期刊文献+
共找到732篇文章
< 1 2 37 >
每页显示 20 50 100
Urinary nuclear magnetic resonance spectroscopy of a Bangladeshi cohort with hepatitis-B hepatocellular carcinoma: A biomarker corroboration study 被引量:4
1
作者 I Jane Cox Abil E Aliev +7 位作者 Mary ME Crossey Mahvish Dawood Mamun Al-Mahtab Sheikh M Akbar Salimur Rahman Antonio Riva Roger Williams Simon D Taylor-Robinson 《World Journal of Gastroenterology》 SCIE CAS 2016年第16期4191-4200,共10页
AIM: To establish if a distinct urinary metabolic profile could be identified in Bangladeshi hepatitis-B hepatocellular carcinoma(HCC) patients compared to cirrhosis patients and controls. METHODS: Urine samples from ... AIM: To establish if a distinct urinary metabolic profile could be identified in Bangladeshi hepatitis-B hepatocellular carcinoma(HCC) patients compared to cirrhosis patients and controls. METHODS: Urine samples from 42 Bangladeshi patients with HCC(39 patients with hepatitis-B HCC), 47 with cirrhosis on a background of hepatitis B, 46 with chronic hepatitis B, and seven ethnically-matched healthy controls were analyzed using nuclear magnetic resonance(NMR) spectroscopy. A full dietary and medication history was recorded for each subject. The urinary NMR data were analyzed using principal component analysis(PCA) and orthogonal partial leastsquared discriminant analysis(OPLS-DA) techniques. Differences in relative signal levels of the most discriminatory metabolites identified by PCA and OPLSDA were compared between subject groups using an independent samples Kruskal-Wallis one-way analysis of variance(ANOVA) test with all pairwise multiple comparisons. Within the patient subgroups, the MannWhitney U test was used to compare metabolite levels depending on hepatitis B e-antigen(HBe Ag) status and treatment with anti-viral therapy. A BenjaminiHochberg adjustment was applied to acquire the level of significance for multiple testing, with a declared level of statistical significance of P < 0.05.RESULTS: There were significant differences in age(P < 0.001), weight(P < 0.001), and body mass index(P < 0.001) across the four clinical subgroups. Serum alanine aminotransferase(ALT) was significantly higher in the HCC group compared to controls(P < 0.001); serum α-fetoprotein was generally markedly elevated in HCC compared to controls; and serum creatinine levels were significantly reduced in the HCC group compared to the cirrhosis group(P = 0.004). A threefactor PCA scores plot showed clustering of the urinary NMR spectra from the four subgroups. Metabolites that contributed to the discrimination between the subgroups included acetate, creatine, creatinine, dimethyamine(DMA), formate, glycine, hippurate, and trimethylamine-N-oxide(TMAO). A comparison of relative metabolite levels confirmed that carnitine was significantly increased in HCC; and creatinine, hippurate, and TMAO were significantly reduced in HCC compared to the other subgroups. HBe Ag negative patients showed a significant increase in creatinine(P = 0.001) compared to HBe Ag positive patients in the chronic hepatitis B subgroup, whilst HBe Ag negative patients showed a significant decrease in DMA(P = 0.004) in the cirrhosis subgroup compared to HBe Ag positive patients. There were no differences in metabolite levels in HCC patients who did or did not receive antiviral treatment. CONCLUSION: Urinary NMR changes in Bangladeshi HCC were identified, corroborating previous findings from Egypt and West Africa. These findings could form the basis for the development of a cost-effective HCC dipstick screening test. 展开更多
关键词 URINARY metabolic profiling HEPATOCELLULAR carcinoma nuclear magnetic resonance spectroscopy Hepatit
下载PDF
Using Nuclear Magnetic Resonance and MS/MS Spectroscopy for the Identification of Brodimoprim Metabolites in Rat Urine 被引量:1
2
作者 Chun YANG Wen Yi HE +4 位作者 Li Jun LI Rui Ming XU Shou Ren ZHANG Zeper ABLIZ Yi Kang SI 《Chinese Chemical Letters》 SCIE CAS CSCD 2001年第6期513-516,共4页
Eight metabolites of brodimoprim (BDP) in rat urine were detected by NMR and ESIMS/MS. They were demethyl-BDP glucuronide, demethyl-BDP sulfurate, demethyl-BDP glucuronide sulfurate, alpha -hydroxyl-BDP, alpha -hydrox... Eight metabolites of brodimoprim (BDP) in rat urine were detected by NMR and ESIMS/MS. They were demethyl-BDP glucuronide, demethyl-BDP sulfurate, demethyl-BDP glucuronide sulfurate, alpha -hydroxyl-BDP, alpha -hydroxyl-BDP glucuronide, BDP sulfurate, N-oxide-BDP sulfurate, and alpha -hydroxyl-N-oxide-BDP sulfurate. All the sulfurates are reported for the first time. 展开更多
关键词 nuclear magnetic resonance spectroscopy MS/MS spectroscopy METABOLITES BRODIMOPRIM
下载PDF
Nuclear magnetic resonance spectroscopy is highly sensitive for lipid-soluble metabolites 被引量:1
3
作者 Haiyang Dai Bikai Hong +4 位作者 Zhifeng Xu Lian Ma Yaowen Chen Yeyu Xiao Renhua Wu 《Neural Regeneration Research》 SCIE CAS CSCD 2013年第22期2103-2110,共8页
Although the water-soluble metabolite profile of human mesenchymal stem cells is known, the lipid profile still needs further investigation. In this study, methanol-chloroform was used to extract lipid-soluble metabol... Although the water-soluble metabolite profile of human mesenchymal stem cells is known, the lipid profile still needs further investigation. In this study, methanol-chloroform was used to extract lipid-soluble metabolites and perchloric acid was used to extract water-soluble metabolites. Fur- thermore, a dual phase extraction method using methanol-chloroform and water was used to obtain both water and lipid fractions simultaneously. All metabolite extractions were analyzed on a 9.4T high-resolution nuclear magnetic resonance spectrometer. Metabolite resonance peaks were as- signed in the acquired spectra according to the chemical shift, and the extraction efficiency of dif- ferent methods was compared. Results showed that in the spectra of water-soluble extracts, major metabolites comprised low molecular weight metabolites, including lactate, acetic acid, fatty acids, threonine, glutamic acid, creatine, choline and its derivatives, while in the spectra of lipid-soluble extracts, most metabolites were assigned to fatty acids. Among the different extraction procedures, perchloric acid was more efficient in extracting water-soluble metabolites and methanol-chloroform was efficient in extracting organic components compared with the dual phase extraction method. Nuclear magnetic resonance spectroscopy showed that as low as 0.7 mg organic yield was enough to obtain clear resonance peaks, while about 6.0 mg water-soluble yield was needed to obtain rela- tively favorable spectral lines. These results show that the efficiency of extracting water and lipid fractions is higher using perchloric acid and methanol-chloroform compared with dual phase ex- traction and that nuclear magnetic resonance spectroscopy is highly sensitive for analyzing lipid-soluble extracts. 展开更多
关键词 neural regeneration nuclear magnetic resonance spectroscopy mesenchymal stem cells metabo-lite profiles extraction method optimization WATER-SOLUBLE lipid-soluble perchloric acid metha-nol-chloroform grants-supported paper NEUROREGENERATION
下载PDF
Conformational Analysis of γ-Butyrolactones by Nuclear Magnetic Resonance Spectroscopy
4
作者 Fu An KANG and Cheng Lie YIN (Department of Chemistry Beijing Normal University , Beijing 100875) 《Chinese Chemical Letters》 SCIE CAS CSCD 1997年第10期885-888,共4页
A series of trans-4, 5-disubstituted -γ-butyrolactones are found to assume two different envelope conformations by means of nuclear magnetic resonance spectroscopy.
关键词 Conformational Analysis of Butyrolactones by nuclear magnetic resonance spectroscopy
下载PDF
Crystallochemical Characterizations, Raman Spectroscopy and Studies Nuclear Magnetic Resonance (NMR) of Cu<sub>2</sub>Zn(Sn, Si)S<sub>4 </sub>Compounds for Photovoltaic Applications
5
作者 Mohamed Hamdi Messaoud Benamira 《Journal of Materials Science and Chemical Engineering》 2022年第1期24-40,共17页
In this study, Si-doped Cu<sub>2</sub>ZnSnS<sub>4</sub> compounds (Cu<sub>2</sub>ZnSn<sub>1-x</sub>Si<sub>x</sub>S<sub>4</sub>, 0 ≤ x ≤ 1) were... In this study, Si-doped Cu<sub>2</sub>ZnSnS<sub>4</sub> compounds (Cu<sub>2</sub>ZnSn<sub>1-x</sub>Si<sub>x</sub>S<sub>4</sub>, 0 ≤ x ≤ 1) were prepared by solid state reaction method for use of materials for photovoltaic cells. The structural and spectroscopic properties of the as-prepared compounds were studied by X-ray diffraction (XRD), <sup>119</sup>Sn, <sup>29</sup>Si and <sup>65</sup>Cu Magic Angle Spinning nuclear magnetic resonance (MAS NMR) and Raman spectroscopy. The Si-substitution in the Sn-site induces three different types of XRD patterns which depend largely on the Si content in the compound. For 0 ≤ x ≤ 0.5, XRD analysis reveals the presence of a pure tetragonal phase of solid solution with I-42m as a space group. Mixed tetragonal and orthorhombic phases were observed for 0.5 < x < 0.8, followed by a pure orthorhombic structure with a space group Pmn2<sub>1</sub> at high content of Si (x ≥ 0.8). <sup>119</sup>Sn MAS NMR spectra show the presence of Sn/Si disorder as a function of the Si content. The <sup>65</sup>Cu MAS NMR spectra of the quadratic solid solution confirm the presence of the two copper sites (Cu-2a and Cu-2c) at 780 ppm while in the case of the orthorhombic solid solution samples, a very broad band is observed. The optical properties were investigated of all compounds by UV-Vis diffuse reflectance and the obtained optical band gap values (1.31 to 2.43 eV) confirm a semiconductor character. 展开更多
关键词 Photovoltaic Cells Cu2ZnSnS4 nuclear magnetic resonance Raman spectroscopy
下载PDF
7.0T nuclear magnetic resonance evaluation of the amyloid beta(1–40) animal model of Alzheimer's disease: comparison of cytology verification 被引量:6
6
作者 Lei Zhang Shuai Dong +1 位作者 Guixiang Zhao Yu Ma 《Neural Regeneration Research》 SCIE CAS CSCD 2014年第4期430-435,共6页
3.0T magnetic resonance spectroscopic imaging brain function in Alzheimer's disease. However, is a commonly used method in the research ot the role of 7.0T high-field magnetic resonance spectroscopic imaging in brain... 3.0T magnetic resonance spectroscopic imaging brain function in Alzheimer's disease. However, is a commonly used method in the research ot the role of 7.0T high-field magnetic resonance spectroscopic imaging in brain function of Alzheimer's disease remains unclear. In this study, 7.0T magnetic resonance spectroscopy showed that in the hippocampus of Alzheimer's disease rats, the N-acetylaspartate wave crest was reduced, and the creatine and choline wave crest was elevated. This finding was further supported by hematoxylin-eosin staining, which showed a loss of hippocampal neurons and more glial cells. Moreover, electron microscopy showed neuronal shrinkage and mitochondrial rupture, and scanning electron microscopy revealed small size hippocampal synaptic vesicles, incomplete synaptic structure, and reduced number. Overall, the results revealed that 7.0T high-field nuclear magnetic resonance spectroscopy detected the lesions and functional changes in hippocampal neurons of Alzheimer's disease rats in vivo, allowing the possibility for assessing the success rate and grading of the amyloid beta (1-40) animal model of Alzheimer's disease. 展开更多
关键词 nerve regeneration Alzheimer's disease AΒ1-40 high-field functional magnetic resonance nuclear magnetic resonance spectroscopy NEUROPATHOLOGY N-ACETYLASPARTATE CREATINE CHOLINE hippocampus NSFC grant neural regeneration
下载PDF
Proton nuclear magnetic resonance-based metabonomic models for non-invasive diagnosis of liver fibrosis in chronic hepatitis C:Optimizing the classification of intermediate fibrosis 被引量:2
7
作者 Andrea Dória Batista Carlos Jonnatan Pimentel Barros +7 位作者 Tássia Brena Barroso Carneiro Costa Michele Maria Goncalves de Godoy Ronaldo Dionísio Silva Joelma Carvalho Santos Mariana Montenegro de Melo Lira Norma ThoméJucá Edmundo Pessoa de Almeida Lopes Ricardo Oliveira Silva 《World Journal of Hepatology》 CAS 2018年第1期105-115,共11页
AIM To develop metabonomic models(MMs), using 1 H nuclear magnetic resonance(NMR) spectra of serum, to predict significant liver fibrosis(SF: Metavir ≥ F2), advanced liver fibrosis(AF: METAVIR ≥ F3) and cirrhosis(C:... AIM To develop metabonomic models(MMs), using 1 H nuclear magnetic resonance(NMR) spectra of serum, to predict significant liver fibrosis(SF: Metavir ≥ F2), advanced liver fibrosis(AF: METAVIR ≥ F3) and cirrhosis(C: METAVIR = F4 or clinical cirrhosis) in chronic hepatitis C(CHC) patients. Additionally, to compare the accuracy of the MMs with the aspartate aminotransferase to platelet ratio index(APRI) and fibrosis index based on four factors(FIB-4). METHODS Sixty-nine patients who had undergone biopsy in the previous 12 mo or had clinical cirrhosis were included. The presence of any other liver disease was a criterion for exclusion. The MMs, constructed using partial least squares discriminant analysis and linear discriminant analysis formalisms, were tested by cross-validation, considering SF, AF and C. RESULTS Results showed that forty-two patients(61%) presented SF, 28(40%) AF and 18(26%) C. The MMs showed sensitivity and specificity of 97.6% and 92.6% to predict SF; 96.4% and 95.1% to predict AF; and 100% and 98.0% to predict C. Besides that, the MMs correctly classified all 27(39.7%) and 25(38.8%) patients with intermediate values of APRI and FIB-4, respectively. CONCLUSION The metabonomic strategy performed excellently in predicting significant and advanced liver fibrosis in CHC patients, including those in the gray zone of APRI and FIB-4, which may contribute to reducing the need for these patients to undergo liver biopsy. 展开更多
关键词 Metabolomics nuclear magnetic resonance spectroscopy Chronic HEPATITIS C Liver FIBROSIS Surrogate MARKERS
下载PDF
Nuclear magnetic resonance based metabolomics and liverdiseases:Recent advances and future clinical applications 被引量:6
8
作者 Roland Amathieu Mohamed Nawfal Triba +4 位作者 Corentine Goossens Nadia Bouchemal Pierre Nahon Philippe Savarin Laurence Le Moyec 《World Journal of Gastroenterology》 SCIE CAS 2016年第1期417-426,共10页
Metabolomics is defined as the quantitative measurement of the dynamic multiparametric metabolic response of living systems to pathophysiological stimuli or genetic modification.It is an"omics"technique that... Metabolomics is defined as the quantitative measurement of the dynamic multiparametric metabolic response of living systems to pathophysiological stimuli or genetic modification.It is an"omics"technique that is situated downstream of genomics,transcriptomics and proteomics.Metabolomics is recognized as a promising technique in the field of systems biology for the evaluation of global metabolic changes.During the last decade,metabolomics approaches have become widely used in the study of liver diseases for the detection of early biomarkers and altered metabolic pathways.It is a powerful technique to improve our pathophysiological knowledge of various liver diseases.It can be a useful tool to help clinicians in the diagnostic process especially to distinguish malignant and non-malignant liver disease as well as to determine the etiology or severity of the liver disease.It can also assess therapeutic response or predict drug induced liver injury.Nevertheless,the usefulness of metabolomics is often not understood by clinicians,especially the concept of metabolomics profiling or fingerprinting.In the present work,after a concise description of the different techniques and processes used in metabolomics,we will review the main research on this subject by focusing specifically on in vitro proton nuclear magnetic resonance spectroscopy based metabolomics approaches in human studies.We will first consider the clinical point of view enlighten physicians on this new approach and emphasis its future use in clinical"routine". 展开更多
关键词 Metabolomics In VITRO nuclear magneticresonance spectroscopy LIVER DISEASES CIRRHOSIS
下载PDF
Substituent, Temperature and Solvent Effects on the Keto-Enol EQUILIBRIUM in <i>&beta;</i>-Ketoamides: A Nuclear Magnetic Resonance Study
9
作者 Sergio L. Laurella Manuel González Sierra +1 位作者 Jorge J. P. Furlong Patricia E. Allegretti 《Open Journal of Physical Chemistry》 2013年第4期138-149,共12页
Substituent, temperature and solvent effects on tautomeric equilibria in several β-ketoamides have been investigated by means of nuclear magnetic resonance spectroscopy (NMR). Keto-enol equilibrium predominates over ... Substituent, temperature and solvent effects on tautomeric equilibria in several β-ketoamides have been investigated by means of nuclear magnetic resonance spectroscopy (NMR). Keto-enol equilibrium predominates over the amide-imidol one. The relative stability of the individual tautomers and the corresponding equilibrium shifts are explained considering electronic and steric effects and tautomer stabilization via internal hydrogen bonds. In solution, these compounds exist mainly as ketoamide and Z-enolamide tautomers, both presenting intramolecular hydrogen bonds. 展开更多
关键词 β-Ketoamides Keto-Enol EQUILIBRIUM nuclear magnetic resonance spectroscopy
下载PDF
缴获电子烟油样品中75种合成大麻素的^(1)H qNMR定量分析研究 被引量:2
10
作者 刘翠梅 贾薇 +1 位作者 宋春辉 花镇东 《分析测试学报》 CAS CSCD 北大核心 2023年第5期605-613,共9页
通过考察75种合成大麻素(SCRAs)的关键定量参数,首次建立了可用于电子烟油样品中75种SCRAs定量分析的核磁共振氢谱定量分析方法(^(1)H qNMR)。以1,3,5-三甲氧基苯为内标,将烟油样品经氘代甲醇稀释后直接进行分析。方法的定量下限为0.03%... 通过考察75种合成大麻素(SCRAs)的关键定量参数,首次建立了可用于电子烟油样品中75种SCRAs定量分析的核磁共振氢谱定量分析方法(^(1)H qNMR)。以1,3,5-三甲氧基苯为内标,将烟油样品经氘代甲醇稀释后直接进行分析。方法的定量下限为0.03%(质量分数),日内相对标准偏差(RSD)小于0.90%,日间RSD小于1.5%,基质加标回收率为93.3%~100%。采用1H qNMR法对19份缴获烟油样品中的4种合成大麻素3,3-二甲基-2-[1-(5-氟戊基)吲唑-3-甲酰氨基]丁酸甲酯(5F-ADB)、2-[1-(5-氟戊基)-1H-吲哚-3-甲酰氨基]-3,3-二甲基丁酸甲酯(5F-MDMB-PICA)、2-[1-(4-氟丁基)-1H-吲唑-3-甲酰氨基]-3,3-二甲基丁酸甲酯(4FMDMB-BUTINACA)、N-(1-氨基-3,3-二甲基-1-氧代丁-2-基)-1-丁基-1H-吲唑-3-甲酰胺(ADB-BUTINACA)进行定量分析,得到其含量范围为0.072%~2.056%。19份烟油样品的^(1)H qNMR定量结果与高效液相色谱法定量结果无显著性差异。该研究所建立的电子烟油中SCRAs的定量分析^(1)H qNMR法无需标准物质,操作简单,定量结果准确,解决了缺乏标准物质时复杂基质中SCRAs定量分析的难题。目前国内外尚未有采用^(1)H qNMR对电子烟油中75种SCRAs定量分析的报道。该研究进一步拓宽了^(1)H qNMR技术在禁毒领域的应用范围,为复杂基质中毒品和新精神活性物质的定量分析提供了新的思路。 展开更多
关键词 电子烟油 新精神活性物质(NPS) 合成大麻素 核磁共振氢谱定量分析
下载PDF
低场^(1)H qNMR定量分析缴获毒品中氯胺酮及4种掺杂物
11
作者 刘翠梅 宋春辉 +2 位作者 贾薇 花镇东 廖琦 《分析测试学报》 CAS CSCD 北大核心 2023年第6期755-761,共7页
建立了可同时定量分析缴获毒品中氯胺酮、二甲基砜、磺胺、烟酰胺和非那西丁的低场氢谱核磁共振定量方法(LF-^(1)H qNMR),并将其定量能力与高场氢谱核磁共振定量方法(HF-^(1)H qNMR)进行了比较。对于LF-^(1)H qNMR,氯胺酮和4种掺杂物的... 建立了可同时定量分析缴获毒品中氯胺酮、二甲基砜、磺胺、烟酰胺和非那西丁的低场氢谱核磁共振定量方法(LF-^(1)H qNMR),并将其定量能力与高场氢谱核磁共振定量方法(HF-^(1)H qNMR)进行了比较。对于LF-^(1)H qNMR,氯胺酮和4种掺杂物的日内相对标准偏差(RSD)、日间RSD和定量下限分别为0.50%~2.9%、2.0%~7.4%和0.3~5 mg/mL;对于HF-^(1)H qNMR,氯胺酮和4种掺杂物的日内RSD、日间RSD和定量下限分别为0.40%~1.1%、1.5%~3.9%和0.003~0.05 mg/mL。采用LF-^(1)H qNMR和HF-^(1)H qNMR对167份缴获氯胺酮样品进行定量分析,两种方法定量结果的相对误差均小于15%。LF-^(1)H qNMR测得氯胺酮、二甲基砜、磺胺、烟酰胺和非那西丁的纯度分别为13.5%~102.6%、1.1%~81.3%、2.6%~83.4%、1.8%~22.7%和3.4%~43.8%;HF-^(1)H qNMR测得的纯度分别为13.2%~99.7%、1.0%~78.4%、2.5%~75.9%、1.7%~21.3%和3.0%~43.5%。两种方法均可在不使用标准物质的情况下实现对氯胺酮和掺杂物的同时定量分析。虽然LF-^(1)H qNMR法的精密度和灵敏度略低于HF-^(1)H qNMR法,但其对复杂基质中多组分同时定量分析的能力较好。LF-^(1)H qNMR的仪器购置和日常维护费用远低于HF-^(1)H qNMR,未来将在法庭科学实验室中得到更广泛的应用。 展开更多
关键词 毒品 氯胺酮 掺杂物 定量分析 高场核磁共振 低场核磁共振
下载PDF
~1H-qNMR法同时测定保健食品中抗坏血酸同分异构体含量
12
作者 夏金涛 张莉 +5 位作者 刘迪 张恒 吴婉琴 陈冉 范小龙 朱松松 《中国食品添加剂》 CAS 北大核心 2023年第12期212-218,共7页
建立一种同时检测保健食品中抗坏血酸同分异构体含量的^(1)H-qNMR法。样品经偏磷酸水溶解超声提取,离心过膜后,取适量上清液于NMR管中,以对苯二酚为内标,以氘水为锁场溶剂,采用^(1)H-qNMR直接对保健食品中的抗坏血酸同分异构体进行定性... 建立一种同时检测保健食品中抗坏血酸同分异构体含量的^(1)H-qNMR法。样品经偏磷酸水溶解超声提取,离心过膜后,取适量上清液于NMR管中,以对苯二酚为内标,以氘水为锁场溶剂,采用^(1)H-qNMR直接对保健食品中的抗坏血酸同分异构体进行定性定量分析。结果表明:抗坏血酸同分异构体和和内标对苯二酚能够很好地分离,2种抗坏血酸的质量浓度在400~4500μg/mL范围内线性良好,相关系数R~2>0.99。方法的日内精密度为1.14%~2.47%,日间精密度为2.22%~3.87%;检出限(LOD)分别为120和130μg/mL;平均加标回收率为93.38%~108.15%,相对标准偏差(RSDs,n=6)为1.74%~4.46%。该方法简单高效、重现性好,10 min内即可完成测样。对市售不同剂型保健食品进行检测,均未检出异抗坏血酸。该方法与高效液相色谱法检测结果无显著性差异,适用于保健食品中抗坏血酸同分异构体含量的测定。 展开更多
关键词 定量核磁共振氢谱(~1H-qnmr) 高效液相色谱 抗坏血酸同分异构体 保健食品
下载PDF
农产品检测用脱氧雪腐镰刀菌烯醇纯度标准物质的研制 被引量:1
13
作者 孟佳佳 郭文博 +3 位作者 聂冬霞 韦阳 赵志辉 韩铮 《南京农业大学学报》 CAS CSCD 北大核心 2024年第3期564-574,共11页
[目的]本文旨在研制脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)国家级纯度标准物质,为农产品中DON的检测等工作提供物质基础。[方法]利用质量平衡法和定量核磁共振法对DON纯度标准物质进行纯度定值。质量平衡法包括采用液相色谱面积归一... [目的]本文旨在研制脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)国家级纯度标准物质,为农产品中DON的检测等工作提供物质基础。[方法]利用质量平衡法和定量核磁共振法对DON纯度标准物质进行纯度定值。质量平衡法包括采用液相色谱面积归一化法测定DON主成分含量,采用卡尔费休库仑法测定纯度标准物质中水分含量,采用顶空气相色谱-质谱法测定挥发性杂质含量,以及采用电感耦合等离子质谱法测定无机离子杂质含量。定量核磁共振法采用苯甲酸为内标,选择合适的共振峰,内标法定量标准物质的纯度,并对标准物质进行均匀性、稳定性检测和不确定度评估。[结果]质量平衡法的纯度定值结果为99.47%,定量核磁共振法定值结果为99.45%,最终所研制的DON纯度标准物质的纯度为99.5%,扩展不确定度为0.4%,均匀性良好,且满足12个月以上的稳定性要求。[结论]本试验所研制的DON纯度标准物质符合国家标准物质技术规范,目前已被批准为国家一级标准物质,并已被用于小麦、玉米等农产品实际检测过程中。 展开更多
关键词 脱氧雪腐镰刀菌烯醇 标准物质 质量平衡法 定量核磁共振法 不确定度评估
下载PDF
定量核磁共振波谱法快速测定灭火剂材料中全氟辛烷磺酰基化合物
14
作者 李杨 黄卫 +3 位作者 王畅 李洋 花磊 田颖 《分析测试技术与仪器》 CAS 2024年第1期33-38,共6页
泡沫灭火剂中全氟辛烷磺酰基化合物(PFOS)的使用受到严格管控.针对灭火剂中PFOS快速测定的需求,建立了基于19F的定量核磁共振波谱(qNMR)检测方法.方法以全氟丁基磺酸钾为标准物质,通过计算全氟丁基磺酸钾的-CF3在化学位移δ-78.94处19F... 泡沫灭火剂中全氟辛烷磺酰基化合物(PFOS)的使用受到严格管控.针对灭火剂中PFOS快速测定的需求,建立了基于19F的定量核磁共振波谱(qNMR)检测方法.方法以全氟丁基磺酸钾为标准物质,通过计算全氟丁基磺酸钾的-CF3在化学位移δ-78.94处19F特征峰和PFOS的-CF2在化学位移δ-117.12处19F特征峰的积分面积比值,进而实现PFOS定量分析.经测试,全氟丁基磺酸钾百分含量与定量峰面积线性相关系数为0.9955,检出限为0.024%,定量限为0.080%.8种灭火剂产品的定性测定结果与实际标注情况相吻合,其中4种泡沫灭火剂产品中PFOS含量在0.106%~1.339%之间.研究结果表明,方法受基质干扰小、检测速度快、灵敏度高,可为泡沫灭火剂中PFOS的管控提供可靠的检测方法与数据支撑. 展开更多
关键词 全氟辛烷磺酰基化合物 泡沫灭火剂 定量核磁共振波谱法 全氟丁基磺酸钾
下载PDF
俾路支褐煤有机结构特征及大分子模型构建
15
作者 任媛 莫文龙 +3 位作者 马亚亚 郭佳 魏贤勇 AKRAM Naeem 《洁净煤技术》 CAS CSCD 北大核心 2024年第6期75-84,共10页
以巴基斯坦俾路支褐煤(BL)为研究对象,由元素分析得出BL化学式为C_(167)H_(130)O_(53)N_(2)S。经X射线光电子能谱(XPS)分析BL有机结构中氧、氮和硫元素存在形式。利用傅里叶变换红外光谱(FT-IR)研究BL有机结构中主要官能团特征,-CH和-CH... 以巴基斯坦俾路支褐煤(BL)为研究对象,由元素分析得出BL化学式为C_(167)H_(130)O_(53)N_(2)S。经X射线光电子能谱(XPS)分析BL有机结构中氧、氮和硫元素存在形式。利用傅里叶变换红外光谱(FT-IR)研究BL有机结构中主要官能团特征,-CH和-CH^(2)为BL脂肪族结构中主要官能团。BL中苯环主要取代形式为三取代和四取代。运用核磁共振光谱(^(13)C-NMR)探究BL有机结构碳骨架结构。BL分子结构中,芳香桥碳与周碳之比X_(BP)为0.21,碳主要由芳香碳和脂肪碳2部分构成,其中脂肪碳质量分数53.23%,芳香碳占比41.93%。芳香结构以苯环和萘环为主,氧主要以羧基、羰基、醚氧和酚羟基形式存在,而氮主要以吡咯氮形式存在,硫主要为噻吩。建立BL二维分子结构模型,通过Materials Studio对其进行加氢饱和,构建BL分子模型三维立体结构,进一步优化所得分子模型,空间效果显著,得到能量最低的BL三维结构模型,发现范德华能是BL分子结构稳定的关键因素。通过计算得到的BL模型结构^(13)C NMR谱图与试验所测谱图基本一致,验证了所构建BL结构模型的合理性。 展开更多
关键词 褐煤 分子结构 核磁共振碳谱 红外光谱 X射线光电子能谱
下载PDF
基于元素俘获谱测井和核磁共振测井的碳酸盐岩储层硅化作用类型判别
16
作者 王士新 杨志国 +3 位作者 刘晓亮 赵德丽 李怀彪 刘厚武 《测井技术》 CAS 2024年第1期94-100,共7页
硅化作用在巴西桑托斯盆地A油田广泛发育,对储层物性有很大影响。在前人对该区硅化作用研究的基础上,以常规测井、元素俘获谱测井和核磁共振测井综合分析为主要手段,结合储层物性数据、X衍射数据和薄片等资料,将硅化作用成因类型进行了... 硅化作用在巴西桑托斯盆地A油田广泛发育,对储层物性有很大影响。在前人对该区硅化作用研究的基础上,以常规测井、元素俘获谱测井和核磁共振测井综合分析为主要手段,结合储层物性数据、X衍射数据和薄片等资料,将硅化作用成因类型进行了进一步细分,分析了不同硅化作用对储层物性的影响,总结出不同硅化作用的典型测井响应特征和判别方法。研究表明,不同硅化类型对储层物性影响不同,早成岩a型对储层物性的影响较小,早成岩b型和后热液b型储层物性随硅质含量的增加而变差,后热液a型储层物性变得极差,非该区域有效储层。在元素俘获谱测井定量计算地层硅质含量的基础上,综合分析常规测井和核磁共振测井曲线特征可以判别出碳酸盐岩储层硅化作用类型,该研究对其他相似地区进行硅化作用类型判别有借鉴意义。 展开更多
关键词 硅化作用 核磁共振测井 元素俘获谱测井 储层物性 桑托斯盆地
下载PDF
台式小核磁共振波谱法测定聚乙烯密度
17
作者 张强 李虞 +2 位作者 张仲明 杨利娟 孙惠 《石油化工》 CAS CSCD 北大核心 2024年第1期84-89,共6页
以密度梯度柱法测得的线型低密度聚乙烯(LLDPE)试样的密度为标准,建立了台式小核磁共振波谱法(简称小核磁法)测试LLDPE密度的标准曲线,分析了试样存放时间、恒温测试温度、存放温度对小核磁法准确度和重复性的影响。实验结果表明,存放时... 以密度梯度柱法测得的线型低密度聚乙烯(LLDPE)试样的密度为标准,建立了台式小核磁共振波谱法(简称小核磁法)测试LLDPE密度的标准曲线,分析了试样存放时间、恒温测试温度、存放温度对小核磁法准确度和重复性的影响。实验结果表明,存放时间60~120 d的LLDPE试样可用作标准试样;恒温温度分别为35.0℃和34.5℃时,小核磁法测得的密度与密度梯度柱法得到的密度较吻合。造粒后LLDPE立即在-23℃下冷冻后可用于建立标准曲线。利用标准曲线,对生产装置取出的试样立刻用小核磁法测试密度,结果满足重复性与准确度的要求。小核磁法测密度快速且可批量测试,节省人力和时间,维护简单,健康环保。利用LLDPE粒料存放时间与小核磁法密度的关系表,可通过小核磁法快速准确测定已知生产时间的LLDPE的密度。 展开更多
关键词 小核磁共振波谱法 密度 恒温温度 重复性
下载PDF
冬虫夏草成分分析技术进展
18
作者 胡西娅 潘绮慧 +10 位作者 纪博睿 安亚彬 祁艳 拉珍 金美洛布 格桑珠嘎 朗杰 德庆央宗 任克京 潘英妮 王硕 《化学分析计量》 CAS 2024年第7期124-129,共6页
综述了冬虫夏草成分分析技术进展。冬虫夏草成分分析技术主要包括色谱及其联用技术、光谱技术、核磁共振波谱技术等。色谱及其联用技术操作简单、分离效果好、效率高、易于自动化,广泛用于冬虫夏草核苷类、多糖类和甾醇类等成分的分离... 综述了冬虫夏草成分分析技术进展。冬虫夏草成分分析技术主要包括色谱及其联用技术、光谱技术、核磁共振波谱技术等。色谱及其联用技术操作简单、分离效果好、效率高、易于自动化,广泛用于冬虫夏草核苷类、多糖类和甾醇类等成分的分离分析中;光谱技术分析速度快,检出限低、灵敏度高,能够精准实现冬虫夏草多糖类、氨基酸和重金属的定性定量分析;核磁共振波谱技术常用于辨别复杂混合物的化学性质,具有高重现性、非选择性、非破坏性等特点,能对冬虫夏草多种成分进行同步分析。提高冬虫夏草成分分析灵敏度与精确度,降低其检出限,研发出更多的新型分析技术与多技术联用将会是未来发展的重点方向。 展开更多
关键词 分析技术 冬虫夏草 色谱 光谱 核磁共振波谱
下载PDF
高温高压降解制备低分子量水溶性酵母葡聚糖
19
作者 王寒梅 刘垚 +1 位作者 何启煜 赵雪 《食品研究与开发》 CAS 2024年第4期96-102,共7页
以啤酒酵母粉为原料,利用硫酸苯酚法和高效凝胶排阻色谱法,分析在压力为0.1MPa时不同温度条件下降解得到的水溶性酵母葡聚糖的得率和分子量,并利用傅里叶变换红外光谱和核磁共振波谱技术,分析不同降解条件下水溶性酵母葡聚糖结构的变化... 以啤酒酵母粉为原料,利用硫酸苯酚法和高效凝胶排阻色谱法,分析在压力为0.1MPa时不同温度条件下降解得到的水溶性酵母葡聚糖的得率和分子量,并利用傅里叶变换红外光谱和核磁共振波谱技术,分析不同降解条件下水溶性酵母葡聚糖结构的变化。研究结果表明,120℃条件下水溶性酵母葡聚糖得率低于20%。而温度升高到135℃,pH值在3~5之间可以使水溶性酵母葡聚糖得率升高到60%~80%。pH值越低,水解时间越长,制备出水溶性酵母葡聚糖和葡寡糖得率越高。135℃、pH3降解3.0~6.0 h,主要得到葡寡糖,得率可达79.89%;pH4降解4.0~6.0 h、pH5降解6.0 h,主要得到12~100 kDa的水溶性酵母葡聚糖。傅里叶变换红外光谱和核磁共振波谱结果发现,高温高压降解后该葡聚糖仍以β-(1,3)为主链,以β-(1,6)为支链。但是pH值越低,β-(1,6)支链含量越低,pH3时β-(1,6)/β-(1,3)积分最低,为0.61。因此,通过控制降解的pH值、温度和时间,高温高压降解法可以有效制备不同分子量的水溶性酵母葡聚糖和葡寡糖。 展开更多
关键词 酵母 水溶性酵母葡聚糖 高温高压降解 傅里叶变换红外光谱 核磁共振波谱
下载PDF
蔗渣生物炭对岩溶峰丛洼地石灰土土-水特征曲线的影响
20
作者 王创业 李科 +2 位作者 郏金晨 徐煜 徐勤学 《佳木斯大学学报(自然科学版)》 CAS 2024年第4期102-107,共6页
岩溶地区岩石裸露、土壤浅薄且持水能力较低,其土壤水分保持和运动状况是其水土漏失治理的重要因素。生物炭拥有多孔结构和高比表面积,能改变土壤持水能力,但其种类、粒径、添加量和土壤类型等因素对土壤持水能力产生正面或负面作用,为... 岩溶地区岩石裸露、土壤浅薄且持水能力较低,其土壤水分保持和运动状况是其水土漏失治理的重要因素。生物炭拥有多孔结构和高比表面积,能改变土壤持水能力,但其种类、粒径、添加量和土壤类型等因素对土壤持水能力产生正面或负面作用,为了研究添加不同比例蔗渣生物炭对岩溶峰丛洼地石灰土持水特性的影响,选取位于广西河池地区岩溶峰丛洼地的石灰土壤作为试验样本,分别添加不同比例生物炭(0%,2%,4%,6%),利用滤纸法测定生物炭-石灰土混合土在0~40MPa吸附能力下土水特性曲线,并使用扫描电子显微镜(SEM)和核磁共振波谱法(NMR),观察生物炭-石灰土混合土的微观孔隙结构。研究结果表明:当土壤含水量超过30%时,不同比例生物炭掺入量的持水能力相似,土壤的持水性并不会随着生物炭掺入量的增加而持续提升。在添加生物炭0%,2%,4%时混合土的持水能力是在逐渐提高的,添加4%和6%时混合土的持水能力基本一致,这表明添加生物炭存在一个最优值和适用范围。建议岩溶峰丛地区石灰土含水率在30%以下时,施加4%~6%的蔗渣生物炭,可提高土壤的持水能力。 展开更多
关键词 岩溶峰丛洼地土壤 生物炭 滤纸法 土-水特征曲线 核磁共振波谱法
下载PDF
上一页 1 2 37 下一页 到第
使用帮助 返回顶部