MOLECULES
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2018
·Vol. 23
·期 3
·554
·
IF 3.098
Qianqian Liang,Qiuying Wang,Yuan Wang,Ya-nan Wang,Jia Hao,Miaomiao Jiang
The primary metabolites in aqueous extract of mulberry (Morus albaL.) leaves were characterized by using proton nuclear magnetic resonance (1H-NMR) spectroscopy. With the convenience of resonance assignment, GABA together with the other 10 primary metabolites was simultaneously identified and quantified in one1H-NMR spectrum. In this study, external calibration curves for metabolites were employed to calculate the concentrations of interests. The proposed quantitative approach was demonstrated with good linearity (r2ranged in the interval of 0.9965–0.9999), precision, repeatability, stability (RSD values in the ranges of 0.35–4.89%, 0.77–7.13% and 0.28–2.33%, respectively) and accuracy (recovery rates from 89.2% to 118.5%). The established1H-NMR method was then successfully applied to quantify 11 primary metabolites in mulberry leaves from different geographical regions within a rapid analysis time and a simple sample preparation procedure.Keywords:quantitative1H-NMR;Morus alba;amino acids;saccharides;organic acids
研究领域:
分析化学
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植物科学
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代谢组学
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产品关联
DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
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2020
·
IF 4.972
Shanshan He,Yanling Wang,Jianhua Xie,Heng Gao,Xiujiang Li,Zhibing Huang
Monascus comprises purple-red molds. Various compounds can be obtained from these species, including statins and food-safe yellow, red, and orange pigments. However, the secondary metabolite citrinin, a mycotoxin, is produced during the late stages of growth. Citrinin biosynthesis should be reduced to apply Monascus pigments safely. Fortunately, this can be achieved by the addition of flavonoids (genistein, daidzein, apigenin, and kaempferol). However, the effects of these flavonoids on other metabolites remain unknown. Here, we report a 1 H NMR-based multivariate metabolomic analysis of the effects of flavonoids on mycotoxin citrinin production by Monascus . Fifteen metabolites involved in lysine and arginine biosynthesis and alanine, aspartate, glutamate, biotin, arginine, proline, and glutathione metabolism were detected. The reduction in glutamate, aspartate, biotin, and 2-phosphoglycerate content suggested their association with the citrinin reduction mechanism. This study identifies the citrinin production pathway in Monascus and will aid in the development of citrinin-control methods.
研究领域:
微生物学
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代谢组学
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食品科学
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DOI
高影响因子
FOOD CHEMISTRY
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2018
·
IF 4.946
MengTing Zhu,Ting Shi,Yi Chen,ShuHan Luo,Tuo Leng,YangLing Wang,Cong Guo,MingYong Xie
A rapid method for the determination of fatty acid (FA) composition in camellia oils was developed based on the 1 H NMR technique combined with partial least squares (PLS) method. Outliers detection, LVs optimization and data pre-processing selection were explored during the model building process. The results showed the optimal models for predicting the content of C18:1, C18:2, C18:3, saturated, unsaturated, monounsaturated and polyunsaturated FA were achieved by Pareto scaling (Par) pretreatment, with correlation coefficient ( R 2 ) above 0.99, the root mean square error of estimation and prediction (RMSEE, RMSEP) lower than 0.954 and 0.947, respectively. Mean-centering (Ctr) was more suitable for the model of C16:0 and C18:0 with the best performance indicators ( R 2 ≥ 0.945, RMSEE ≤ 0.377, RMSEP ≤ 0.212). This study indicated that 1 H NMR has the potential to be applied as a rapid and routine method for the analysis of FA composition in camellia oils.
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
MOLECULES
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2025
·Vol. 30
·期 14
·2942
·
IF 4.6
Xinyu Gao,Jiahao Niu,Zhengjian Xiao,Da Rong,Mingming Yu,Sherwin K B Sy,Cong Wang,Zhihua Lv
Melatonin supplements have been widely used to improve sleep quality and overcome sleep disorders, with melatonin and vitamin B6 serving as the primary active ingredients. This study developed a novel analytical method for the simultaneous quantification of melatonin and vitamin B6 using 1 H-NMR spectroscopy. The characteristic signals of melatonin and vitamin B6 hydrochloride at δ 7.09 ppm and δ 8.12 ppm were selected for quantitative analysis, with maleic acid used as the internal standard. The method was validated for specificity, precision, and stability. The results demonstrate that the method exhibits high precision and complies with the guidelines established by the China Food and Drug Administration (CFDA). Furthermore, this method has been successfully applied to commercially available formulations. Compared to conventional methods, the 1 H-NMR technique offers a more efficient and simpler alternative, making it suitable for the simultaneous quantitative determination of melatonin and vitamin B6 hydrochloride. This approach ensures the quality, stability, and safety of commercial melatonin products.
研究领域:
分析化学
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药物分析
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核磁共振（NMR）谱学
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质量控制
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产品关联
DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
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2021
·Vol. 17
·期 4
·509-519
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IF 0.89
Hou Zhuoni,Liang Zongsuo,Li Yuanyuan,Su Feng,Chen Jipeng,Zhang Xiaodan,Yang Dongfeng
Background: Although chromatography and spectrometry-based methods have been used to analyse phenolic acids in Chinese traditional medicine Salvia miltiorrhiza Bunge (SMB), quantitative nuclear magnetic resonance (qNMR) has never previously been used to analyse fresh SMB root extracts.
Objective: To establish a fast and simple method of quantitating danshensu, lithospermic acid, rosmarinic acid, and salvianolic acid B content in fresh SMB root using 1H-NMR spectroscopy. Method: Fresh SMB root was extracted using a 70% methanol aqueous solution and quantitatively
analysed for danshensu, lithospermic acid, rosmarinic acid, and salvianolic acid B using 1H-NMR spectroscopy. Different internal standards were compared and the results were validated using highperformance liquid chromatography. Results: The established method was accurate
and precise with good recovery. The LOD and LOQ indicated the excellent sensitivity of the method. The robustness was testified by the modification of four different parameters, and the differences among each parameter were all less than 2%. Conclusion: qNMR offers a fast, reliable, and accurate
method of identifying and quantifying danshensu, lithospermic acid, rosmarinic acid, and salvianolic acid B in fresh SMB root extracts.
研究领域:
生药学
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分析化学
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中医药
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产品关联
DOI
高影响因子
CHEMICO-BIOLOGICAL INTERACTIONS
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2014
·
IF 2.982
Zhaoguang Lu,Junsong Wang,Minghui Li,Qingwang Liu,Dandan Wei,Minghua Yang,Lingyi Kong
A goldfish ( Carassius auratus ) model of Parkinson’s disease (PD) was constructed by a single dose of 1-methyl-4-phenyl-1,2,3,6-tetrahydropyridine (MPTP) according to previously reported methods. Global metabolite changes in brain of the MPTP induced goldfish model of PD were investigated. 1 H NMR-based metabolomics combined with various statistical methods such as orthogonal partial least squares discriminant analysis (OPLS-DA) and two-dimensional statistical total correlation spectroscopy (2D-STOCSY) found significant increase of leucine, isoleucine, valine, alanine, alanylalanine, creatinine, myo -inositol, 18:2 fatty acid, total fatty acids, arachic alcohol, taurine and significant decrease of N-acetylaspartate, (phospho)creatine, (phospho)choline, betaine, glutamine, 3-hexenedioate, acetamide, malonate, isocitrate, scyllo -inositol, phosphatidylcholines, cholesterols, n-3 fatty acids, polyunsaturated fatty acids (PUFAs) in brain of MPTP induced PD goldfish. These disturbed metabolite levels were involved in oxidative stress , energy failure, neuronal cell injury and death, consistent with those observed in clinical PD patients, and rodents and primates model of PD, indicating that the acute MPTP model of goldfish was an ideal and valuable model for PD research. In addition, several unusual metabolites in brain were significantly changed between MPTP induced PD and control goldfish, which might also play an important role in the pathogenesis of PD. This study also demonstrated the applicability and potential of 1 H NMR-based metabolomics approach for evaluation of animal models of disease induced by chemicals, such as MPTP-induced PD goldfish.
研究领域:
神经科学
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代谢组学
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毒理学
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产品关联
DOI
PubMed
高影响因子
Journal of Food Measurement and Characterization
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2021
·Vol. 15
·期 3
·2716-2726
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IF 2.431
Qian Junqing,Zhao Changyan,Zhu Hanxiao,Tong Jun,Zhao Xiaohua,Yang Haiyan,Guo Hui
Walnut oil is endowed with a variety of physiological functions due to abundant natural compounds, and the effect of unsaturated fatty acids is crucial. In order to accurately and conveniently detect the fatty acids components and content in walnut oil, a quantitative method was developed to detect fatty acids content based on the 1 H-NMR and 13 C-NMR techniques. In addition, HPLC combined with MS was used to conduct qualitative analysis. HPLC method with an evaporative light-scattering detector was for the quantitative analysis and the fatty acids content was compared with the content from NMR. The result showed that there was no significant difference between 1 H-NMR, 13 C-NMR and HPLC (P > 0.05) and indicated that the NMR has the potential to be applied as a routine method for the analysis of fatty acids content in walnut oil.
研究领域:
分析化学
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食品科学
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营养学
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产品关联
DOI
高影响因子
Journal of Ocean University of China
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2025
·Vol. 24
·期 6
·1827-1833
·
IF 1.2
Xin Wenyuan,Zhou Yunbing,Liu Daixi,Wang Cong,Sherwin K. B. Sy
Astaxanthin (AX) and vitamin E (VE) are widely consumed nutritional supplements in China, with its beneficial effects predominantly attributed to all-trans AX and VE. The aim of this study is to develop and validate a rapid and accurate method for quantifying the content of AX and VE in nutritional supplement products using highly sensitive 1 H NMR method. Coumarin was chosen as the internal standard. Specific signals from AX was optimal at H-7,7′ in the chemical shift range of δ 6.17–6.24 ppm, whereas the signals of VE at δ 2.59 ppm. To demonstrate the reliability of this analytical approach the proposed method underwent rigorous validation, specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, accuracy, precision, and recovery. The accuracy of the validation method was 3.10% for AX and 1.99% for VE. The results indicated that the method was precise and reliable. The method has been successfully applied to simultaneous quantification of AX and VE in nutritional supplements products.
研究领域:
分析化学
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营养科学
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药物分析
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产品关联
DOI
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
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2020
·
IF 5.065
Shengbo Zhu,Wei Li,Bingyang Lu,Weixing Chen,Wenzhi Zhang,Xiaoling Niu,Xinbing Chen,Zhongwei An
Two series of terminal epoxy compounds, PmOBC (m = 1, 2, 3, 4) and P1OBEn (n = 6, 8, 10, 12), were synthesized for investigating the effect of epoxidation on mesomorphic and thermal stabilities. Molecular polarization and configuration obtained by DFT calculations can provide theoretical perspective. In addition, thermal stability is evaluated by the combination of DSC , TGA , and 1 H NMR. Compared with the corresponding alkenyl compounds, epoxidation reduces the molecular dipole moment and increase the molecular steric effect , which is not conducive to the formation of LC phases, but the reduced intramolecular energy may be helpful to improve thermal stability. Therefore, these terminal epoxy LCs are very promising for application in display devices requiring extremely high-temperature environments.
研究领域:
材料科学
·
物理化学
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产品关联
DOI
高影响因子
MAGNETIC RESONANCE IN CHEMISTRY
·
2025
·
IF 1.4
Xiaoyan Zhang,Yaozuo Yuan,Yang Liu,Caiyu Zhang,Huiwen Deng,Songzi Jiang,Li Gan,Hui Fu,Xiaojuan Deng,Baoning Su,Jing Zhang,Fan Wu,Xingxiang Lv,Tong Liu,Yang Liu,Taijun Hang,Haiwei Shi
The research team established a quantitative 1 H NMR method to determine the relative ethoxy content ( EO %) in ethylcellulose using a CDCl 3 /TFA-d solvent mixture. High-field NMR spectroscopy enabled direct measurement without the use of internal or external calibrants by integrating the methyl proton signals (δ 1.15 ppm) and the methylene/methine proton signals (δ 2.5–5.5 ppm), and using their equivalent 1 H numbers and corresponding mass fractions for calculations. The EO % was calculated as: EO % = 315 r 486 − 614 r $$ \frac{315r}{486-614r} $$ × 100, where r = I A I A + I B $$ \frac{I_A}{I_A+{I}_B} $$ (I A methyl 1 Hs integral; Iᴃ methylene/methine 1 Hs integral). Round robin multi-laboratory validation testing showed that the qNMR results deviated by less than 3% from the certificate of analysis (COA) values (44%–51%). The COA values, derived using the pharmacopeial gas chromatography-flame ionization detection (GC-FID) method, may be affected by factors related to incomplete derivatization and the volatility and instability of the product (iodoethane) and the inert internal reference standard (n-octane). Therefore, the qNMR method with its operational simplicity, reduced chemical hazards, and robust performance presents an alternative for quality control of pharmaceutical-grade ethylcellulose.
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Hongtu Qiu,Kexin Qu,Hua Zhang,Jong-Bang Eun
In this study, 1 H nuclear magnetic resonance was used to track the evolution of oxidation products of different multi-element oleogels (DMEOs) during temperature-accelerated oxidative degradation. The nutritional properties of the DMEOs were also indirectly explored. Oleogels prepared using sitosterol/lecithin oleogelator showed higher nutritional properties than those prepared using carnauba wax or ethyl cellulose oleogelators. Only a small amount of primary oxidation product hydroxide, (Z,E)-conjugated dienic systems, and (E,E)-conjugated dienic systems were produced from all oleogels upon accelerated oxidation. Furthermore, no 1 H signal peaks of secondary oxidation products, such as aldehydes or ketones, were detected. However, very small amounts of primary alcohols (−CH 2 OH–), secondary alcohols (−CHOH–), and epoxides were identified. Moreover, resveratrol loading and surfactant addition effectively stabilized the internal structure and unsaturated fatty acid acyl content of the oleogels.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHEMICAL ENGINEERING SCIENCE
·
2012
·
IF 2.431
Yingjie Xu,Wu Qian,Qiongqiong Gao,Haoran Li
The 1 H NMR chemical shifts of alcohol+hydrocarbon systems over the whole concentration range at 298.15 K were measured. Based on the concept of local composition (LC), the concentration-dependent 1 H NMR chemical shift data of the OH and CH groups for 13 alcohol+hydrocarbon systems were correlated with only one energy parameter, respectively. Using the parameters obtained from the spectra alone, the isothermal and isobaric vapor–liquid equilibria (VLE) data of the above-mentioned alcohol+hydrocarbon systems were predicted with satisfactory results. By this way, the spectroscopic information can be used to predict VLE data of alcohol+hydrocarbon systems directly.
研究领域:
化学
·
物理化学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）