Liu Wei, Zhang Zhujun, Liu Zuoqin
Key Laboratory of Analytical Chemistry for Life Science of Shaanxi Province, School of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, PR China.
Anal Chim Acta. 2007 Jun 5;592(2):187-92. doi: 10.1016/j.aca.2007.04.027. Epub 2007 Apr 21.
In this paper, a chemiluminescence (CL) micro-flow system combined with on-line solid phase extraction (SPE) is presented for determination of beta-lactam antibiotics (penicillin, cefradine, cefadroxil, cefalexin) in milk. It is based on the enhancement effect of beta-lactam antibiotics on the luminol-K3Fe(CN)6 CL system. The micro-flow system was fabricated from two polymethyl methacrylate (PMMA) plates (50 mm x 40 mm x 5 mm) with the microchannels of 200 microm wide and 150 microm deep. C18-modified silica gel was packed into the microchannel (length: 10 mm; width: 1 mm; depth: 500 microm) to serve as SPE device. Extraction and preconcentration of the analytes were carried out using on-line SPE micro-flow system and the selectivity of CL detection was improved. The detection limits were 0.5 microg mL(-1) of penicillin, 0.04 microg mL(-1) of cefradine, 0.08 microg mL(-1) of cefadroxil and 0.1 microg mL(-1) of cefalexin. The proposed method was also applied to analyze the beta-lactam antibiotics in milk. Experimental results were in good agreement with those obtained by high performance liquid chromatography (HPLC) method with UV detection.
本文介绍了一种结合在线固相萃取(SPE)的化学发光(CL)微流控系统,用于测定牛奶中的β-内酰胺类抗生素(青霉素、头孢拉定、头孢羟氨苄、头孢氨苄)。该方法基于β-内酰胺类抗生素对鲁米诺-K3Fe(CN)6化学发光体系的增强作用。微流控系统由两块聚甲基丙烯酸甲酯(PMMA)板(50 mm×40 mm×5 mm)制成,微通道宽200微米,深150微米。将C18改性硅胶填充到微通道(长度:10 mm;宽度:1 mm;深度:500微米)中作为固相萃取装置。使用在线固相萃取微流控系统对分析物进行萃取和预浓缩,提高了化学发光检测的选择性。青霉素的检测限为0.5微克/毫升,头孢拉定的检测限为0.04微克/毫升,头孢羟氨苄的检测限为0.08微克/毫升,头孢氨苄的检测限为0.1微克/毫升。该方法还应用于牛奶中β-内酰胺类抗生素的分析。实验结果与采用紫外检测的高效液相色谱(HPLC)法得到的结果吻合良好。