摘要
[目的]采用QuEChERS前处理-气相色谱质谱(GC-MS)技术,建立不同食品基质中痕量五氯酚及其钠盐的快速检测方法。[方法]样品中加入超纯水涡旋均匀,加入1%(V/V)乙酸乙腈溶液与QuEChERS的盐包涡旋均匀,离心取上清液后,常温氮吹近干,经0.3 mol/L的碳酸钾混匀,乙酸酐衍生,正己烷涡旋萃取,DB-5MS色谱柱分离,GC-MS测定,外标法定量。[结果]五氯酚被衍生剂衍生成五氯苯乙酸酯,五氯酚浓度为1~50 ng/mL时,线性关系良好(R^(2)=0.99992),检出限为0.1μg/kg。在3种加标浓度下,空白基质五氯酚的加标回收率控制在90%~100%。[结论]该方法的灵敏度高、选择性好,定性、定量准确,适用于不同食品基质中五氯酚及其钠盐残留的检测要求。
[Objective]To establish a rapid detection method for trace amounts of pentachlorophenol and its sodium salt in different food matrices by using QuECHERS pretreatment-gas chromatography mass spectrometry(GC-MS)technology.[Method]Add ultrapure water to the sample and vortex uniformly,add 1%(V/V)acetic acid acetonitrile solution and QuECHERS salt packet to vortex uniformly.After centrifugation to take the supernatant,blow dry with nitrogen at room temperature.After mixing with 0.3 mol/L potassium carbonate,derivatize with acetic anhydride,vortex extraction with n-hexane,separate on DB-5MS column,determine by GC-MS,and quantify by external standard method.[Result]Pentachlorophenol was derivatized into pentachlorophenyl acetate by the derivatizing agent.When the concentration of pentachlorophenol was 1-50 ng/mL,the linear relationship was good(R^(2)=0.99992).The detection limit was 0.1μg/kg.At the three spiked concentrations,the spiked recovery rate of the blank matrix pentachlorophenol was controlled within 90% to 100%.[Conclusion]The method has high sensitivity,good selectivity,qualitative and quantitative accuracy,and it is suitable for the detection requirements of pentachlorophenol and its sodium salt residues in different food matrices.
作者
林长钦
苏哪锋
李家宏
田春香
李双宜
LIN Chang-qin;SU Na-feng;LI Jia-hong(Zhongshan City Quality Metrology Supervision and Testing Institute,Zhongshan,Guangdong 528400)
出处
《安徽农业科学》
CAS
2021年第6期190-192,共3页
Journal of Anhui Agricultural Sciences
基金
中山市社会公益科技研究项目(2018B1131)。
