期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1218, 期 42, 页码 7640-7647出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2011.06.027
关键词
Capillary electrochromatography; CEC-MS; Polymeric monolith; Sulfonamides; Meat sample
资金
- National Science Council of Taiwan [NSC 100-2632-M-033-001-MY3]
- Chung Yuan Christian University, Taiwan [CYCU-98-CR-CH]
In this work, a series of poly(divinylbenzene-alkyl methacrylate) monolithic stationary phases, which were prepared by single step in situ polymerization of divinylbenzene and various alkyl methacrylates (butyl-, octyl-, lauryl- or stearyl methacrylate), were developed as separation columns of nine common sulfonamide antibiotics for capillary electrochromatography (CEC) coupled to mass spectrometry (MS). Results indicated that the sulfonamide's retention became weak with increased carbon chain length of alkyl methacrylate monomer (for example, t(R) = 68 min and 21 min for butyl- and lauryl methacrylate, respectively). Among them, the poly(divinylbenzene-octyl methacrylate) (poly(DVB-OMA)) monolith was regarded as the optimal separation column as this provided better resolution within the shortest retention time. Moreover, the cross-sectional roughness of the monolithic column-end, that was used to couple to the ESI interface, strongly influenced the electrospray stability in the CEC-MS. Before the column was connected to the ESI-MS, a simple polishing was done to reduce the roughness of the column end that resulted to a great improvement in the signal stability. The relative standard deviations (RSDs) of the peak areas for the unpolished and polished ends of the poly(DVB-OMA) columns (n = 5) were in the range of 46.1-60.2% and 8.9-16.4%, respectively. Furthermore, optimization of the mobile phase composition and the gradient elution strategy successfully determined the sulfonamide antibiotics in meat samples with as low as 10 mu g/L level. (C) 2011 Elsevier B.V. All rights reserved.
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