A new traceability scheme for the development of international system-traceable persistent organic pollutant reference materials by quantitative nuclear magnetic resonance

Saito, Tetsuya; Ihara, Toshihide; Koike, Masayoshi; Kinugasa, Shinichi; Fujimine, Yoshinori; Nose, Kazuo; Hirai, Takayuki

doi:10.1007/s00769-008-0461-z

Cited by 73 publications

(47 citation statements)

References 14 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…4 Thus, it is crucial to select a target proton in the D-(+)-glucose for this study. 18 which is mainly related to the interaction between the solvent and the free-electron pair of the anomeric oxygen, 19 monitoring either α-C1 proton at 5.21 ppm or β-C1 proton at 4.64 ppm, but not both protons, was sufficient to quantitate D-(+)-glucose in D2O by qNMR.…”

Section: Optimization Of Dosy Acquisition Conditionsmentioning

confidence: 99%

“…The use of an appropriate IS makes qNMR analysis extremely attractive for purity determination. 4 In food analysis, some researchers have applied qNMR to the determination of interests in natural products, 5 foods and beverages, [6][7][8][9][10] because fewer tedious procedures are necessary prior to an assay. Sugimoto et al 8 have successfully measured quercetin in tartary buckwheat noodle by qNMR, and showed that hexamethyldisilane was effective as an IS in normalizing the proton at H-2′ in quercetin, though the use of this IS was limited due to its poor solubility in aqueous solution.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Quantitative Analysis of D-(+)-Glucose in Fruit Juices Using Diffusion Ordered-1H Nuclear Magnetic Resonance Spectroscopy

et al. 2014

View full text Add to dashboard Cite

show abstract

Section: Optimization Of Dosy Acquisition Conditionsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Quantitative Analysis of D-(+)-Glucose in Fruit Juices Using Diffusion Ordered-1H Nuclear Magnetic Resonance Spectroscopy

et al. 2014

View full text Add to dashboard Cite

show abstract

“…As a consequence for NMR quantification, it is not necessary to have a reference standard available which is of the same chemical structure as the sample. For many organic samples, a direct traceability to a small set of internationally accepted reference standards can be achieved [10,11].…”

Section: Introductionmentioning

confidence: 99%

Using high-performance quantitative NMR (HP-qNMR®) for certifying traceable and highly accurate purity values of organic reference materials with uncertainties <0.1 %

Weber¹,

Hellriegel²,

Rück³

et al. 2013

Accred Qual Assur

View full text Add to dashboard Cite

Quantitative nuclear magnetic resonance (qNMR) in combination with metrological weighing is optimised to demonstrate the power of the qNMR measurement method. It is shown that with 1 H-qNMR it is possible to certify the purity of organic reference materials (expressed as mass fraction) with relative expanded uncertainties of \0.1 % for a 95 % confidence interval (k = 2). Following well-defined selection criteria, a set of twelve different chemical compounds is evaluated and certified to serve as internal references for 1 H-qNMR measurements. A series of comparison measurements is made amongst a subset of the selected compounds. The purity of maleic acid is determined by six different 1 H-qNMR measurement series, and all results show full consistency. All the six mean values are covered within the range of ±0.05 %. In two more measurement series, four different nuclei are analysed within the same sample against one calibrator. Even with non-optimised signal intensity ratios and varying signal pattern, a high consistency was obtained. Therefore, the validity and robustness of 1 H-qNMR measurement results are demonstrated. 1 H-qNMR measurement results are directly traceable to a variety of internationally accepted primary reference materials, and therefore, traceability to SI units is obtained. All experiments are performed under ISO/IEC 17025 and ISO Guide 34 accreditation.

show abstract

“…[2][3][4][5][6][7] The qNMR method permits the absolute quantification of a target compound without the need for a standard of that compound. In addition, it is rapid and easy.…”

mentioning

confidence: 99%

“…NMR acquisition and processing were performed as previously described. [2][3][4][5][6][7] For each sample, 16 scans were recorded with a 90° pulse and a 60-s pulse delay, since highprecision qNMR spectra can be attained when the pulse angle is 90° and the pulse delay time is greater than the quintuple spin-lattice relaxation time ( Quantitative Determination of Stevioside and Rebaudioside A by qNMR Commercial standards of stevioside (STD-I through -V) and rebaudioside A (RBDA-I through -V) were dried at 105°C for 2 h, according to the preparation method of the standard described in the JECFA specifications, 1) and then 20 mg of each standard was accurately weighed and dissolved individually in 1.0 mL of the qNMR reference solution and subjected to 1 H-NMR measurement. The purities (%w/w) of stevioside and rebaudioside A in the standards were calculated from Eq.…”

mentioning

confidence: 99%

Absolute Quantitation of Stevioside and Rebaudioside A in Commercial Standards by Quantitative NMR

Tada¹,

Takahashi²,

Ishizuki³

et al. 2013

CHEMICAL & PHARMACEUTICAL BULLETIN

View full text Add to dashboard Cite

The extract produced from the leaves of Stevia rebaudiana Bertoni (Asteraceae) contains sweet steviol glycosides, mainly stevioside and rebaudioside A (Fig. 1), and has long been used as a sweetener in Japan. In 2008, the specifications for "steviol glycosides" were established by the Food and Agriculture Organization of the United Nations (FAO)/World Health Organization (WHO) Joint Expert Committee on Food Additives (JECFA), and "stevia extracts" were approved as generally recognized as safe (GRAS) by the U.S. Food and Drug Administration (FDA). Thereafter, the purified stevia extracts specified in JECFA and FDA became popular worldwide.According to the assay for steviol glycocides in the JECFA specifications, 1) the total content of nine types of steviol glycosides (Fig. 2) should not be less than 95%. In the assay method, rebaudioside A is quantified from the peak area on LC using the rebaudioside A standard, and each steviol glycoside except rebaudioside A is quantified from their respective peak areas and absorption coefficients using the stevioside standard as the quantification standard.Various commercial standard reagents of stevioside and rebaudioside A are available, although their purities are different and their exact purities are not indicated in the product literatures. Therefore, if the claimed values are employed in the quantitative analysis of a sample, the quantitated contents of the stevioside and rebaudioside A in the identical sample will be assigned different measured values according to the standard used for the quantification.Quantitative NMR (qNMR) using an internal standard with traceability to the International System of Units (SI units) has recently been used to determine the absolute purities of various chemical substances.2-7) The qNMR method permits the absolute quantification of a target compound without the need for a standard of that compound. In addition, it is rapid and easy. The compound is quantified from the ratios of the integral values of the proton signals of the internal standard and the target compound. In addition, various compounds can be quantified using the same internal standard.In this study, we utilized the qNMR method to determine the purity of stevioside and rebaudioside A in commercial standards. The knowledge of their absolute purities will increase the accuracy of other analytical methods that use standards, such as LC.

show abstract

A new traceability scheme for the development of international system-traceable persistent organic pollutant reference materials by quantitative nuclear magnetic resonance

Cited by 73 publications

References 14 publications

Quantitative Analysis of D-(+)-Glucose in Fruit Juices Using Diffusion Ordered-1H Nuclear Magnetic Resonance Spectroscopy

Quantitative Analysis of D-(+)-Glucose in Fruit Juices Using Diffusion Ordered-1H Nuclear Magnetic Resonance Spectroscopy

Using high-performance quantitative NMR (HP-qNMR®) for certifying traceable and highly accurate purity values of organic reference materials with uncertainties <0.1 %

Absolute Quantitation of Stevioside and Rebaudioside A in Commercial Standards by Quantitative NMR

Contact Info

Product

Resources

About