首页|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

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

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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R2 分别为 0.999 5 和 0.999 7.PFOA和PFOS的检出限分别为0.02 µg·kg-1 和 0.10 µg·kg-1,定量限分别为 0.05 µg·kg-1 和 0.25 µg·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.
Determination of Perfluorooctanoic Acid and Perfluorooctane Sulfonic Acid in Puffed Food by Dispersed Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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(R2)of 0.999 5 and 0.999 7,respectively.The detection limits of PFOA and PFOS were 0.02 µg·kg-1 and 0.10 µg·kg-1,respectively,and the quantification limits were 0.05 µg·kg-1 and 0.25 µg·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.

dispersion solid-phase extractionultra high performance liquid chromatography-tandem mass spectrometrypuffed foodperfluorooctanoic acid

刘莎、魏兴峰、杨迪、黄水林、全海倩

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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

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

2024

现代食品
国家粮食储备局郑州科学研究设计院

现代食品

影响因子:0.169
ISSN:2096-5060
年,卷(期):2024.30(17)