摘要
建立了浊点萃取法（CPE）对牛奶样品进行净化和浓缩后用高效液相色谱（HPLC）检测的方法。采用三氯乙酸（CCl3COOH）结合非离子型表面活性剂Triton X-100对牛奶进行破乳,以非离子表面活性剂聚乙二醇600（PEG 600）为萃取剂,研究牛奶中三聚氰胺的萃取行为。破乳的最佳条件：Triton X-100的质量浓度为20 g/L,CCl3COOH的质量浓度为20 g/L,100℃水浴加热10 min;CPE方法的最佳条件：PEG600的质量浓度为130 g/L,Na2CO3和Na2SO4的质量浓度分别为5 g/L和260 g/L,平衡温度70℃,平衡时间30 min。在优化的实验条件下,牛奶样品的加标回收率为80%-98%,相对标准偏差为1.2%-5.7%,检出限为0.9mg/kg。该方法简便、快速、灵敏度高、污染少。
A method for the detremination of melamine from milk samples was developed by cloud point extraction combination with high performance liquid chromatography （HPLC）. Triton X - 100 was used for demulsification of milk in the presence of trichloroacetic acid. Surfactant of PEG - 600 was used as extractant and the extraction efficiency of melamine was studied. The optimum conditions of demulsification and CPE were as follows： concentration of Triton X -100：20 g/L; concentration of CCl3COOH： 20 g/L; heating temperature： 100℃; heating time： 10 min; concentrations of PEG600, Na2CO3 and Na2SO4 were 130 g/L, 5 g/L and 260 g/L, respectively; equilitration temperature： 70 ℃ ; equilitration time： 30 min. Under the optimal conditions, the calibration curve was linear for melamine concentration in the range of 0.4 - 80 mg/L with corelation coefficient of 0. 999 8. Spiked recoveries for the standard addition of melamine in the milk was in the range of 80% - 98% with RSDs between 1.2% and 5.7%. The limit of detection for melamine was 0. 9 mg/kg. The method shows advantages of simplicity, high sensitivity and less pollutants.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第10期1221-1224,共4页
Journal of Instrumental Analysis
关键词
三聚氰胺
浊点萃取
表面活性剂
高效液相色谱
melamine
cloud point extraction
surfactant
high performance liquid chromatography
