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作 者:白泽清 BAI Ze-qing(Xiamen Products Quality Supervision&Inspection Institute,Fujian Xiamen 361004,China;National Testing Center for Logistics Packing Products(Fujian),Fujian Xiamen 361004,China;Xiamen Key Laboratory for Safety Evaluation and Testing of Food Packaging Material,Fujian Xiamen 361004,China)
机构地区:[1]厦门市产品质量监督检验院,福建厦门361004 [2]国家物流包装产品质量检验检测中心(福建),福建厦门361004 [3]厦门市食品包装材料安全评价及检测重点实验室,福建厦门361004
出 处:《包装工程》2022年第19期167-172,共6页Packaging Engineering
基 金:国家市场监督管理总局科技计划(2019MK081)。
摘 要:目的提出聚亚苯基砜(PPSU)奶瓶4,4′–联苯二酚迁移量的超高效液相色谱–串联质谱分析方法(UPLC–MS/MS),为婴幼儿食品包装质量安全测试方法提供依据。方法在70℃、2 h条件下,采用体积分数50%的乙醇溶液(食品模拟物)对样品进行迁移实验,采用C18色谱柱分离,以超纯水和甲醇为流动相梯度洗脱,通过电喷雾电离源(ESI)负离子模式和多反应监测(MRM)进行采集、扫描,并进行定性和定量检测,采用外标法进行定量分析。结果在优化条件下,目标物在5~200μg/L内线性关系良好,相关系数(R2)大于0.9999,检出限和定量下限分别为1.5μg/L和5μg/L。该方法的基质效应值为95.8%~114%,加标回收率为95.2%~105%,相对标准偏差(RSD)为1.0%~1.7%(n=6)。结论该方法具有快速、准确且灵敏度高等特点,适用于PPSU奶瓶4,4′–联苯二酚迁移量的测定。The work aims to develop an ultra-performance liquid chromatograph-tandem mass spectrometry(UPLC-MS/MS)method for determination of 4,4′-dihydroxybiphenyl migrated from polyphenylene sulfone feed-ing-bottles(PPSU)to provide test method basis of quality and safety of infant food packaging.The 50%(V/V)etha-nol/water solution was chosen as food simulant to conduct the migration tests under testing conditions of(70℃,2 h),and the analytes were separated on a C18 chromatographic column by gradient elution with a mobile phase consisting of deionized water and methyl alcohol.The qualitative and quantitative testing of 4,4′-dihydroxybiphenyl were carried out by multiple-reaction monitoring(MRM)collecting and scanning with electrospray ionization(ESI)source operating in the negative ionization mode,and external standard method was used for quantitative detection.Under the optimized conditions,there was a good linear relationship(with correlation coefficient R2>0.9999)for the analyte in the concentration range of 5-200μg/L.The limit of detection(LOD)and the limit of quantitation(LOQ)were 1.5μg/L and 5μg/L,respectively.The matrix effects of the method were in the range of 95.8%-114%,and the recovery range was 95.2%to 105%,and the relative standard deviation(RSD)was 1.0%-1.7%(n=6).This method is suitable for rapid determination of migration quantity of 4,4′-dihydroxybiphenyl in PPSU feeding-bottles,with the advantages of good accuracy and high sensitivity.
关 键 词:聚亚苯基砜奶瓶 4 4′–联苯二酚 迁移量 超高效液相色谱–串联质谱
分 类 号:TS206.4[轻工技术与工程—食品科学]
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