- N-hydroxysuccinimidyl p-methoxybenzoate as suitable derivative reagent for isotopic dilution assay of biogenic amines in food
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We present a simple methodology for the simultaneous identification and determination of biogenic amines in food matrices, based on the use of a stable isotope-coded derivatization and liquid chromatography tandem mass spectrometry. The tagging reagent is N-hydroxysuccinimidyl ester of d0/d4-4-methoxybenzoic acid (d0/d4-4-MBA-OSu) which mainly functionalizes primary amines. The identification and structural characterization of tagged biogenic amines were exploited by matrix-assisted laser desorption/ionization-mass spectrometry (MS) and MS/MS. Multiple-reaction monitoring has been applied in the assay of biogenic amines in different foodstuffs, providing a method whose reliability is confirmed by the values of accuracy (12%) and by the calculated analytical parameters.
- Mazzotti, Fabio,Di Donna, Leonardo,Napoli, Anna,Aiello, Donatella,Siciliano, Carlo,Athanassopoulos, Constantinos M.,Sindona, Giovanni
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- A fast track for the accurate determination of methoxyl and ethoxyl groups in lignin
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A method based on headspace-isotope dilution (HS-ID) GC-MS for the quantitative analysis of methoxyl and ethoxyl groups in any kind of lignin has been developed. The method involves the application of an isotopically labeled internal standard (4-(methoxy-
- Sumerskii, Ivan,Zweckmair, Thomas,Hettegger, Hubert,Zinovyev, Grigory,Bacher, Markus,Rosenau, Thomas,Potthast, Antje
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p. 22974 - 22982
(2017/07/10)
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- N-hydroxysuccinimidyl p-methoxybenzoate as suitable derivative reagent for isotopic dilution assay of biogenic amines in food
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We present a simple methodology for the simultaneous identification and determination of biogenic amines in food matrices, based on the use of a stable isotope-coded derivatization and liquid chromatography tandem mass spectrometry. The tagging reagent is N-hydroxysuccinimidyl ester of d0/d4-4-methoxybenzoic acid (d0/d4-4-MBA-OSu) which mainly functionalizes primary amines. The identification and structural characterization of tagged biogenic amines were exploited by matrix-assisted laser desorption/ionization-mass spectrometry (MS) and MS/MS. Multiple-reaction monitoring has been applied in the assay of biogenic amines in different foodstuffs, providing a method whose reliability is confirmed by the values of accuracy (12%) and by the calculated analytical parameters.
- Mazzotti, Fabio,Di Donna, Leonardo,Napoli, Anna,Aiello, Donatella,Siciliano, Carlo,Athanassopoulos, Constantinos M.,Sindona, Giovanni
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p. 800 - 810
(2015/02/19)
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- Synthesis of 14C- and13C/2H-labeled SGLT inhibitors AVE2268 and AVE8887
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Isotopically labeled analogues of two structurally very similar SGLT inhibitors AVE2268 (1a) and AVE8887 (1b) have been synthesized by various routes. The radioactive labeled [14C]-AVE2268 was prepared in 5 steps including a Friedel-Crafts acylation as the key step for the 14C-label introduction. For [14C]-AVE8887 the same synthetic approach was not successful and therefore an alternative thiophene metalation/Weinreb amide sequence was developed. This pathway was also applied to obtain stable isotopically labeled analogs of both AVE2268 and AVE8887. Copyright r 2010 John Wiley & Sons, Ltd.
- Derdau, Volker,Fey, Thorsten,Atzrodt, Jens
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p. 381 - 383
(2011/04/24)
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- Synthesis of isotopically labelled SGLT inhibitors and their metabolites
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Isotopically labelled analogues of two structurally very similar SGLT inhibitors AVE2268 (1a) and AVE8887 (1b) have been synthesized by various routes. The radioactive labelled [14C]-AVE2268 was prepared in five steps including a Friedel-Crafts acylation as the key step for the 14C-label introduction. For [14C]-AVE8887 the same synthetic approach was not successful and therefore an alternative thiophene metallation/Weinreb amide sequence was developed. This pathway was also applied to obtain stable isotopically labelled analogues of both AVE2268 and AVE8887. Finally, the synthesis of two metabolites, sulfate 12 and glucuronide 13 were achieved by applying interesting protecting group and oxidation strategies.
- Derdau, Volker,Fey, Thorsten,Atzrodt, Jens
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experimental part
p. 1472 - 1482
(2010/04/02)
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- Rearrangements and Isomerism in the Molecular Ion of o-Methoxybenzoic Acid
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The molecular ion of o-methoxy-d3-benzoic acid can unddergo three different rearrangements and hydrogen/deruterium exchange between the functional groups.This can result in 14 isomers of the molecular ion before it decomposes giving fragments a
- Gillis, Richard G.,Porter, Quentin N.
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- N,N'-Heptamethylenebis(4-methoxybenzamide)
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4-(Q-O)-4'-R1 -N,N'-alkylenebis(benzamides), N,N'-alkylenebis(3,4-methylenedioxybenzamides) or N,N'-alkylenebis[4-(lower-alkoxy)benzamides], having endocrinological properties, where Q is lower-alkyl, lower-alkoxyalkyl, lower-alkenyl, halo-lower-alkyl, halo-lower-alkenyl, lower-cycloalkyl, phenyl and BN-(lower-alkyl) where BN is di-(lower-alkyl)amino or a saturated N-heteromonocyclic radical having from five to seven ring atoms and alkylene has at least five carbon atoms between its two connecting linkages and R1 is Q-O-, hydrogen, lower-alkoxy, lower-alkyl, halo, benzyloxy, hydroxy, di-(lower-alkyl)amino, nitro, amino or trihalomethyl are prepared preferably by reacting the appropriate diamine or N-(aminoalkyl)-benzamide with two or one molar equivalents, respectively, of the appropriate benzoyl halide.
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