聚氯乙烯类食品包装材料中三甲基锡向食品模拟物的迁移规律

doi:10.7506/spkx1002-6630-201614035

摘要/Abstract

摘要：

目的：建立聚氯乙烯类包装材料和食品模拟物中三甲基锡的超高效液相色谱-串联质谱（ultra performanceliquid chromatography-tandem mass spectrometry，UPLC-MS/MS）联用测定方法。用该方法研究聚氯乙烯中的三甲基锡向食品模拟物的迁移规律。方法：聚氯乙烯包装材料样品用乙酸乙酯提取。食品模拟物经阳离子固相萃取柱净化富集，洗脱液水浴条件下氮气吹干，残渣用流动相溶解，旋涡混匀，过0.22 μm微孔滤膜，经C18色谱柱完成分离，MS/MS仪上采用多反应监测正离子模式测定三甲基锡，外标法定量。在设定的不同温度条件下，将聚氯乙烯包装材料浸泡于食品模拟物中，于不同的时间点移取浸泡液，经前处理后测定三甲基锡迁移量。结果：三甲基锡在0.1～100.0 μg/L范围内线性关系良好（相关系数r=0.999 8），检出限为0.02 μg/L。在1.0、10.0、50.0 μg/L 3 个添加水平范围内的平均回收率为90.6%～97.3%，相对标准偏差不高于6.9%。测定结果显示，三甲基锡迁移量在水模拟物中为0.19～1.65 μg/L、在体积分数10%乙醇模拟物中为0.19～9.89 μg/L、在3 g/100 mL乙酸模拟物中为0.11～9.96 μg/L、在正己烷模拟物中为0.15～3.54 μg/L。结论：建立的阳离子固相萃取-UPLC-MS/MS联用法测定食品模拟物中三甲基锡的方法快速简单、准确有效，三甲基锡在体积分数10%乙醇溶液和3 g/100 mL乙酸溶液迁移量较高，且随温度升高、时间延长，迁移量增加，一定时间后达到迁移平衡。

关键词: 超高效液相色谱-串联质谱, 三甲基锡, 食品模拟物, 聚氯乙烯, 食品包装材料

Abstract:

Objective: To develop an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
method for determining trimethyltin (TMT) in polyvinyl chloride (PVC) food packaging materials and four food simulants
and to further study the migration pattern of TMT from the packaging materials to the food simulants. Methods: TMT
was extracted from PVC food packaging materials with ethyl acetate. After purification and enrichment with OASIS
MCX C18 cartridge, the eluate containing food simulants was evaporated to dryness with nitrogen in water bath, redissolved
with the mobile phase, vortexed and filtered through a 0.22 μm membrane. The filtrate was detected by
UPLC-MS-MS using positive ion electrospray ionization under multiple reaction monitoring (MRM) mode with a UPLC C18
column as separation column, and quantified by an external standard method. At different temperatures, PVC food packaging
materials were soaked in four food simulants, namely, water, 10% ethanol solution, 3 g/100 mL acetic acid solution and
n-hexane, respectively. At certain time points, the soaking solution was analyzed by UPLC-MS/MS. Results: The standard
calibration curve of TMT was linear in the range of 0.1–100.0 μg/L with a correlation coefficient of 0.999 8. The recoveries
at three spiked levels (1.0, 10.0 and 50.0 μg/L) ranged from 90.6% to 97.3%, with relative standard derivations (RSDs) lower
than 6.9%. TMT was detected in the range of 0.19–1.65, 0.19–9.89, 0.11–9.96 and 0.15–3.54 μg/L in water, 10% ethanol
solution 3 g/100 mL acetic acid solution and n-hexane, respectively. Conclusion: The solid phase extraction-UPLC-MS/
MS method is simple, reliable, accurate,and applicable to determinate TMT in food simulants. TMT in PVC food packaging
materials easily migrates to 10% ethanol solution and 3 g/100 mL acetic acid solution. These results showed that TMT
migration has positive correlations with temperature and time, but the process was balanced after a certain period of time.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), trimethyltin, food simulant, polyvinyl chloride (PVC), food packaging materials

中图分类号:

R155.5

许欣欣，陈慧玲，毛丽莎，胡辛楠. 聚氯乙烯类食品包装材料中三甲基锡向食品模拟物的迁移规律[J]. 食品科学, doi: 10.7506/spkx1002-6630-201614035.

XU Xinxin, CHEN Huiling, MAO Lisha, HU Xinnan. Migration Pattern of Trimethyltin from PVC Food Packaging Materials to Food Simulants[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201614035.

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