Quantitative <sup>1</sup>H NMR spectroscopy analysis of the poly(3-hydroxyalkanoate) extracted from Rhizobium meliloti cells

Jan, S; Roblot, C.; Tavernier, Patricia; Courtois, J.; Courtois, B.; Portais, JC; Barbotin, Jean‐Noël; Séguin, J.P.

doi:10.1051/jcp/1995921793

Cited by 6 publications

(7 citation statements)

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“…[25][26][27][28][29][30][31] Proton QNMR has been applied to determine "octane number" in gasoline, 32,33 active ingredients in pharmaceutical formulations, 34,35 analysis of organic osmolytes and their metabolites in crude plant tissue extracts, 36 determination of intracellular pH, 37 and in polymer chemistry to determine acrylic unsaturation in ultraviolet light-curable resins. 38 Quantitative 1 H NMR has been used to characterize colon tumors, 39 microbial extracts, 40 polyethylene, 41 poly(ethylene glycol)s, 42 starches, 43 peroxidation of lipoproteins, 44 characterization of block copolymers, 45 and quantitation of brain water and cerebral metabolites. 46 Recently, a method for quantitative determination of compounds in continuous-flow LC NMR has been reported.…”

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confidence: 99%

Method Performance and Validation for Quantitative Analysis by ¹H and ³¹P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

Maniara¹,

Rajamoorthi²,

Rajan³

et al. 1998

Anal. Chem.

188

129

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Nuclear magnetic resonance (NMR) can be used to provide an independent and intrinsically reliable determination of chemical purity. Unlike chromatography, it is possible to employ a universal reference standard as an internal standard for the majority of chemical products assayed by quantitative NMR (QNMR). This is possible because the NMR response can be made the same for all chemical components, including the internal standard, by optimizing certain instrumental parameters. Experiments were performed to validate the quantitative NMR method described in this paper for the analysis of organic chemicals. Experimental precision, accuracy, specificity, linearity, limits of detection and quantitation, and ruggedness were systematically addressed, and system suitability criteria were established. The level of the major chemical ingredient can be determined with accuracy and precision significantly better than 1%, and impurities may be quantified at the 0.1% level or below. Thus, QNMR rivals chromatography in sensitivity, speed, precision, and accuracy, while avoiding the need for a reference standard for each analyte. Examples are given of (1)H and (31)P NMR used for quantitative analysis of agricultural chemicals, and a method for characterization of analytical standards is presented.

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confidence: 99%

Method Performance and Validation for Quantitative Analysis by ¹H and ³¹P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

Maniara¹,

Rajamoorthi²,

Rajan³

et al. 1998

Anal. Chem.

188

129

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“…Exopolysaccharides (EPS) are commercially useful for producing gels and modifying the rheological properties of aqueous systems, and they have potential in replacing plant and algae EPS traditionally used in food, pharmaceutical, textile, and oil industries (25). Under specific conditions, rhizobia also synthesize poly-␤-hydroxybutyrate (PHB) (12,21,30,35), an intracellular carbon and energy storage polymer with potential industrial applications due to its thermoplastic and biodegradable properties (5).…”

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confidence: 99%

Exopolysaccharide and Poly-(beta)-Hydroxybutyrate Coproduction in Two Rhizobium meliloti Strains

Tavernier¹,

Portais²,

Nava³

et al. 1997

Appl Environ Microbiol

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The effects of different nitrogen and carbon sources on cell growth, pH, and exopolysaccharide (EPS) and poly-␤-hydroxybutyrate (PHB) production by two strains of Rhizobium meliloti (M5N1 and Su47) are reported. Differences in the behavior of glucose-and fructose-grown cells were shown, in particular with the M5N1 strain. Growth in a glucose-containing medium was accompanied by acidification of the culture medium, which leads to cell death. On fructose, acidification was detected only in the medium with a mineral nitrogen supply. A lag phase in EPS production was observed with cells grown with glucose, probably related to an initial extracellular conversion of the carbohydrate into an acid. No lag phase was observed in EPS production from fructose or in PHB synthesis whatever the carbon source. A decrease in PHB content was noticed for both strains under conditions where acidification of media occurred. The extent of production, emphasized by the use of a coproduction index, indicates that the M5N1 strain is a more promising organism than is the Su47 strain for polymer production. Such a strain, put in rich medium (containing yeast extract) supplemented with fructose, accumulated PHB up to 85% of dry cell weight and excreted about 1.5 g of EPS per liter in the medium. Regulation of the coproduction of EPS and PHB by these cells is suggested.

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“…The method precision and accuracy are on the order of 0.5 and 1.0%, respectively, which rivals results from modern chromatographic techniques. The many reports on quantitative NMR spectroscopy appearing in the literature over the years, some of which are referenced herein, − support the applicability of NMR spectroscopy for quantitative chemical analysis. Of special note are the United States Pharmacopoeia and the British Pharmacopoeia, where the general quantitative NMR methodology is compendial.…”

Section: Discussionmentioning

confidence: 71%

“…Although more expensive and less sensitive than typical chromatographic techniques, such as gas chromatography/mass spectometry, NMR spectroscopy is less involved, because it does not require extensive sample preparation and generates results that are easily interpreted. NMR spectroscopy is an accurate quantitative technique when conducted under appropriate conditions; this potential was demonstrated more than 20 years ago. − Past reports have typically exploited proton − and 13 C NMR spectroscopy; − however, examples using 31 P − and other nuclei − are found in the literature. In addition, the accuracy and precision of NMR signal intensity measurements have recently been reviewed .…”

mentioning

confidence: 99%

“…NMR spectroscopy is an accurate quantitative technique when conducted under appropriate conditions; this potential was demonstrated more than 20 years ago. [1][2][3] Past reports have typically exploited proton [4][5][6][7] and 13 C NMR spectroscopy; [8][9][10][11] however, examples using 31 P [12][13][14][15] and other nuclei [16][17][18][19][20][21][22] are found in the literature. In addition, the accuracy and precision of NMR signal intensity measurements have recently been reviewed.…”

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Quantitative NMR Spectroscopy Using Coaxial Inserts Containing a Reference Standard: Purity Determinations for Military Nerve Agents

Henderson

2001

Anal. Chem.

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A novel 31P NMR method for the determination of purity for the military nerve agents sarin, soman, and VX has been developed. In contrast to more conventional quantitative NMR methods, stem coaxial inserts are placed into the sample tube to introduce reference material into the analysis without mixing or reaction with the analyte. All sample preparation is eliminated, and the analysis is completed expeditiously in less than 25 min. The method is highly specific and rugged with respect to operator-induced variability, experimental parameters, and all influences from nuclear magnetic relaxation. Nerve agent purity can be determined with a precision and accuracy typically better than 1%, and impurities can be detected at concentrations as low as 25 microg/mL. The limit of quantitation has been estimated at 85 microg/mL. In terms of precision, accuracy and execution time, the method rivals typical chromatographic methods.

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Quantitative ¹H NMR spectroscopy analysis of the poly(3-hydroxyalkanoate) extracted from Rhizobium meliloti cells

Cited by 6 publications

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Method Performance and Validation for Quantitative Analysis by ¹H and ³¹P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

Method Performance and Validation for Quantitative Analysis by ¹H and ³¹P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

Exopolysaccharide and Poly-(beta)-Hydroxybutyrate Coproduction in Two Rhizobium meliloti Strains

Quantitative NMR Spectroscopy Using Coaxial Inserts Containing a Reference Standard: Purity Determinations for Military Nerve Agents

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Quantitative 1H NMR spectroscopy analysis of the poly(3-hydroxyalkanoate) extracted from Rhizobium meliloti cells

Cited by 6 publications

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Method Performance and Validation for Quantitative Analysis by 1H and 31P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

Method Performance and Validation for Quantitative Analysis by 1H and 31P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

Exopolysaccharide and Poly-(beta)-Hydroxybutyrate Coproduction in Two Rhizobium meliloti Strains

Quantitative NMR Spectroscopy Using Coaxial Inserts Containing a Reference Standard: Purity Determinations for Military Nerve Agents

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Quantitative ¹H NMR spectroscopy analysis of the poly(3-hydroxyalkanoate) extracted from Rhizobium meliloti cells

Method Performance and Validation for Quantitative Analysis by ¹H and ³¹P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

Method Performance and Validation for Quantitative Analysis by ¹H and ³¹P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals