Study of Sample Preparation Method Using Internal Standard Solution to Accurate Quantitative Analysis with &lt;sup&gt;1&lt;/sup&gt;H NMR Spectroscopy

Yamazaki, Taichi; Ohtsuki, Takashi; Miura, Toru; Suematsu, Takako; Horinouchi, Takaaki; Murakami, Masayo; Saito, Tetsuya; Ihara, Toshihide; Tada, Akio; Tahara, Maiko; Goda, Yukihiro; Akiyama, Hiroshi; Nakao, Shinji; Yamada, Yuko; Koike, Ryo; Sugimoto, Naotoshi

doi:10.2116/bunsekikagaku.63.323

Cited by 6 publications

(2 citation statements)

References 1 publication

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The calibrator concentrations for 25(OH)D 3 , 25(OH)D 2 , 3‐ epi ‐25(OH)D 3 , and 24,25(OH) 2 D 3 were as follows: 0.873, 0.0920, 0.0940, and 0.0960 ng/mL for calibrator level 1; 8.80, 0.924, 0.938, and 0.962 ng/mL for calibrator level 2; 44.0, 4.62, 4.69, and 4.81 ng/mL for calibrator level 3; and 88.0, 9.23, 9.37, and 9.61 ng/mL for calibrator level 4. These concentrations were determined by quantitative NMR measurements . Human Serum Standard Reference Material (SRM972a) was obtained from the National Institute of Standards and Technology (NIST, Gaithersburg, MD, USA).…”

Section: Methodsmentioning

confidence: 99%

A novel caged Cookson‐type reagent toward a practical vitamin D derivatization method for mass spectrometric analyses

Shimada

Sato

Takiwaki

et al. 2020

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

Rationale 25‐Hydroxylated vitamin D is the best marker for vitamin D (VD). Due to its low ionization efficiency, a Cookson‐type reagent, 1,2,4‐triazoline‐3,5‐dione (TAD), is used to improve the detection/quantification of VD metabolites by liquid chromatography/tandem mass spectrometry (LC/MS/MS). However, the high reactivity of TAD makes its solution stability low and inconvenient for practical use. We here describe the development of a novel caged Cookson‐type reagent, and we assess its performances in the quantitative and differential detection of four VD metabolites in serum using LC/MS/MS. Methods Caged 4‐(4′‐dimethylaminophenyl)‐1,2,4‐triazoline‐3,5‐dione (DAPTAD) analogues were prepared from 4‐(4′‐dimethylaminophenyl)‐1,2,4‐triazolidine‐3,5‐dione. Their stability and reactivity were examined. The optimized caged DAPTAD (14‐(4‐(dimethylamino)phenyl)‐9‐phenyl‐9,10‐dihydro‐9,10‐[1,2]epitriazoloanthracene‐13,15‐dione, DAP‐PA) was used for LC/MS/MS analyses of VD metabolites. Results The solution stability of DAP‐PA in ethyl acetate dramatically improved compared with that of the non‐caged one. We measured the thermal retro‐Diels‐Alder reaction enabling the release of DAPTAD and found that the derivatization reaction was temperature‐dependent. We also determined the detection limit and the lower limit of quantifications for four VD metabolites with DAPTAD derivatization. Conclusions DAP‐PA was stable enough for mid‐ to long‐term storage in solution. This advantage shall contribute to the detection and quantification of VD in clinical laboratories, and as such to the broader use of clinical mass spectrometry.

show abstract

Section: Methodsmentioning

confidence: 99%

A novel caged Cookson‐type reagent toward a practical vitamin D derivatization method for mass spectrometric analyses

Shimada

Sato

Takiwaki

et al. 2020

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

show abstract

“…On the other hand, in recent years, 1 H qNMR methodology have begun to be investigated, and multiple studies have demonstrated that accurate quantification with metrological traceability can be achieved via 1 H qNMR under optimized conditions. [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16] Additionally, 1 H qNMR has already been introduced into some compendial guidelines and official standards in such as United States Pharmacopeia (USP), Japanese Pharmacopeia (JP), and Japan's Specifications and Standards for Food Additive as a quantitation method for determining accurate purities or contents of analytical standards. As one outcome of collaborative studies, 1 H qNMR was adopted in the Japanese Industrial Standard (JIS) as JIS K 0138 (General rules for quantitative nuclear magnetic resonance spectroscopy) in January 2018.…”

Section: Introductionmentioning

confidence: 99%

Collaborative Study to Validate Purity Determination by <sup>1</sup>H Quantitative NMR Spectroscopy by Using Internal Calibration Methodology

Miura

Sugimoto²,

Bhavaraju

et al. 2020

Chem. Pharm. Bull.

Self Cite

View full text Add to dashboard Cite

NMR spectroscopy has recently been utilized to determine the absolute amounts of organic molecules with metrological traceability since signal intensity is directly proportional to the number of each nucleus in a molecule. The NMR methodology that uses hydrogen nucleus ( 1 H) to quantify chemicals is called quantitative 1 H-NMR ( 1 H qNMR). The quantitative method using 1 H qNMR for determining the purity or content of chemicals has been adopted into some compendial guidelines and official standards. However, there are still few reports in the literature regarding validation of 1 H qNMR methodology. Here, we coordinated an international collaborative study to validate a 1 H qNMR based on the use of an internal calibration methodology. Thirteen laboratories participated in this study, and the purities of three samples were individually measured using 1 H qNMR method. The three samples were all certified via conventional primary methods of measurement, such as butyl p-hydroxybenzoate Japanese Pharmacopeia (JP) reference standard certified by mass balance; benzoic acid certified reference material (CRM) certified by coulometric titration; fludioxonil CRM certified by a combination of freezing point depression method and 1 H qNMR. For each sample, 1 H qNMR experiments were optimized before quantitative analysis. The results showed that the measured values of each sample were equivalent to the corresponding reference labeled value. Furthermore, assessment of these 1 H qNMR data using the normalized error, E n -value, concluded that statistically 1 H qNMR has the competence to obtain the same quantification performance and accuracy as the conventional primary methods of measurement.

show abstract

Formic acid hydrolysis/liquid chromatography isotope dilution mass spectrometry: An accurate method for large DNA quantification

Shibayama

Fujii

Inagaki

et al. 2016

Journal of Chromatography A

View full text Add to dashboard Cite

Study of Sample Preparation Method Using Internal Standard Solution to Accurate Quantitative Analysis with <sup>1</sup>H NMR Spectroscopy

Cited by 6 publications

References 1 publication

A novel caged Cookson‐type reagent toward a practical vitamin D derivatization method for mass spectrometric analyses

A novel caged Cookson‐type reagent toward a practical vitamin D derivatization method for mass spectrometric analyses

Collaborative Study to Validate Purity Determination by <sup>1</sup>H Quantitative NMR Spectroscopy by Using Internal Calibration Methodology

Formic acid hydrolysis/liquid chromatography isotope dilution mass spectrometry: An accurate method for large DNA quantification

Contact Info

Product

Resources

About