• Journal of the Korean Magnetic Resonance Society
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• v.22 no.3
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• pp.46-53
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• 2018

NMR-based metabolomics needs various knowledge to elucidate metabolic perturbation such as NMR experiments, NMR spectrum processing, raw data processing, metabolite identification, statistical analysis, and metabolic pathway analysis regarding technical aspects. Among them, some concepts of raw data processing and multivariate analysis are not easy to understand but are important to correctly interpret metabolic profile. This article introduces NMR spectrum processing, raw data processing, and multivariate analysis.

• Journal of the Korean Magnetic Resonance Society
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• v.24 no.1
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• pp.30-37
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• 2020

Quantitative nuclear magnetic resonance (qNMR) has been gaining attention as a purity assessment method. In particular, qNMR is recognized as the primary method to realize the Internal System of Units (SI) in organic analysis. The capability of quantitative analysis is recognized as the beginning of NMR development. NMR signals are proportional to the number of nuclei and qNMR has been used in various fields, such as metabolomics and food and pharmaceutical analysis. However, careful sample preparation and thorough optimization of measurement parameters are required to obtain accurate and reliable results. In this review, quantitative methods used in qNMR are discussed, and the important factors to be considered also introduced. The recent development of qNMR techniques including combination with chromatography and, multidimensional NMR are also presented.

• Analytical Science and Technology
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• v.20 no.5
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• pp.400-405
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• 2007

The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

• Journal of the Korean Society of Radiology
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• v.18 no.5
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• pp.499-508
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• 2024

As a result of analyzing the spectrum using a ¹H-NMR spectrometer and a ¹H-NMR spectrum prediction program for Visipaque contrast agent, the molecular structure positions in the 2.18 ppm and 2.17 ppm regions were found to be different from each other. The 2.25 ppm and 2.34 ppm regions did not appear in the spectrum analysis using the spectrometer, but did appear in the analysis using the prediction program. In addition, the 2.58 ppm region appeared in the spectrum analysis using the spectrometer, but did not appear in the analysis using the prediction program. The 4.42 ppm region did not appear in the spectrum analysis using the spectrometer, but did appear in the analysis using the prediction program. In addition, the 5.61 ppm region appeared in the spectrum analysis using the spectrometer, but did not appear in the analysis using the prediction program. Based on this, it is thought that if we analyze it using the prediction program as a reference, we will be able to identify the chemical structure more clearly.

• Journal of the Korean Magnetic Resonance Society
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• v.20 no.3
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• pp.87-94
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• 2016

Although NMR technique has been using in many areas of chemistry, its merit on quantitative analysis seems not to acknowledge greatly because of the many inferior intrinsic aspects, particularly its sensitivity. Recently, new NMR techniques, high-field NMR, and demands for cutting edge techniques of analysis, however, seem to change the role of NMR spectroscopy in this field. This review shows the application of NMR development in quantitative analysis and will discuss the basic idea, limitations, and pitfalls. Then it will show you several successful applications applied in quantitative analysis and you will see how useful and accurate method it is.

• The Korea Journal of Herbology
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• v.23 no.3
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• pp.27-32
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• 2008

Objectives : In this paper, we describe that $^1H-NMR$ spectroscopy may be superior to the conventional HPLC for the quantitative analysis of hesperidin from Citrus unshiu. Methods : $^1H-NMR$ spectra (400 MHz) were recorded in $DMSO-d_6$ using a Varian UNITY Inova AS 400 FT NMR spectrometer. One hundred milligram of powdered Citrus unshiu was weighed out and mixed with 1 ml of $DMSO-d_6$ with sonication for 30 min (room temperature). The extracts were filtrated through a 0.45 ${\mu}m$ PVDF filter and 0.5 ml of filtrated extract used for quantitative $^1H-NMR$ measurement (added 1 mg of dimethyl terephthalate as internal standard). The quantity of hesperidin was calculated by the ratio of the intensity of the compound to the known amount of internal standard. For HPLC analysis, the half gram of plant material was extracted with 60 ml of MeOH for 2 hours. The extracts were made 100 ml volume and analyzed by a Waters HPLC system using a YMC ODS column. The total flow rate was 1.0 ml/min with a sample volume 10 ${\mu}l$ and UV detection at 280nm. Results : The contents of hesperidin in Citrus unshiu was determined $5.33{\pm}0.06$% in the quantitative $^1H-NMR$ method and $5.15{\pm}0.12%$ in HPLC method. Using the quantitative $^1H-NMR$ the contents of hesperidin can be determined in much shorter time than the conventional HPLC measurements. Conclusions : From those results, the advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curve. Besides, it allows rapid and simple quantification for hesperidin with an analysis time for only 10 min without any pre-purification steps.

• Analytical Science and Technology
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• v.18 no.2
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• pp.168-172
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• 2005

A comparison study of XRF and $^{31}P$-NMR method for the analysis of phosphorous in lubricating oil has been described. Pure oil and water were used for the observation of matrices effect variation by different analytical methods. Quantitative analysis was carried out by XRF and $^{31}P$-NMR using real samples. Significant difference is observed from the slopes on the calibration curves by the XRF due to the matrices (water: 124.0, oil: 276.6). While the result obtained from XRF showed a large matrix effect, the slopes obtained from $^{31}P$-NMR results of two different matrices, however, are in good agreement ranged of ${\pm}9%$ (water: 4.9, oil: 5.3).

• Journal of the Korean Magnetic Resonance Society
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• v.20 no.1
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• pp.27-35
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• 2016

NMR spectrometer has been regarded as essential tool for structure elucidation in variable scientific field as like organic synthesis, natural product and macro protein research. Also NMR can be applied for defining dynamic behavior like ligand and receptor binding. One of advantage of research with NMR is that to be great confident to confirm structure and the measured sample could be recovered. Nevertheless NMR also has a weak points than other spectroscopic methods that require a lot of time for interpreting acquired spectrum and running time due to low sensitivity. For last two decade Bruker has developed hardware and software solution for overcome those weak points. In order to overcome low sensitivity Bruker introduced Cryo and Micro diameter probe head technology. And researcher can reduce the time for routine spectrum processing and interpretation works due to lots of introductions in software solutions for quantification, identification and statistics analysis. With four examples, this article describing those new hardware and software solutions in field of recent pharmaceutical research as follows. - New Horizons for NMR in the Biopharmaceutical Industry - The development and application of solid-state NMR spectroscopy (SSNMR) in pharmaceutical analysis - Assisted NMR Data Interpretation in Synthetic Chemistry - Complete Analysis of New Psychoactive Substances Using NMR.

• Journal of the Korean Magnetic Resonance Society
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• v.20 no.1
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• pp.7-12
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• 2016

PTMEG(Polytetramethylene ether glycol) is a polymer compound widely used as a wide range of applications in the textile industry. PTMEG substance carrying various 1,800~2,000 molecular weight are mainly used as the raw material of the spandex production. Molecular weight and degree of polymerization value for 4 different PTMEG samples under pilot plant scale synthetic process were determined by a new quantitative NMR method. In NMR experiments, p-toluenesulfonic acid(TSOH) was used for external standard material of PTMEG quantitative analysis. were measuring The concentration of the primary standard TSOH was measured by UV/Vis spectroscopy. By using NMR peak assignments and the integral values of designated proton NMR peaks, We were able to measure the % composition of the synthetic PTMEG polymers, concentrations, molecular weight and the degree of polymerization that show the synthetic process of each manufacturing pilot plant. By utilizing a newly developed quantitative NMR method were able to obtain the molecular weight of PTMEG samples within 0.08 error % range.

• Journal of the Korean Magnetic Resonance Society
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• v.22 no.2
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• pp.26-33
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• 2018

Xanthium sibiricum is used as a traditional folk medicine for the treatment of cancer, fever, headache, nasal sinusitis, and skin pruritus. This study aimed to identify components from Xanthium sibiricum extracts using an SPE-800MHz NMR-MS hyphenated system. The simultaneous acquisition of MS and NMR spectra from the same chromatographic peaks significantly increases the depth of information acquired for the compound and allows the elucidation of structures that would not be possible using MS or NMR data alone. LC -NMR analysis was conducted using a HPLC separation system coupled to 800 MHz spectrometer equipped with a cryoprobe, and a SPE unit was used to automatically trap chromatographic peaks using a HPLC pump. LC-MS analysis was conducted with a Q-TOF MS instrument using ESI ionization in the negative ion mode. Using the hyphenated analysis, several secondary metabolites were identified, such as 3',5'-O-dicaffeoylquinic acid, 1',5'-O-dicaffeoyl- quinic acid, and ethyl caffeate. These results demonstrate that the SPE-800MHz NMR-MS hyphenated system can be used to identify metabolites within natural products that have complex mixtures.