分散固相萃取-超高效液相色谱-串联质谱法测定膨化食品中的全氟辛酸和全氟辛烷磺酸  

Determination of Perfluorooctanoic Acid and Perfluorooctane Sulfonic Acid in Puffed Food by Dispersed Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘莎 魏兴峰 杨迪 黄水林 全海倩 LIU Sha;WEI Xingfeng;YANG Di;HUANG Shuilin;QUAN Haiqian(Shenzhen Shum Yip Space Food&Environmental Testing Technology Co.,Ltd,Shenzhen 518040,China)

机构地区：[1]深圳市深业航天食品与环境检测科技有限公司,广东深圳518040

出　　处：《现代食品》2024年第17期215-219,共5页Modern Food

摘　　要：目的:建立了同时测定膨化食品中全氟辛酸(Perfluorooctanoic Acid,PFOA)和全氟辛烷磺酸(Perfluorooctane Sulfonic Acid,PFOS)的超高效液相色谱-串联质谱法。方法:样品经2%甲酸-乙腈提取后,盐析分层,高速离心后,乙腈相使用50 mg C18、20 mg GCB、100 mg PSA固相萃取剂联合净化。在正离子模式下使用电喷雾电离源进行离子化,并采用多反应监测模式进行测定。结果:PFOA和PFOS的内标曲线在各自给定的浓度范围呈现良好线性关系,相关系数R^(2)分别为0.9995和0.9997。PFOA和PFOS的检出限分别为0.02µg·kg^(-1)和0.10µg·kg^(-1),定量限分别为0.05µg·kg^(-1)和0.25µg·kg^(-1)。在1倍、2倍、10倍定量限的添加浓度下,PFOA和PFOS在饼干、薯片、方便面中的平均回收率为73.9%~93.1%,相对标准偏差为3.89%~7.22%。结论:方法回收率高、重现性好、操作简单,可满足膨化食品中PFOA和PFOS的测定要求。Objective:An ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for simultaneous determination of perfluorooctanoic acid(PFOA)and perfluorooctane sulfonic acid(PFOS)in puffed food products had been developed.Method:The method involved extraction of the samples with 2%formic acid-acetonitrile,followed by salted out and centrifugation.The acetonitrile phase was purified using a combination of 50 mg C18,20 mg GCB,and 100 mg PSA solid-phase extraction sorbents.The final followed by ionization using an electrospray ionization source(ESI)in positive ion mode and determination was conducted by multiple reaction monitoring(MRM)mode.Result:The internal standard calibration curves for PFOA and PFOS showed excellent linearity within their respective concentration ranges with correlation coefficients(R^(2))of 0.9995 and 0.9997,respectively.The detection limits of PFOA and PFOS were 0.02µg·kg^(-1) and 0.10µg·kg^(-1),respectively,and the quantification limits were 0.05µg·kg^(-1) and 0.25µg·kg^(-1),respectively.At the concentration of 1,2,and 10 times the limit of quantification,the average recoveries of PFOA and PFOS in biscuits,potato chips,and instant noodles were 73.9%~93.1%,and the relative standard deviations were 3.89%~7.22%.Conclusion:The method has high recovery,good reproducibility,and simple operation,and can meet the requirements for the determination of PFOA and PFOS in puffed foods.

关 键 词：分散固相萃取 超高效液相色谱-串联质谱法 膨化食品 全氟辛酸 

分 类 号：O657.63[理学—分析化学]