He Limin, Su Yijuan, Shen Xiangguang, Zheng Yaqiu, Guo Hongbin, Zeng Zhenling
Department of Pharmacology and Toxicology, College of Veterinary Medicine, South China Agriculture University, Guangzhou, China.
J Sep Sci. 2009 Oct;32(19):3310-8. doi: 10.1002/jssc.200900407.
A method for molecularly imprinted SPE of the melamine from environmental water samples was investigated. Cyromazine-imprinted polymers were synthesized in water-methanol systems for the selective extraction of melamine from aqueous samples, followed by HPLC analysis. Molecular recognition properties and binding capability to melamine were evaluated by adsorption test and Scatchard analysis, which showed the dissociation constant (KD) and the maximum binding quantity (Qmax) were 0.032 micromol/L and 4.77 micromol/g for high affinity binding site, and 0.26 micromol/L and 19.10 micromol/g for lower affinity binding site, respectively. Under the optimum extraction protocol, the method can be successfully applied to selectively extract and enrich melamine in environmental water. The linearity was ranged from 0.500 to 100.0 ng/mL (r > 0.999) in tap water, lake water, and seawater analysis. When 50 mL of the water samples loaded, the LODs of the method were ca. 0.1 ng/mL, and the LOQs were ca. 0.5 ng/mL. The mean recoveries of melamine from blank water samples spiked at 0.5, 5.0, and 50 ng/mL were more than 86.3%, with the RSD less than 8.8%.
研究了一种从环境水样中分子印迹固相萃取三聚氰胺的方法。在水 - 甲醇体系中合成了环丙氨嗪印迹聚合物，用于从水样中选择性萃取三聚氰胺，随后进行高效液相色谱分析。通过吸附试验和Scatchard分析评估了对三聚氰胺的分子识别特性和结合能力，结果表明，高亲和力结合位点的解离常数（KD）和最大结合量（Qmax）分别为0.032 μmol/L和4.77 μmol/g，低亲和力结合位点的解离常数和最大结合量分别为0.26 μmol/L和19.10 μmol/g。在最佳萃取方案下，该方法可成功应用于选择性萃取和富集环境水中的三聚氰胺。在自来水、湖水和海水分析中，线性范围为0.500至100.0 ng/mL（r > 0.999）。当加载50 mL水样时，该方法的检测限约为0.1 ng/mL，定量限约为0.5 ng/mL。在0.5、5.0和50 ng/mL加标的空白水样中，三聚氰胺的平均回收率超过86.3%，相对标准偏差小于8.8%。
