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作 者:黄晓钢 刘德云 陈意光 熊小婷 刘利频 李泽荣 凌光耀 饶璞 Huang Xiaogang;Liu Deyun;Chen Yiguang;Xiong Xiaoting;Liu Lipin;Li Zerong;Ling Guangyao;Rao Pu(National Packaging Product Quality Supervision and Inspection Center(Guangzhou),Guangzhou Quality Supervision and Testing Institute,Guangzhou 511447;Guangzhou Labstone Instrument Technology Co.,Ltd.,Guangzhou 510430,China)
机构地区:[1]广州质量监督检测研究院,国家包装产品质量监督检验中心(广州),广东广州511447 [2]广州西唐机电科技有限公司,广东广州510430
出 处:《广东化工》2022年第20期216-218,215,共4页Guangdong Chemical Industry
摘 要:建立了气相色谱-质谱法(GC-MS)测定食品金属罐内涂层中3-丁烯-2-醇的方法。样品采用水、4%乙酸、10%乙醇、20%乙醇、50%乙醇、95%乙醇和橄榄油浸泡。除95%乙醇之外的其他模拟液采用乙腈萃取,95%乙醇直接过滤膜后上机测试。用DB-624(60 m×0.250 mm×1.4μm)色谱柱进行分离,以选择离子模式(SIM)进行检测,内标法定量。结果表明,3-丁烯-2-醇在0.02~0.50 mg/L(或mg/kg)范围内的线性关系良好,相关系数大于0.999。在3个浓度加标水平下,方法回收率为97.3%~106%,相对标准偏差(RSD)为0.7%~4.9%。3-丁烯-2-醇在各类食品模拟液中的检出限(LOD,S/N≥3)可达到0.01 mg/L(或mg/kg),定量限(LOQ,S/N≥10)可达到0.02 mg/L(或mg/kg)。该方法简便、可靠、灵敏、稳定,方法的LOD满足GB 9685-2016的限量要求,可满足食品接触用涂层中3-丁烯-2-醇迁移量的检测需求。A method for the determination of 3-buten-2-ol in food contact coatings by gas chromatography-mass spectrometry(GC-MS) was established in this paper. Samples were soaked in water, 4 % acetic acid, 10 % ethanol, 20 % ethanol, 50 % ethanol, 95 % ethanol and olive oil. The simulated solution of 95 % ethanol was directly filtered through the membrane, other simulated solutions were extracted with acetonitrile. Separation was carried out with a DB-624(60 m×0.250 mm ×1.4 μm) column.Selected ion mode(SIM) was used for detection. Internal standard method was used for quantitative analysis. The results showed that the linear relationship of 3-buten-2-ol was good within 0.02~0.50 mg/L(or mg/kg), and the correlation coefficient was greater than 0.999. The recoveries of the method were 97.3 %~106 %, and the relative standard deviations(RSD) were 0.7 %~4.9 % at three concentration levels. The limit of detection(LOD, S/N≥3) of 3-buten-2-ol in various food simulants can reach 0.01 mg/L(or mg/kg), the limit of quantification(LOQ, S/N≥10) can reach 0.02 mg/L(or mg/kg). The method is simple, reliable,sensitive and stable. The LOD of the method meets the limit requirements in GB 9685-2016. The method is applicable for determination of migration of 3-buten-2-ol in food contact coatings.
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