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作 者:谢景千[1] 杨俊[1] 黎永乐[1] XIE Jing-Qian;YANG Jun;LI Yong-Le(Shenzhen Academy of Metrology and Quality Inspection,Shenzhen 518055,China)
出 处:《食品安全质量检测学报》2020年第24期9100-9107,共8页Journal of Food Safety and Quality
基 金:国家重点研发计划项目(2018YFC1603201、2018YFC1603200);广东省市场监督管理局科技项目(2020CS05)。
摘 要:目的建立液相色谱-串联质谱法测定食品接触材料中双酚F和双酚S迁移量的分析方法。方法样品经水、4%乙酸、10%乙醇、20%乙醇、50%乙醇、95%乙醇和橄榄油等7种食品模拟液浸泡实验后,浸泡液经过滤后进样,以甲醇-水为流动相,经过T3色谱柱分离,用外标法在负离子模式下以电喷雾电离多反应模式监测进行定量分析。结果6种食品模拟物(除橄榄油外)中双酚F和双酚S分别在10~200μg/L和0.5~10.0μg/L浓度范围内有好的线性,相关系数r均大于0.9995,方法检出限分别为0.002、0.0001 mg/kg,定量限分别为0.01、0.0005 mg/kg,在食品模拟物橄榄油中双酚F和双酚S分别50.0~750、2.50~37.5μg/kg浓度范围内线性很好,相关系数r均为0.9999,检出限分别为0.01、0.0005 mg/kg,定量限分别为0.05、0.0025 mg/kg。双酚F的加标回收率为90.4%~108%,相对标准偏差为0%~5.27%,双酚S加标回收率为84.4%~107%,相对标准偏差为0%~4.60%。结论该方法操作简便、灵敏度高、准确性好,能满足食品接触材料中双酚F和双酚S的迁移量的检测。Objective To establish a method for the determination of bisphenol F and bisphenol S migration from food contact materials by liquid chromatography-tandem mass spectrometry.Methods After immersion of samples in 7 kinds of food stimulants,including water,4%acetic acid solution,10%ethanol solution,20%ethanol solution,50%ethanol solution,95%ethanol solution and olive oil,the immersion solutions were filtrated.The separation was performed by using a T3 chromatographic column with methanol-water as mobile phase.The eluent was quantitatively determined by external reference method of liquid chromatography-tandem mass spectrometry using multiple reaction monitoring under the negative-ion mode.Results The calibration curves of bisphenol F and bisphenol S in 6 kinds of food simulations(expect for olive oil)were linear in the range of 10-200μg/L and 0.5-10.0μg/L with correlation coefficients more than 0.9995,the limits of detection of the method for bisphenol F and bisphenol S were 0.002 mg/kg and 0.0001 mg/kg,and the limits of quantification were 0.01 mg/kg and 0.0005 mg/kg.The calibration curves of bisphenol F and bisphenol S in food simulation of olive oil were linear in the range of 50.0-750μg/kg and 2.50-37.5μg/kg,the correlation coefficients of bisphenol F and bisphenol S were 0.9999,the limits of detection of bisphenol F and bisphenol S in olive oil were 0.01 mg/kg and 0.0005 mg/kg,and the limits of quantification were 0.05 mg/kg and 0.0025 mg/kg.The recoveries of bisphenol F were 90.4%-108%,with relative standard deviations of 0%-5.27%,and the recoveries of bisphenol S were 84.4%-107%,with relative standard deviations of 0%-4.6%.Conclusion This method is convenient,sensitive and accreted,which is suitable for quantitative analysis of bisphenol F and bisphenol S migration in food contact materials.
关 键 词:液相色谱-串联质谱法 食品接触材料 双酚F 双酚S 迁移
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