Facultad de Química, Departamento de Química Analítica, Universidad Nacional Autónoma de México, 04510 México, D.F., Mexico.
Talanta. 2012 Jan 15;88:553-60. doi: 10.1016/j.talanta.2011.11.032. Epub 2011 Nov 17.
A selective and simple analytical method for the trace level determination of carbofuran in complex environmental and biological samples was developed based on immunoaffinity extraction (IAE) followed by on-line preconcentration and HPLC/UV analysis of the purified extract. The immunosorbent for IAE was prepared by sol-gel encapsulation of monoclonal anti-carbofuran antibodies, and was fully characterized for capacity, repeatability, binding strength, binding kinetics and cross-reactivity. Method performance was evaluated with two different types of difficult samples: dam water and methanolic extracts of epithelial cervical-uterine tissue. Linear behavior and quantitative recoveries were obtained from the analysis of samples spiked with carbofuran at 0.2-4 ng/mL (dam water, 50 mL samples) and 10-40 ng/mL (biological tissue extract, 2 mL samples). RSD (n=7) and detection limits were, respectively, 10.1% (spike 0.40 ng/mL) and 0.13 ng/mL for dam water; 8.5% (spike 20 ng/mL) and 5 ng/mL for the biological tissue extract. The excellent sample purification achieved with the IAE column allows precise and accurate determination of carbofuran in complex matrices, even when using non-selective UV detection in the chromatographic analysis.
基于免疫亲和萃取(IAE),结合在线预浓缩和 HPLC/UV 分析,开发了一种用于痕量水平测定复杂环境和生物样品中克百威的简单选择性分析方法。IAE 的免疫吸附剂是通过单克隆抗克百威抗体的溶胶-凝胶包封制备的,并对其容量、重复性、结合强度、结合动力学和交叉反应性进行了全面表征。使用两种不同类型的困难样品评估了方法性能:大坝水和宫颈-子宫内膜组织的甲醇提取物。通过在 0.2-4 ng/mL(大坝水,50 mL 样品)和 10-40 ng/mL(生物组织提取物,2 mL 样品)浓度下添加克百威分析样品,得到线性行为和定量回收率。对于大坝水,RSD(n=7)和检测限分别为 10.1%(添加 0.40 ng/mL 克百威)和 0.13 ng/mL;对于生物组织提取物,RSD(n=7)和检测限分别为 8.5%(添加 20 ng/mL 克百威)和 5 ng/mL。IAE 柱实现的优异样品净化允许在复杂基质中精确和准确地测定克百威,即使在色谱分析中使用非选择性 UV 检测也是如此。