液相色谱-串联质谱法测定ARA&DHA油脂中的壬基酚  

Determination of nonylphenol in ARA & DHA oil by liquid chromatography tandem mass spectrometry

作　　者：李翔宇 舒敏 肖敏 柴莎莎 汪志明 

机构地区：[1]嘉必优生物工程(武汉)有限公司,武汉430073 [2]湖北省营养化学品生物合成工程技术研究中心,武汉430223

出　　处：《食品科技》2016年第4期289-293,共5页Food Science and Technology

基　　金：国家高技术研究发展计划(863计划)项目(2014AA021703)

摘　　要：采用将内标溶于油脂中的方法对样品前处理,冷冻高速离心去除油脂及杂质干扰,应用高效液相色谱柱进行分离,采用电喷雾(ESI),以负离子检测方式进行质谱分析,同位素内标法定量,建立了液相色谱-质谱(LC-MS-MS)法检测ARA&DHA油脂中壬基酚(NP)含量的方法。实验结果表明,壬基酚质量浓度在5μg/kg^500μg/kg范围内与色谱峰面积呈良好的线性关系,相关系数R^2=0.9998,检出限为0.3μg/kg。在3个添加水平下,样品的加标回收率为96.9%~105.2%,相对标准偏差(RSD)在2.9%~7.3%之间(n=6)。该方法的建立为ARA&DHA油脂中壬基酚的检测提供了一种前处理简便、选择性好、灵敏度高的检测方法。A new method for determining nonylphenol（NP） in ARA ＆ DHA oil by LC-MS-MS was established in this paper. NP was extracted from ARA ＆ DHA oil after D5-NP been added, and the extracted solution was determined by HPLC-MS-MS, using C18 reverse phase column and electron spray ionization （ESI）. Internal standard was used for quantification. The results showed that the concentration of the NP has a good linear relationship with the chromatographic peak area in the range of 5 μg/kg -500 μg/kg with correlation coefficient of 0.9998, and detection limit of 0.3 μg/kg. The recoveries under three spiked levels were 96.9%-105.2%, and the relative standard deviations were 2.9%-7.3% （n=6）. The established method provides a method, which has the characteristic of simple pretreatment, good selectivity and high sensitivity, for the detection of NP in ARA ＆ DHA oil.

关 键 词：壬基酚 液相色谱-质谱 ARA&DHA油脂 

分 类 号：TS221[轻工技术与工程—粮食、油脂及植物蛋白工程]