广州海关技术中心 国家食品接触材料检测重点实验室(广东),广东 广州 510623
董犇,博士,研究方向:食品接触材料中高关注物质检测及安全评估,E-mail:dongb@iqtc-fcm.com
李丹,研究员,研究方向:食品接触材料检测及安全评估,E-mail:lid@iqtcnet.cn
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黎梓城,吴学峰,董犇等.超高效液相色谱-四极杆飞行时间质谱法同时测定食品接触用塑料中50种添加剂的迁移量[J].分析测试学报,2022,41(06):903-909.
LI Zi-cheng,WU Xue-feng,DONG Ben,et al.Determination of Migration of 50 Additives in Food Contact Plastics by Ultra-performance Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(06):903-909.
黎梓城,吴学峰,董犇等.超高效液相色谱-四极杆飞行时间质谱法同时测定食品接触用塑料中50种添加剂的迁移量[J].分析测试学报,2022,41(06):903-909. DOI: 10.19969/j.fxcsxb.22022503.
LI Zi-cheng,WU Xue-feng,DONG Ben,et al.Determination of Migration of 50 Additives in Food Contact Plastics by Ultra-performance Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(06):903-909. DOI: 10.19969/j.fxcsxb.22022503.
为评估食品接触用塑料中添加剂的迁移风险,采用超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF MS)建立了同时测定食品接触用塑料中50种添加剂迁移量的方法。以甲醇和0.01%(体积分数)甲酸-5 mmol/L乙酸铵溶液为流动相进行洗脱,采用目标离子采集(Target MS/MS)模式对目标物的一级离子与二级离子进行监测。结果表明,各物质在0.02~5 mg/L质量浓度范围内线性关系良好,方法检出限为0.01~0.1 mg/kg,加标回收率为92.6%~104%,相对标准偏差(RSD)为0.60%~8.4%。在20款实际样品中有12个样品检出塑料添加剂,其中2个样品检出壬基酚,迁移量为0.033~0.071 mg/kg;6个样品检出抗氧化剂1076和抗氧化剂168,迁移量为0.12~3.3 mg/kg;4个样品检出光引发剂369、光引发剂ITX和光引发剂TPO,迁移量为0.054~4.0 mg/kg。该方法简单、灵敏、准确,适用于食品接触用塑料中50种添加剂迁移量的检测。
In order to assess the risks from the migration of additives in food contact plastics,a method for simultaneous determination of the migration of 50 additives in food contact plastics was established by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-QTOF MS).Methanol and the aqueous mixture of formic acid(0.01%,volume fraction) and 5 mmol/L ammonium acetate were adopted as the mobile phases for elution.The primary and secondary ions of the target were monitored in target ion acquisition(Target MS/MS) mode.The results of each substance showed good linear relationships in the mass concentration range of 0.02-5 mg/L.The detection limits of the method were between 0.01 mg/kg and 0.1 mg/kg,and the spiked recoveries ranged from 92.6% to 104%,with the relative standard deviations(RSDs) of 0.60%-8.4%.A total of 12 plastic samples were detected in 20 actual samples,of which nonylphenol was detected in 2 samples,and the migration amounts were 0.033-0.071 mg/kg.Meanwhile,antioxidant 1076 and antioxidant 168 were found in 6 samples,and the migration amounts ranged between 0.12 mg/kg and 3.3 mg/kg,while photoinitiator 369,photoinitiator ITX and photoinitiator TPO were detected in 4 samples,and the migration amounts were between 0.054 mg/kg and 4.0 mg/kg. The method is sensitive,accurate and simple,and it is suitable for the detection of migration of 50 additives in plastics for food contact materials.
塑料添加剂迁移量食品接触材料超高效液相色谱-四极杆飞行时间质谱
plastic additivesmigrationfood contact materialsultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry
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