {^1H}-^15N heteronuclear nuclear Overhauser effects indicate that the protein＇s core is rigid on the picosecond timescale. The absence of amide cross-peaks for residues G 13 to H 19 in the ^1H-^15N heteronuclear single quantum correlation spectrum suggests that this region, a loop between β-strands 1 and 2, undergoes motion on the millisecond to microsecond timescale. Dali searches using the structure closest to the average structure do not identify any high similarities to any other known protein structure, suggesting that the structure of Rv2302 may represent a novel protein fold.
文摘A range of new compounds such as N1,N4-bis（diphenylmethlene）benzene-l,4-diamine zirconium （IV） chloride [{（Ar）2NC6HsN（Ar）z}ZrCl4] （Ar = C6H5） complex counting the chelating amine and chloride in position trans have been prepared. Well-defined NI,N4-bis（diphenylmethlene）benzene-l,4-diamine zirconium （IV） chloride [{（Ar）2NC6H5N（Ar）2}ZrCl4] （Ar = C6H5） was obtained by stoichiometric addition of {（Ar）2NC6H5N（Ar）2} （Ar = C6H5） and {ZrC14} in ethanol at reflex temperature. IR, 1H NMR, electronic properties using hyperchem program study has been improved for this compound such as bond distance, and this compound was also defined as electric conductivity which proves to be useful for conductively compound.
