Faculty of Technology, Telemark University College, Porsgrunn, Norway.
J Sep Sci. 2010 Mar;33(6-7):988-95. doi: 10.1002/jssc.200900815.
A hydrophilic interaction liquid chromatography-UV method was developed for the determination of melamine in milk powder. Sulfobetaine type zwitterionic hydrophilic interaction liquid chromatography stationary phase was used to achieve straightforward separation of melamine in milk powder without any sample derivatization or addition of ion-pair reagent. The sample preparation was simple and fast with the steps of acetonitrile/perchloric acid extraction-centrifugation-filtration. No SPE or other pre-concentration procedure was required. By using large volume sample injection and choosing low UV wavelength (210 nm), the LOD and LOQ were 0.005 and 0.015 microg/mL for melamine standards, and 0.02 and 0.06 microg/mL for the spiked milk extracts. The LOD and LOQ of the latter correspond to 0.95 and 2.2 microg/g melamine in the milk powder. The correlation coefficients for melamine standard, pre-spiked milk extracts and post-spiked milk extracts in the range of 0-0.5 microg/mL were 0.9978, 0.9976 and 0.9995, respectively. This newly developed method is sensitive and cost effective, therefore, suitable for screening of melamine in tainted milk products.
建立了一种亲水作用色谱-紫外检测法用于检测奶粉中的三聚氰胺。采用两性离子亲水作用色谱固定相,无需对样品进行衍生化或添加离子对试剂,即可直接分离奶粉中的三聚氰胺。样品制备简单快速,经乙腈/高氯酸提取-离心-过滤处理。无需固相萃取或其他浓缩步骤。采用大体积进样和选择低紫外波长(210nm),三聚氰胺标准品的检出限和定量限分别为 0.005 和 0.015μg/mL,添加的牛奶提取物的检出限和定量限分别为 0.02 和 0.06μg/mL。后者的检出限和定量限分别对应于奶粉中三聚氰胺的 0.95 和 2.2μg/g。三聚氰胺标准品、预添加牛奶提取物和后添加牛奶提取物在 0-0.5μg/mL 范围内的相关系数分别为 0.9978、0.9976 和 0.9995。该新方法灵敏且经济,因此适用于检测受污染的乳制品中的三聚氰胺。