液相色谱-串联质谱法测定食品中壬基酚残留  

Determination of Nonyl Phenol Residue in Food by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王浩[1] 贾婧怡 于晓瑾[1] 张杉[1] 张旭[1] 陈江龙 WANG Hao;JIA Jingyi;YU Xiaojin;ZHANG Shan;ZHANG Xu;CHEN Jianglong(China National Food Quality and Safety Supervision and Inspection Center,Beijing 100094)

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《食品工业》2020年第2期271-275,共5页The Food Industry

基　　金：婴配食品生产与应用全程质量管控与评价技术(2017YFC1601003);食品安全国家标准项目计划(spaq-2017-080).

摘　　要：试验旨在建立食品中壬基酚残留的液相色谱-三重四极杆串联质谱检测方法。样品经乙腈提取壬基酚同时除去蛋白质。以Hypersil GOLD C18色谱柱(4.6 mm×50 mm, 1.9μm)分离,流动相为甲醇-水(10︰90, V/V),流速0.35 mL/min,液相色谱-串联质谱仪测定,内标法定量。在该优化条件下,包装饮用水的检出限为0.050μg/kg,定量限为0.100μg/kg, RSD为2.9%~5.6%;其它类食品的检出限均为1.00μg/kg,定量限均为2.00μg/kg, RSD为2.8%~9.4%。典型基质加标水平设定为10, 20和100μg/kg,方法平均回收率为86.0%~114.3%,平均相对标准偏差为2.8%~9.5%(n=6)。该方法前处理简单,灵敏度高,适用于食品中壬基酚残留的准确定性、定量分析。A liquid chromatography-tandem mass spectrometry(LC-MS/MS) method was established for determination of nonylphenol residues in food. Nonylphenol residues extraction and protein removal in samples were used by acetonitrile. The chromatographic separation was carried out on a Hypersil GOLD C18 column(4.6 mm×50 mm, 1.9 μm) using a methanol and water(10︰90, V/V) mobile phase by isocratic elution at a flow rate of 0.35 m L/min. Internal standard method was used for quantitative analysis. The limits of quantification and the limits of detection for drinking water were 0.050 μg/kg and 0.100 μg/kg, respectively, and RSD was 2.9%-5.6%. The limits of quantification and the limits of detection for general food were 1.00 μg/kg and 2.00 μg/kg, respectively, and RSD was 2.8%-9.4%. Three different levels of nonylphenol standards were added to general food samples, which were 10, 20 and 100 μg/kg. The method recovery ranged from 86.0% to 114.3%, also the mean relative standard deviations ranged from 2.8% to 9.5%(n=6). As a result, a simple, rapid, sensitive and effective method for qualification and quantification of nonylphenol residues in food was provided.

关 键 词：液质联用法 食品 壬基酚 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]