摘要
目的建立食品接触塑料产品中13种荧光增白剂迁移量的测定方法,可用于食品接触塑料产品中相关物质的风险监控。方法采用不同类型食品模拟物进行迁移试验,对水基和酒精类模拟物,用四氢呋喃稀释2倍后测定,对于化学替代溶剂95%(体积分数)乙醇,过膜后测定;对于化学替代溶剂异辛烷,FWA121采用50%甲醇水(含0.4%乙酸),两者按照体积比1∶1萃取后测定,其他化合物用氮气吹至近干后用95%乙醇按体积比1∶1复溶后测定。用高效液相色谱-三重四极杆质谱检测。采用液相色谱XB Phenyl色谱柱(2.1 mm×50 mm,3μm)进行分离,质谱采用电化学喷雾正模式电离,多重反应监测(MRM)模式,外标法定量。结果在优化的条件下,13种荧光增白剂线性关系良好,r^(2)均大于0.999,方法检出限在0.03~6μg/kg之间,加标回收率在85.3%~104%,相对标准偏差(n=6)在0.1%~9.7%。对30批次塑料材质样品进行检测,发现2批次阳性样品。结论方法前处理步骤简单,各化合物色谱分离度好,灵敏度高,专一性好,满足食品接触塑料产品中13种荧光增白剂迁移量的检测需求。
The work aims to establish an HPLC-MS/MS method for determining migration levels of 13 fluorescent whitening agents(FWAs)in food-contact plastic products for risk monitoring of relevant substances.Migration tests were conducted with diverse food simulants.Water-based/alcoholic simulants were analyzed after 2-fold THF dilution,chemical alternative solvent,95%ethanol,was determined after filtration and another chemical alternative solvent,isooctane was treated as follows:FWA121 was extracted with 50%methanol-water(containing 0.4%acetic acid)at a 1∶1 volume ratio before analysis.Other compounds were evaporated to near-dryness under nitrogen,and then reconstituted with 95%ethanol at a 1∶1 volume ratio prior to determination.The analysis was performed through high-performance liquid chromatography-triple quadrupole mass spectrometry.Separation was achieved on an XB Phenyl column(2.1 mm×50 mm,3μm)with electrospray ionization(ESI)in positive mode.Quantification was carried out in multiple reaction monitoring(MRM)mode by an external standard method.Under optimized conditions,all 13 FWAs showed linearity(r^(2)>0.999),detection limits of 0.03-6μg/kg,spiked recoveries of 85.3-104%,and RSDs(n=6)of 0.1%-9.7%.Two positive samples were identified among 30 batches of plastic products.The method features simplified pretreatment,excellent chromatographic resolution,high sensitivity and specificity,fulfilling detection requirements for FWA migration in food-contact plastics.
作者
宋梓锋
刘德云
何国山
陈意光
熊小婷
李慧勇
饶璞
李泽荣
SONG Zifeng;LIU Deyun;HE Guoshan;CHEN Yiguang;XIONG Xiaoting;LI Huiyong;RAO Pu;LI Zerong(Guangzhou Quality Supervision and Testing Institute,Collaborative Innovation Center for NQI-Quality Safety of Guangzhou,Guangzhou 511447,China;Technology Innovation Center of Food Related Product Quality and Safety,State Administration for Market Regulation,Collaborative Innovation Center for NQI-Quality Safety of Guangzhou,Guangzhou 511447,China;National Quality Inspection and Testing Center for Packaging Products(Guangzhou),Collaborative Innovation Center for NQI-Quality Safety of Guangzhou,Guangzhou 511447,China)
出处
《包装工程》
北大核心
2025年第15期144-153,共10页
Packaging Engineering
基金
广州市科技计划项目(2023B04J0407)
广州市院士专家工作站(2024-D012)
广州市市场监督管理局科技计划项目(2024KJ07)。
关键词
荧光增白剂
迁移量
食品接触塑料
高效液相色谱-三重四极杆质谱(HPLC-MS/MS)
fluorescent whitening agents(FWAs)
migration
food-contact plastics
high-performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS)
