超高效液相色谱-质谱法测定被膜剂中烷基苯酚聚氧乙烯醚类  

Determination of alkylphenol ethoxylates in coating agent by ultra high performance liquid chromatography-mass spectrometry

作　　者：范小龙 褚毅宏 吴婉琴 江丰 朱松松 朱正伟 朱晓玲 张亚珍 王福燕[5] FAN Xiaolong;CHU Yihong;WU Wanqin;JIANG Feng;ZHU Songsong;ZHU Zhengwei;ZHU Xiaoling;ZHANG Yazhen;WANG Fuyan(Hubei Provincial Institute for Food Supervision and Test,Hubei Wuhan 430075,China;Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Hubei Wuhan 430075,China;Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation,Hubei Wuhan 430075,China;Thermowell(Hubei)Intelligent Technology Co.,Ltd,Hubei Wuhan 430075,China;School of Medicine,Jianghan University,Hubei Wuhan 430075,China)

机构地区：[1]湖北省食品质量安全监督检验研究院,湖北武汉430075 [2]湖北省食品质量安全检测工程技术研究中心,湖北武汉430075 [3]国家市场监管重点实验室(动物源性食品中重点化学危害物检测技术),湖北武汉430075 [4]赛默威(湖北)智能科技有限公司,湖北武汉430075 [5]江汉大学医学部,湖北武汉430075

出　　处：《中国食品卫生杂志》2024年第6期688-694,共7页Chinese Journal of Food Hygiene

摘　　要：目的建立超高效液相色谱-质谱法(UPLC-MS)测定被膜剂中辛基苯酚聚氧乙烯醚(OPEO)和壬基苯酚聚氧乙烯醚(NPEO)的含量。方法被膜剂样品经水提取,固相萃取柱净化后,采用Thermo Acclaim RSLC 120 C_(18)(2.1 mm×100 mm,2.2μm)色谱柱分离,乙腈和0.1%甲酸水为流动相,梯度洗脱,电喷雾正离子模式,选择离子监测模式定量。结果OPEO和NPEO在0~400μg/L浓度范围内线性良好(r^(2)>0.996),在0.12、0.24、1.2 mg/kg添加水平下的平均回收率为88.5%~96.9%,相对标准偏差为2.9%~7.0%,两种化合物定量限均为0.12 mg/kg。结论该方法操作简便、快速、准确,其灵敏度、准确度和精密度均适用于被膜剂中烷基苯酚聚氧乙烯醚类的定性分析和定量检测。Objective A method of ultra performance liquid chromatography-mass spectrometry(UPLC-MS)was established for the determination of octylphenol ethoxylates(OPEO)and nonylphenol ethoxylates(NPEO)in coating agent.Methods Samples were extracted with water,and purified by solid phase extraction column.And Thermo Acclaim RSLC 120 C_(18)(2.1 mm×100 mm,2.2μm)chromatographic column was used for separation.Acetonitrile and 0.1%formic acid water were mobile phase,gradient elution and quantification was performed in SIM mode with positive ion mode of electrospray ionization.Results Octylphenol ethoxylates(OPEO)and nonylphenol ethoxylates(NPEO)were in the range of 0-400μg/L,and the linear relationships was good(r^(2)>0.996).The recoveries at three spiked levels(0.12,0.24 mg/kg,1.2 mg/kg)were 88.5%-96.9%with the relative standard deviation of 2.9%-7.0%,and the limits of quantitative was 0.12 mg/kg.Conclusion The method was simple,rapid and accurate.Its sensitivity,accuracy and precision were suitable for the quantitative analysis and determination of alkylphenol ethoxylates in coating agent.

关 键 词：超高效液相色谱-质谱法 被膜剂 烷基苯酚聚氧乙烯醚类 

分 类 号：R155[医药卫生—营养与食品卫生学]