Optimisation of the liquid chromatographic separation of pirimicarb and its metabolites V–VII: application to a soil sample used as a candidate reference material

• Published in: Analytica chimica acta Vol. 286; no. 3; pp. 457 - 468
• Main Authors: Honing, M., Barceló, D., Ghijsen, R.T., Brinkman, U.A.Th
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Amsterdam Elsevier B.V 28.02.1994; Elsevier
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Exact sciences and technology; Liquid chromatography; Other chromatographic methods; Pirimicarb; Soils; Soils; Pirimicarb; Liquid chromatography; Chemical analysis; Column packing; Metabolite; Organic carbamate; Modified material; Stationary phase
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/0003-2670(94)85091-7

The simultaneous separation of the N-dimethylcarbamate pirimicarb and its metabolites V–VII was carried out by liquid chromatography (LC) using diode array detection (DAD). Two columns, a 250 × 4.6 mm i.d. column packed with 5-μm particles with a cyanopropyl modified silica stationary phase and a 150 × 4.6 mm i.d. column packed with 3-μm particles with a base deactivated C 8 modified silica stationary phase, were compared. The addition of a buffer in the eluent, for both columns, was needed to improve the peak shape of metabolite V and the resolution of the metabolites V–VII and consequently the pH dependence of the retention time was tested. Additionally chromatograms of two soil samples of different origin, spiked at a concentration level of 1 μg g −1 for pirimicarb, analysed by LC-DAD, gas chromatography (GC) with nitrogen phosphorus detection and GC-mass spectrometry are shown. Detection limits and reproducibility data of primicarb in a candidate reference sample using LC-DAD and a cyanopropyl column are reported.