LC-MS-MS法测定包装材料中壬基酚含量及其迁移量  

Determination nonylphenol residues and migrationin in packages by liquid chromatography tandem mass spectrometry

作　　者：李翔宇 舒敏 陆姝欢 柴莎莎 肖敏 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：《中国食品添加剂》2016年第8期172-176,共5页China Food Additives

基　　金：国家高技术研究发展计划(863计划)项目资助(No.2014AA021703)

摘　　要：采用冷冻高速离心去除油脂及杂质干扰的样品前处理方式,应用高效液相色谱柱进行分离,采用电喷雾（ESI）,以负离子检测模式进行质谱分析,同位素内标法定量,建立了液相色谱-质谱（LC-MSMS）法检测ARA＆DHA产品及包装材料壬基酚（NP）的含量检测分析方法。实验结果表明,壬基酚质量浓度在5~500μg/kg范围内与色谱峰面积呈良好的线性关系,相关系数R2=0.9998,检出限为0.3μg/kg,定量限为1.0μg/kg。ARA＆DHA的微胶囊样品、油脂样品及包装袋三种不同样品的壬基酚不同添加量加标回收率在93.2%~102.9%之间,相对标准偏差（RSD）在2.2%~7.0%之间（n=6）。该方法前处理简便、选择性好、灵敏度高,运用此方法同时研究了包装袋中的壬基酚在ARA＆DHA油脂及微胶囊样品中的迁移量,结果表明,壬基酚含量高的包装袋存在显著的壬基酚迁移现象,故需对包装袋的壬基酚进行严格控制。A new method for determining nonylphenol （NP） in ARA＆DHA products （oil, power and packages） by LC-MS-MS was established. NP was extracted from ARA＆DHA products after D4 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 NP has a good linear relationship with chromatographic peak area in the range of 5 - 500~tg/kg with correlation coefficient of 0.9998, and detection limit of 0.3μg/kg , quantitation limit of 1.0μg/kg. The recoveries under three spiked levels were 93.2% - 102.9%, and the relative standard deviations were 2.2% - 7.0% （n=6） . At the same time, the migration of nonylphenol from the ARA＆DHA products packages was also studied. The data showed significant migration of nonylphenol in the packages, therefore, nonylphenol content in the packages should be well controlled.

关 键 词：壬基酚 液相色谱-质谱 ARA&DHA 包装袋 

分 类 号：TS207.5[轻工技术与工程—食品科学] TS206.4[轻工技术与工程—食品科学与工程]