摘要
目的建立6种食品模拟物中2,4-二氯苯甲酸的定量检测方法,并对食品接触用硅橡胶制品中2,4-二氯苯甲酸迁移行为进行研究。方法各食品模拟物中2,4-二氯苯甲酸采用Aq-C18色谱柱进行分离,以乙腈和0.025%磷酸水溶液作为流动相,高效液相色谱法(high performance liquid chromatography,HPLC)检测。参照GB31604.1—2015《食品安全国家标准食品接触材料及制品迁移试验通则》和GB 5009.156—2016《食品安全国家标准食品接触材料及制品迁移试验预处理方法通则》,通过短期和长期迁移试验对硅橡胶中2,4-二氯苯甲酸的迁移行为进行研究。结果2,4-二氯苯甲酸在6种食品模拟物的相应浓度范围内均有良好的线性关系(r^(2)>0.999),方法灵敏度(检出限最高为0.20mg/kg)、准确度(回收率在91.8%~113.1%之间)、精密度(相对标准偏差不大于5.2%)均符合标准要求。短期迁移试验结果表明,硅橡胶中2,4-二氯苯甲酸的迁移量随着迁移试验次数的增加而减少;向50%乙醇溶液中的迁移风险最大。长期迁移试验结果表明,2,4-二氯苯甲酸的迁移在试验初始的2d内快速上升,在4 d内达到迁移平衡;温度升高可以使迁移更快达到平衡;平衡时向50%乙醇溶液和橄榄油的迁移量相当。结论该方法操作步骤简便、稳定性好,具有良好的线性范围,检出限低,能够满足食品接触材料中2,4-二氯苯甲酸迁移量的检测需求。食品接触用硅橡胶制品中2,4-二氯苯甲酸迁移量受迁移试验次数、食品模拟物类型、迁移温度和时间的影响,企业和消费者应合理生产和使用相关产品以降低2,4-二氯苯甲酸的迁移风险。
Objective To establish a quantitative method for the determination of 2,4-dichlorobenzoic acid in 6 kinds of food simulants,and study the migration behavior of 2,4-dichlorobenzoic acid in silicone rubber products for food contact.Methods The 2,4-dichlorobenzoic acid in each food simulant was separated by Aq-C18 chromatographic column,acetonitrile and 0.025%phosphoric acid aqueous solution were used as mobile phase,and detected by high performance liquid chromatography(HPLC).The migration behavior of 2,4-dichlorobenzoic acid in silicone rubber was studied through short-term and long-term migration tests with reference to GB 31604.1—2015 National standard for food safety-Food contact materials and products general rules for migration tests and GB 5009.156—2016 National standard for food safety-Food contact materials and products general rules of migration test pretreatment method.Results The 2,4-dichlorobenzoic acid had good linear relationships in the corresponding concentration range of 6 kinds of food simulants(r^(2)>0.999),and the sensitivity(the maximum limit of detection was 0.20 mg/kg),accuracy(recoveries was 91.8%-113.1%)and precision(relative standard deviations was no less than 5.2%)all met the test requirements.The results of the short-term migration assay showed that the migration of 2,4-dichlorobenzoic acid decreased as the repeated times of migration tests increased;and the migration risk to 50%ethanol was the greatest.The results of the long-term migration test showed that the migration of 2,4-dichlorobenzoic acid increased rapidly in the first 2 days,and reached the equilibrium within 4 days;the time for migration to reach equilibrium decreased with the increasing of temperature;the amount migrated to 50%ethanol and olive oil was similar amounts by the time migration reached equilibrium.Conclusion The method has the advantages of simple operation,good stability,good linear range and low detection limit,which can meet the requirements of the detection of 2,4-dichlorobenzoic acid migrated from food contact materials.The migration of 2,4-dichlorobenzoic acid in silicone rubber products for food contact is affected by the number of migration test,the type of food simulant,the temperature and time of migration test,enterprises and consumers should reasonably produce and use relevant products to reduce the migration risk of 2,4-dichlorobenzoic acid.
作者
葛丹阳
刘桂华
姜欢
祝雨筱
罗世鹏
商贵芹
胡长鹰
GE Dan-Yang;LIU Gui-Hua;JIANG Huan;ZHU Yu-Xiao;LUO Shi-Peng;SHANG Gui-Qin;HU Chang-Ying(Department of Food Science and Engineering,Jinan University,Guangzhou 510632,China;Changzhou Industrial and Consumable Products Inspection Company Limited,Changzhou 213000,China;Nanjing Customs Testing Center for Dangerous Goods and Packaging,Changzhou 213000,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第2期435-442,共8页
Journal of Food Safety and Quality
基金
国家重点研发计划项目(2018YFC1603205、2018YFC1603200)
2019年度食品安全国家标准立项计划项目(spaq-2019-013)
广东省重点领域研发计划项目(2019B020212002)。
关键词
硅橡胶
高效液相色谱法
2
4-二氯苯甲酸
迁移
食品接触材料
非有意添加物
silicone rubber
high performance liquid chromatography
2
4-dichlorobenzoic acid
migration
food contact materials
non intentionally added substances
