可降解食品接触材料中三种新型增塑剂的迁移量检测方法及迁移规律研究

Study on the Determination Method and the Migration Rules of Three New Plasticizers in Degradable Food Contact Material

文章建立了6种食品模拟物中磷酸三异辛酯(TOP)、癸二酸二异辛酯(NINS)及1,2-环己烷二甲酸二异辛酯(DEHT)3种新型增塑剂迁移量的检测方法。采用液相色谱串联四极杆-飞行时间高分辨质谱仪(HPLC-QTOF),以甲醇和5 mmol/L甲酸铵为流动相,用T3色谱柱(100 mm×2.1 mm,2.7μm)在梯度洗脱下对目标物进行分离,在信息依赖采集模式(IDA)下进行检测。并研究了阳性可降解食品接触材料样品在不同接触时间、温度及食品模拟物中的迁移规律。结果表明:3种新型增塑剂在0.005~0.250 mg/L质量浓度范围内线性良好(R2>0.99),检出限在0.1~0.9μg/L之间,添加回收率在79.3%~108.0%范围内,相对标准偏差(RSD)在0.84%~9.80%之间。迁移规律结果表明,同等条件下TOP向50%乙醇模拟物中的迁出率最高,NINS向95%乙醇溶液中的迁出率最高;它们的迁移量均随温度升高而增大,随迁移时间的延长先快速上升然后4 d后趋于平衡。研究可为企业和监管机构对可降解食品接触材料的生产和质量控制提供技术支撑。

A method for determination of the migration of three new plasticizers,triisooctyl phosphate(TOP),diisooctyl sebacate(NINS)and diisooctyl 1,2-cyclohexane dicarboxylate(DEHT),in six food simulants was established.A liquid chromatography-tandem quadrupole time-of-flight high resolution mass spectrometer(HPLC-QTOF)was used to separate the target substances by gradient elution on a T3 column(100 mm×2.1 mm,2.7μm)with methanol and 5 mmol/L ammonium formate as the flow,and the detection was carried out under information dependent acquisition mode(IDA).Besides,the migration of positive biodegradable food contact material samples at different contact times,temperatures and food simulants was studied.The results showed that the three new plasticizers had good linearity(R2>0.99)in the concentration range of 0.005~0.250 mg/L,the detection limit was between 0.1~0.9μg/L,and the recovery rate was between 79.3%~108.0%,while the RSD was between 0.84%~9.80%.The migration regularity showed that under the same conditions,in 50%ethanol simulant results the highest migration rate of TOP,and in 95%ethanol simulant results the highest migration rate of NINS.The amount of migration increases with the increase of temperature and migration time,while the migration increases rapidly first and then tends to equilibrium after 4 days. This research could provide technicalsupport for the quality control of biodegradable food contact materials for enterprises and regulatory agencies.