摘要
建立在线凝胶渗透色谱–气相色谱-串联质谱法(GPC-GCMS/MS)测定食用植物油中11种有机磷阻燃剂的分析方法。0.5 g食用油样品用(3∶7)丙酮/环己烷溶液稀释定容5 mL,GPC-GCMS/MS采用多反应监测模式(MRM)测定,外标法定量。11种有机磷阻燃剂在1~50μg/L范围内,线性关系良好,相关系数r>0.997 0,方法检出限为1.0~3.0μg/kg,定量限为3.0~9.0μg/kg。空白样品中添加3个水平质量浓度,回收率在65.6%~129.0%之间,相对标准偏差RSD为0.2%~13.9%。该方法样品前处理简单,仪器自动化程度高,重复性较好,适用于食用植物油中有机磷阻燃剂的检测。
A method was established for the determination of 11 organophosphorus flame retardants in edible oils by gel permeation chromatography-gas chromatography-tandem mass spectrometry(GPC-GCMS/MS).The 0.5 g edible oil sample was diluted with(3∶7) acetone/cyclohexane solution to a constant volume of 5 mL. GPC-GCMS/MS was determined by multiple reaction monitoring mode(MRM) and quantified by external standard method. The linear calibration correlation coefficients r for all 11 OPFRs were at least 0.9970 in the range of 1~50 μg/L.The detection limit of the method was 1.0~3.0 μg/kg, and the lower limit of determination was 3.0~9.0 μg/kg. Three levels of spiked test were performed. Most of the recoveries were in the range of 65.6%~129.0%, and the relative standard deviations(RSDs) for the 11 OPFRs were 0.2%~13.9%(n=6). The method exhibited simple sample pretreatment, high instrument automation, good reproducibility, and was suitable for the detection of organic phosphorus flame retardants in edible vegetable oils.
作者
倪海平
刘祥萍
李登昆
张云
Ni Haiping;Liu Xiangping;Li Dengkun;Zhang Yun(Nanjing Municipal Center for Disease Control and Prevention Affiliated to Nanjing Medical University,Nanjing 210003)
出处
《中国粮油学报》
CAS
CSCD
北大核心
2022年第12期246-250,共5页
Journal of the Chinese Cereals and Oils Association
