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,3 μm）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,r2均大于0.999,方法检出限在0.03~6 μg/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。
Abstract
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, 3 μm) 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 (r2>0.999), detection limits of 0.03-6 μg/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.
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）
Key words
fluorescent whitening agents (FWAs) /
migration /
food-contact plastics /
high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS)
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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）
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