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 language | English |
|---|---|
| Pages (from-to) | 678-683 |
| Number of pages | 6 |
| Journal | Fresenius' Journal of Analytical Chemistry |
| Volume | 350 |
| Issue number | 12 |
| DOIs | |
| Publication status | Published - 1 Dec 1994 |
| Externally published | Yes |
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- 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 journal › Article
}
TY - JOUR
T1 - A study of HPLC separation and spectrophotometric, polarographic and voltammetric detection of 4-substituted derivatives of N-nitroso-N-methylaniline
AU - Barek, Jiří
AU - Hai, Pham Tuan
AU - Pacáková, Věra
AU - Štulík, Karel
AU - Švagrová, Ivana
AU - Zima, Jiří
PY - 1994/12/1
Y1 - 1994/12/1
N2 - 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.
AB - 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.
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U2 - 10.1007/BF00323664
DO - 10.1007/BF00323664
M3 - Article
AN - SCOPUS:0000315543
VL - 350
SP - 678
EP - 683
JO - Fresenius Journal of Analytical Chemistry
JF - Fresenius Journal of Analytical Chemistry
SN - 0937-0633
IS - 12
ER -