超高效液相色谱-串联质谱法测定动物源性食品中的五氯酚  

Determination of Pentachlorophenol in Food of Animal Origin by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄霞 邓枫 HUANG Xia;DENG Feng(Changsha Medical university,Changsha 410219,China)

机构地区：[1]长沙医学院,湖南长沙410219

出　　处：《食品安全导刊》2025年第5期99-102,共4页China Food Safety Magazine

摘　　要：目的:建立超高效液相色谱-串联质谱法测定动物源性食品中五氯酚的方法。方法:乙腈超声提取样品,离心取上清液氮吹至近干,使用甲醇和正己烷进行溶解,离心取下层液体经Agilent plus C_(18)色谱柱(50 mm×2.1 mm,1.8μm)分离,流动相为乙腈-乙酸铵水溶液(含0.1%甲酸),梯度洗脱,采用电喷雾电离,多反应监测模式下进行检测。结果:方法在0.50~20.00μg·L^(-1)具有良好的线性关系(r>0.9995),方法的检出限为0.50μg·kg^(-1),定量限为1.67μg·kg^(-1)。样品的回收率为81.0%~98.8%,相对标准偏差为0.54%~3.86%。结论:该方法符合《实验室质量控制规范食品理化检测》(GB/T 27404—2008)中的技术要求,适用于动物源性食品中五氯酚残留的测定。Objective:To establish an ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of pentachlorophenol in food of animal origin.Method:Acetonitrile samples were extracted by ultrasonic extraction,supernatant liquid nitrogen was centrifuged and blown to near-dry,dissolved with methanol and n-hexane,and the lower liquid was centrifuged and separated on Agilent plus C18 column(50 mm×2.1 mm,1.8μm)with the mobile phase consisting of acetonitrile-ammonium acetate aqueous solution(containing 0.1%formic acid).Gradient elution,electrospray ionization,multi-reaction monitoring mode was used for detection.Result:The results showed a good linear relationship(r>0.9995)in the range of 0.50μg·L^(-1)to 20.00μg·L^(-1).The limit of detection was 0.50μg·kg^(-1),and the limit of quantification was 1.67μg·kg^(-1).The recoveries were 81.0%to 98.8%,and the relative standard deviation was 0.54%to 3.86%.Conclusion:The method meets the technical requirements in GB/T 27404—2008,and is suitable for the determination of pentachlorophenol residues in food of animal origin.

关 键 词：五氯酚 超高效液相色谱-串联质谱法 内标法 

分 类 号：O657.63[理学—分析化学] TS207.5[理学—化学]