期刊
JOURNAL OF SEPARATION SCIENCE
卷 37, 期 20, 页码 3000-3006出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201400360
关键词
Capillary electrophoresis; Contactless conductivity detection; Melamine; Milk; Sample clean-up
资金
- National Science Foundation of China (NSFC) [J1103305]
- Fund for Innovative Chemical Experiment and Research of Sun Yat-sen University
Based on an efficient sample clean-up and field-amplified sample injection online preconcentration technique in capillary electrophoresis with contactless conductivity detection, a new analytical method for the sensitive determination of melamine in milk samples was established. In order to remove the complex matrix interference, which resulted in a serious problem during field-amplified sample injection, liquid-liquid extraction was utilized. As a result, liquid-liquid extraction provides excellent sample clean-up efficiency when ethyl acetate was used as organic extraction by adjusting the pH of the sample solution to 9.5. Both inorganic salts and biological macromolecules are effectively removed by liquid-liquid extraction. The sample clean-up procedure, capillary electrophoresis separation parameters and field-amplified sample injection conditions are discussed in detail. The capillary electrophoresis separation was achieved within 5 min under the following conditions: an uncoated fused-silica capillary, 12 mM HAc + 10 mM NaAc (pH = 4.6) as running buffer, separation voltage of + 13 kV, electrokinetic injection of + 12 kV x 10 s. Preliminary validation of the method performance with spiked melamine provided recoveries >90%, with limits of detection and quantification of 0.015 and 0.050 mg/kg, respectively. The relative standard deviations of intra-and inter-day were below 6%. This newly developed method is sensitive and cost effective, therefore, suitable for screening of melamine contamination in milk products.
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