A study of HPLC separation and spectrophotometric, polarographic and voltammetric detection of 4-substituted derivatives of N-nitroso-N-methylaniline

Jiří Barek, Pham Tuan Hai, Věra Pacáková, Karel Štulík, Ivana Švagrová, Jiří Zima

Research output: Contribution to journalArticle

3 Citations (Scopus)

Abstract

Optimised conditions have been found for the separation of N-nitroso-N-methylaniline derivatives substituted in the position 4 (4-R-NMA, where R =- H,- CH3, - OCH3, - Cl, - CN, - OH and - NO2), using reversed phase HPLC with a C18 chemically bonded stationary phase. Suitable mobile phases are mixtures of aqueous 0.01 mol l-1 KH2PO4 with methanol (4+6) or acetonitrile (7+3), or a mixture of water, methanol, acetonitrile and 80% H3PO4 (200+200+200+3). Four detection techniques have been investigated: Direct UV photometry, polarography on a hanging mercury drop electrode, anodic voltammetry on a glassy carbon fibre array electrode and indirect anodic voltammetric detection after photolytic denitrosation of the analytes. The UV photometry is the most universal and yields limits of detection around 10-6 mol l-1. Polarography exhibits the poorest sensitivity (with a limit of detection of ca. 10-5 mol l-1) but it can be used for selective detection of 4-NO2-NMA. Direct voltammetric detection is selective for the oxidizable derivatives and the limits of detection attained are lower than those obtained by UV photometry (for 4-OH-NMA) or comparable with (for 4-OCH3-NMA). When the analytes are photolytically denitrosated to yield oxidizable derivatives, the voltammetric detection of 4-H-NMA, 4-Cl-NMA, 4-CH3-NMA and 4-NO2-NMA has limits of detection one order of magnitude lower than those obtained UV photometrically.

Original languageEnglish
Pages (from-to)678-683
Number of pages6
JournalFresenius' Journal of Analytical Chemistry
Volume350
Issue number12
DOIs
Publication statusPublished - 1 Dec 1994
Externally publishedYes

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Photometry
Limit of Detection
Polarographic analysis
High Pressure Liquid Chromatography
Polarography
Derivatives
Methanol
Electrodes
Glassy carbon
Voltammetry
Mercury
Water
N-methyl-N-nitrosoaniline
acetonitrile

ASJC Scopus subject areas

  • Biochemistry

Cite this

A study of HPLC separation and spectrophotometric, polarographic and voltammetric detection of 4-substituted derivatives of N-nitroso-N-methylaniline. / Barek, Jiří; Hai, Pham Tuan; Pacáková, Věra; Štulík, Karel; Švagrová, Ivana; Zima, Jiří.

In: Fresenius' Journal of Analytical Chemistry, Vol. 350, No. 12, 01.12.1994, p. 678-683.

Research output: Contribution to journalArticle

Barek, Jiří ; Hai, Pham Tuan ; Pacáková, Věra ; Štulík, Karel ; Švagrová, Ivana ; Zima, Jiří. / A study of HPLC separation and spectrophotometric, polarographic and voltammetric detection of 4-substituted derivatives of N-nitroso-N-methylaniline. In: Fresenius' Journal of Analytical Chemistry. 1994 ; Vol. 350, No. 12. pp. 678-683.
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AU - Barek, Jiří

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AU - Štulík, Karel

AU - Švagrová, Ivana

AU - Zima, Jiří

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