ISSN:
1618-2650
Source:
Springer Online Journal Archives 1860-2000
Topics:
Chemistry and Pharmacology
Notes:
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.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1007/BF00323664
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