Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemical and Environmental Sciences, Hebei University, Baoding, PR China.
Electrophoresis. 2010 Jul;31(13):2236-41. doi: 10.1002/elps.201000025.
A novel and simple method was, for the first time, developed for effective separation and sensitive detection of cyromazine (CM) and its metabolite melamine (MM) by CZE with DAD (CZE-DAD). Among different solvents, ACN containing 20% NH(4)OH was found to be the best one as an extractant of CM and MM in real samples. After centrifugation and filtering, the extract was analyzed by CZE-DAD directly. The linearity is good in the range of 0.7-50 mg/L with correlation coefficient (r) of 0.9998. Under the optimal conditions, the method LOQ for the two analytes was 0.38 mg/kg for feed samples and 0.42 mg/kg for egg and liquid milk samples. The peaks of MM and CM were identified by comparison of their migration times in real samples with that in standard solution and spiked sample. The effective baseline separation and high sensitivity of MM and CM were achieved. The proposed method has been applied successfully for the quantitative determination of CM and MM residues in real samples. The average total recoveries ranged from 92.5 to 97.4% with the RSD of 3.0-5.1% for CM and from 93.0 to 97.6% with the RSD of 2.8-4.9% for MM. The proposed method offers the effective separation selectivity of CZE as well as a quicker analysis time for simultaneous determination of CM and MM in feed, egg and liquid milk.
首次发展了一种新颖且简单的方法，通过 CZE 与 DAD（CZE-DAD），可有效分离和灵敏检测环丙氨嗪（CM）及其代谢物三聚氰胺（MM）。在不同溶剂中，发现含有 20% NH(4)OH 的 ACN 最适合作为实际样品中 CM 和 MM 的提取剂。离心和过滤后，直接用 CZE-DAD 分析提取物。在 0.7-50mg/L 范围内具有良好的线性关系，相关系数（r）为 0.9998。在最佳条件下，两种分析物的方法 LOQ 对于饲料样品为 0.38mg/kg，对于鸡蛋和液态奶样品为 0.42mg/kg。通过比较实际样品中 MM 和 CM 的迁移时间与标准溶液和加标样品中的迁移时间来鉴定 MM 和 CM 的峰。实现了 MM 和 CM 的有效基线分离和高灵敏度。该方法已成功应用于实际样品中 CM 和 MM 残留量的定量测定。CM 的平均总回收率范围为 92.5-97.4%，RSD 为 3.0-5.1%，MM 的平均总回收率范围为 93.0-97.6%，RSD 为 2.8-4.9%。该方法提供了 CZE 的有效分离选择性以及更短的分析时间，可用于同时测定饲料、鸡蛋和液态奶中的 CM 和 MM。
