ChemInform Abstract: N‐Nitrosamines in Chemical Production

Mejstřík, Viktor; Drzkova, L.; Ságner, Z.; Krampera, F.; Matrka, M.

doi:10.1002/chin.198747390

Cited by 4 publications

(5 citation statements)

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“…The classic reagent for the indirect determination of alkylating agents 4-(4-nitrobenzyl)pyridine (NBP) is still frequently used. A comprehensive review was published in 1984 1 (a translation from the Czech original is available from the authors), and some more recent developments are cited in a paper from this laboratory. 2 Alkylation of NBP gives a colourless pyridinium salt, which is then converted to a coloured tetrahydropyridine by addition of a base.…”

Section: Introductionmentioning

confidence: 99%

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Determination of polar alkylating agents as thiocyanate/isothiocyanate derivatives by reaction headspace gas chromatography

Lee

Guivarch

Dau

et al. 2003

Analyst

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We report a new method for the determination of the methyl, ethyl and isopropyl esters of methanesulfonic acid, and of dimethyl sulfate. Derivatisation with aqueous sodium thiocyanate gives a mixture of the corresponding alkylthiocyanates and alkylisothiocyanates which, unlike the underivatised analytes, are readily analysed by GC. On-column isomerisation is negligible. These lower alkyl derivatives are sufficiently volatile for static reaction headspace analysis, and detection limits obtained by electron impact MS are below 0.05 µg ml 21 with respect to the injection solution. The method was used to demonstrate that levels of methanesulfonic acid esters in a drug substance (a mesylate salt that had been processed using methanol and ethanol) are below 1 µg g 21 .

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Section: Introductionmentioning

confidence: 99%

“…A satisfactory but elaborate solution is to isolate the pyridinium adduct before addition of base. TLC methods have been described, 1 and we have successfully used HPLC with post-column reaction detection (unpublished method).…”

Section: Introductionmentioning

confidence: 99%

Determination of polar alkylating agents as thiocyanate/isothiocyanate derivatives by reaction headspace gas chromatography

Lee

Guivarch

Dau

et al. 2003

Analyst

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“…3). 8,9 Alkylation of this reagent yields a colourless pyridinium ion, which on addition of a strong base is converted into the violet tetra-hydropyridine. Blank values, about 0.5-0.8 ppm, are high but acceptable for the present purposes, since the actual concentrations in production batches (determined by LC-MS) are invariably less than 0.1 ppm.…”

Section: Introductionmentioning

confidence: 99%

Determination of N,N-dimethylaminoethyl chloride and the dimethylaziridinium ion at sub-ppm levels in diltiazem hydrochloride by LC-MS with electrospray ionisation

Lee

Hubert

Dau

et al. 2000

Analyst

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An LC-MS method is described for the determination of the synthetic reagent N,N-dimethylaminoethyl chloride (DMC) in the drug substance diltiazem hydrochloride, for which the permissible limit is not more than 1 ppm (microgram g-1). The N,N-dimethylaziridinium ion (DMA), the reactive intermediate formed by cyclisation of DMC, is also detected. A column switching arrangement is used: diltiazem hydrochloride is trapped on a reversed-phase HPLC column, and the polar analytes are separated by ion exchange chromatography. Ionisation is effected by positive-ion electrospray, and the quadrupole filter mass spectrometer is operated in the selected ion recording mode. The detection limit (peak height-to-baseline noise ratio = 3) for DMC varies from day to day in the range < 0.05 to 0.1 ppm. The response for DMC is linear (r > 0.999) over the concentration range 0.2-10 ppm, and the repeatability is better than 7% (relative standard deviation) at 1.0 ppm. Concentrations of DMC in diltiazem hydrochloride from the manufacturing facility under study ranged from undetectable to about 0.07 ppm. An indirect TLC method has been published for the determination of DMC in mepyramine maleate, but it lacks the necessary sensitivity and specificity. The LC-MS method presented is direct, straightforward and suitable for routine use.

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“…Therefore, sensitive analytical methods are needed for the determination of trace amounts of these substances. Several analytical methods for the determination of triazine derivatives have been reported including UV-visible spectrophotometry [5,6] and polarography [7][8][9][10] but the use of these techniques is limited to a concentration level between 10\-10\ mol/l. Differential pulse stripping voltammetry has been widely applied for trace determinations of various categories of organic compounds including derivatives of pyridine, pyrimidine and purine compounds [11][12][13][14][15].…”

Section: Introductionmentioning

confidence: 99%

Adsorptive stripping voltammetric analysis of 2,4,6-tri(2'pyridyl)-1,3,5-triazine at a mercury electrode

Kamal

Zuhri

Nasser

1996

Analytical and Bioanalytical Chemistry

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The redox behaviour of adsorbed species of 2,4,6-tri(2'-pyridyl)-1,3-5-triazine (TPTZ) at the surface of a mercury electrode was examined using cycling voltammetry. Based on the adsorption and accumulation of TPTZ at the charged mercury surface cathodic adsorptive stripping voltammetry (CSV) is applied for the trace determination of TPTZ using a differential pulse (DP) technique. Experimental and operational parameters for the quantitative analysis of TPTZ are optimized and the detection limit was found to be 3x10(-9) mol/l. The effect of some interferences, e.g. organic compounds, cations and anions, are investigated.

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ChemInform Abstract: N‐Nitrosamines in Chemical Production

Abstract: 390ChemInform Abstract (50 refs.).

Cited by 4 publications

References 0 publications

Determination of polar alkylating agents as thiocyanate/isothiocyanate derivatives by reaction headspace gas chromatography

Determination of polar alkylating agents as thiocyanate/isothiocyanate derivatives by reaction headspace gas chromatography

Determination of N,N-dimethylaminoethyl chloride and the dimethylaziridinium ion at sub-ppm levels in diltiazem hydrochloride by LC-MS with electrospray ionisation

Adsorptive stripping voltammetric analysis of 2,4,6-tri(2'pyridyl)-1,3,5-triazine at a mercury electrode

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