摘要
建立了快速、高效的酱油中三氯丙醇的固相萃取净化-气相色谱-串联质谱法(GC-QqQ-MS/MS)测定方法。0.5g酱油,加0.5mL饱和NaCl盐析,超声15min后经弗罗里硅土固相萃取柱净化,无水乙醚洗脱,d5-3-MCPD为内标,七氟丁酰基咪唑衍生化,加饱和NaCl 3mL混匀,有机层进GC-QqQ-MS/MS分析。净化时间少于20min。方法回收率为101.36%,线性范围在0.05-5.0mg/kg,线性相关系数R2=0.99997,方法检出限为0.005mg/kg,该方法对酱油中三氯丙醇的测定有良好的效果。
A fast, effective method for analysis of 3 -MCPD in soy sauces was developed by modified SPE- GC -QqQ- MS/MS method. 0. 5g of soy sauces, which was added 0. 5 mL saturated NaC1, and was extracted by ultrasonic for 15rain, and then was purified by Florisil -SPE. D5 -3 -MCPD and N - Heptafluorobutyrylimidazole was used as the internal standard and derivative reagent respectively The re- covery was 101.36% ,liner ranges were 0.05 -5.0mg/kg,correlation coefficient R2 =0. 99997 ,the limit of detection was O. 005mg/kg. This method meet the requirement of determiantion of 3 - MCPD in soy sauces.
出处
《齐鲁师范学院学报》
2012年第5期73-76,共4页
Journal of Qilu Normal University
基金
山东省质量技术监督检验局科研项目(2009KY13)
