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[高效毛细管电泳法测定牛奶和奶粉中的三聚氰胺]

[Determination of melamine in milk and milk powder by high performance capillary electrophoresis].

作者信息

Rao Qinxiong, Tong Jing, Guo Ping, Li Haiyan, Li Xiaowei, Ding Shuangyang

机构信息

Institute for Agri-food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201106, China.

出版信息

Se Pu. 2008 Nov;26(6):755-8.

Abstract

A high performance capillary electrophoresis (HPCE) method has been established for the separation of melamine in milk and milk powder. The separation was carried out on a fused-silica uncoated capillary column (58.5 cm x 75 microm). The sample was injected by hydrodynamic injection (3.5 kPa (35 mbar) x 8 s) at a temperature of 25 degrees C. The analysis was completed in about 6 min in 40 mmol/L Na2HPO4-20 mmol/L citric acid buffer (pH 2.6) at 25 kV of separation voltage and 232 nm of detection wavelength. The linear range of melamine was 1 - 100 mg/kg, and the correlation coefficient was higher than 0. 997. The limits of quantification (LOQs) in milk and milk powder were 0.5 mg/kg and 1.0 mg/kg, respectively. The average recoveries were in the range of 72.2% -97.3% in the spiked range of the concentration of LOQs and 50 mg/kg, and the relative standard deviations were between 2.1% and 3.9%.

摘要

建立了一种用于分离牛奶和奶粉中三聚氰胺的高效毛细管电泳(HPCE)方法。分离在未涂层熔融石英毛细管柱(58.5 cm×75μm)上进行。在25℃温度下通过流体动力学进样(3.5 kPa(35 mbar)×8 s)进样。在40 mmol/L Na2HPO4 - 20 mmol/L柠檬酸缓冲液(pH 2.6)中,于25 kV分离电压和232 nm检测波长下,约6分钟完成分析。三聚氰胺的线性范围为1 - 100 mg/kg,相关系数高于0.997。牛奶和奶粉中的定量限(LOQs)分别为0.5 mg/kg和1.0 mg/kg。在定量限浓度和50 mg/kg的加标范围内,平均回收率为72.2% - 97.3%,相对标准偏差在2.1%至3.9%之间。

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