摘要
建立了原料乳中水杨酸的检测方法.样品经乙腈提取,采用超高效液相色谱进行测定.在ZORBAX Eclipse Plus C18反相柱上分离,梯度洗脱,流动相为磷酸水和磷酸甲醇,DAD检测.水杨酸的线性范围为0.5～20μg/m L,相关系数平方(R~2)大于0.995,检出限为0.5 mg/kg,定量限为1.25 mg/kg,3个不同水平的加标回收率为88.0%～118.9%,相对标准偏差不大于10%.方法具有操作简单、重现性好、灵敏度高、杂质干扰小等特点,可以用于原料乳中水杨酸的检测.
A method for the detection of salicylic acid in raw milk was set up. The sample was extracted with acetonitrile and determined by ultra performance liquid chromatography,and separated on a ZORBAX Eclipse Plus C18 reversed-phase column,using gradient elution,with a mobile phase of phosphoric acid water and methanolic acid,and a DAD detection.The linear range of salicylic acid was 0.5 ～ 20 μg/m L,the correlation coefficient squared( R~2) was more than 0.995,the detection limit was 0.5 mg/kg,the quantification limit was 1. 25 mg/kg,the average recovery rate of the three different levels were between 88.0 % to 118.9%,and the relative standard deviation was not more than 10%. The method had the characteristics of simple operation,good reproducibility,high sensitivity,small impurity interference and can be used for the detection of salicylic acid in raw milk.
引文
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