改进QuEChERS方法结合气相色谱串联质谱检测黄瓜中的邻苯二甲酸酯类
目的 建立Fe3O4磁性纳米材料QuEChERS结合气相色谱串联质谱联用仪检测黄瓜中15种邻苯二甲酸酯类残留的方法。方法 样品采用乙腈超声提取, 经无水MgSO4和NaCl盐析离心后, 通过Fe3O4磁性纳米材料结合C18和GCB吸附剂净化, 采用气相色谱串联质谱MRM模式测定。结果 在20~2000 μg/kg范围内线性关系良好(r2≥0.9985), 检出限(S/N=3)为0.37~1.58 μg/kg。进行了20、50和200 μg/kg 3个添加浓度的15种邻苯二甲酸酯类的回收率试验, 回收率在84.9%~111.6%; RSD为0.41%~6.84%。结论 该方法准确、灵敏, 符合多残留检测和痕量分析的技术要求, 适用黄瓜等蔬菜中邻苯二甲酸酯类残留的分析。
Objective To establish a method based on QuEChERS sample preparation method with Fe3O4 magnetic nanoparticles as the absorbing material and gas chromatography-tandem mass spectrometry (GC-MS/MS) for the determination of 15 kinds of phthalate esters residues in cucumber. Method The samples were extracted by ultrasound (homogeneity) using acetonitrile, and then salted out with sodium chloride and anhydrous magnesium sulfate. The supernatant was purified by C18, Fe3O4 magnetic nanoparticles and gra-phitized carbon black (GCB) sorbents, and detected by GC-MS/MS with multiple reaction monitoring (MRM) mode. Results Under the optimum conditions, a good linearity was obtained in the range of 20~2000 ug/kg with correlation coefficients ranging from 0.9985 to 1, and the detection limit(S/N=3)ranging from 0.37 to 1.58 ug/kg. Recovery data were obtained for 15 kinds of phthalate esters spiked into sample extracts at concentrations of 20, 50 and 200 ug/kg. The average recoveries of the phthalate esters ranged from 84.9% to 111.6% and the relative standard deviation (RSD) ranged from 0.41% to 6.84%. Conclusion This method is accurate and sensitive to meet the requirements of multiple residues determination, and can be applied in the analysis of phthalate esters residues in vegetables.
标题：改进QuEChERS方法结合气相色谱串联质谱检测黄瓜中的邻苯二甲酸酯类
英文标题：Determination of 15 kinds of phthalate esters in cucumber using gas chro-matography-tandem mass spectrometry with QuEChERS method
作者：
宫俊杰 天津科技大学海洋与环境学院;龙大食品集团有限公司
孙欣 山东农业大学食品科学与工程学院
王明林 山东农业大学食品科学与工程学院
邓泽慧 山东农业大学食品科学与工程学院
宋艳秋 山东农业大学食品科学与工程学院
刘文岭 天津科技大学海洋与环境学院
张敏 龙大食品集团有限公司
中文关键词:邻苯二甲酸酯类,Fe3O4磁性纳米材料,QuEChERS,气相色谱质谱法,黄瓜,
英文关键词:phthalate esters,Fe3O4 magnetic nanoparticles,QuEChERS,gas chromatography-tandem mass spectrometry,cucumber,
发表日期：2015-12-01
- 文件大小:
- 831.02 KB
- 下载次数:
- 60
-
高速下载
|
|
