原料奶中三聚氰胺检测的三种前处理方法比较

The comparison of three pre-treatment methods for melamine's measure of raw milk

以国家标准检测方法为参照,对高效液相色谱法检测原料乳中三聚氰胺含量的三种前处理方法进行了比较,利用反相离子对色谱法,在离子对试剂缓冲盐溶液-乙腈=9∶1为流动相,1.0mL/min的流速,C18色谱柱,40℃柱温的条件下,使用配有紫外检测器的高效液相色谱仪在240nm范围内对目标组分进行分离和测定。通过加入三种不同沉淀剂的方法,对原料奶中的三聚氰胺进行提取,结果显示,方法一具有非常好的准确度和精密度,但整个操作过程非常复杂,耗时较长;方法二的沉淀效果较好,但试剂峰过高,基线波动较大;而方法三不仅沉淀效果好,准确度及精密度较佳,更在前处理时间及检测成本上具有明显优势,适用于原料奶中三聚氰胺的快速检测。

Based on the national standards, three pre - treatment methods for melamine＇ s measure of raw milk were compared. By the ion reversed - phase chromatography, the target component was separated and measured using the HPLC with UV detector at 240nm while the mobile phase was composed with buffler and aeetonitrile （9 ： 1 ）, flow rate was 1. 0mL/min and the temperature was 40℃. Three different extractions of melamine in raw milk were got by adding three different precipitation. The results shown that, the first method has very good accuracy and precision, but the whole process was very complicated and took a long time; the second method precipitation effect was better, but the reagent peaks were exorbitant and its baseline was fluctuations; and the third method not only had good precipitation effect, accuracy and precision, but also had obvious advantages in the pre - treatment time and testing cost. Method 3 is suitable for the rapid determination of melamine in raw milk.