Determination of Migration of Six Cyclosiloxanes in Silicone Rubber Products for Food Contact by GC－MS/MS

GE Dan-yang; LIU Gui-hua; JIANG Huan; ZHU Yu-xiao; SHANG Gui-qin; LUO Shi-peng; HU Chang-ying

doi:10.19969/j.fxcsxb.22061901

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Determination of Migration of Six Cyclosiloxanes in Silicone Rubber Products for Food Contact by GC－MS/MS

Scientific Papers | 更新时间：2023-01-04

- Determination of Migration of Six Cyclosiloxanes in Silicone Rubber Products for Food Contact by GC－MS/MS
- Journal of Instrumental Analysis Vol. 41, Issue 10, Pages: 1486-1493(2022)
- 作者机构：
  
  1.暨南大学食品科学与工程系，广东广州 510632
  2.常州工业及消费品检验有限公司，江苏常州 213000
  3.南京海关危险货物与包装检测中心，江苏常州 213000
  4.江苏理工学院化学与环境工程学院，江苏常州 213000
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22061901
  CLC：
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葛丹阳,刘桂华,姜欢等.GC－MS/MS法测定食品接触用硅橡胶制品中6种环硅氧烷迁移量[J].分析测试学报,2022,41(10):1486-1493.

GE Dan-yang,LIU Gui-hua,JIANG Huan,et al.Determination of Migration of Six Cyclosiloxanes in Silicone Rubber Products for Food Contact by GC－MS/MS[J].Journal of Instrumental Analysis,2022,41(10):1486-1493.
葛丹阳,刘桂华,姜欢等.GC－MS/MS法测定食品接触用硅橡胶制品中6种环硅氧烷迁移量[J].分析测试学报,2022,41(10):1486-1493. DOI： 10.19969/j.fxcsxb.22061901.

GE Dan-yang,LIU Gui-hua,JIANG Huan,et al.Determination of Migration of Six Cyclosiloxanes in Silicone Rubber Products for Food Contact by GC－MS/MS[J].Journal of Instrumental Analysis,2022,41(10):1486-1493. DOI： 10.19969/j.fxcsxb.22061901.

摘要

基于气相色谱－串联质谱（GC－MS/MS）建立了食品接触用硅橡胶制品中6种环硅氧烷（D4 ~ D9）向50%乙醇、95%乙醇、异辛烷迁移量的检测方法，并应用于38批次实际样品的检测。取10 mL迁移实验得到的50%乙醇浸泡液，使用2 mL正己烷萃取，经过滤后测定，95%乙醇和异辛烷浸泡液直接经过滤后测定。采用HP－5 MS色谱柱分离，多反应监测模式进行分析。结果表明，D4 ~ D9在0.05 ~ 1.00 mg/L或0.20 ~ 5.00 mg/L范围内具有良好的线性关系，相关系数（,r,2,）不低于0.996 0。各目标物的检出限为0.02 ~ 0.07 mg/L，定量下限为0.05 ~ 0.20 mg/L，回收率为90.1% ~ 106%，相对标准偏差不大于13%。使用该方法对市面上的食品接触用硅橡胶制品进行迁移实验，发现D4~D9向50%乙醇存在迁移风险；向95%乙醇和异辛烷迁移的检出率为80%，迁移风险最大。D4 ~ D9在95%乙醇和异辛烷第3次的迁移检出率显著大于第1次，而在50%乙醇中第1次迁移和第3次迁移的检出率无明显差异。

Abstract

A method for the determination of the migration of six cyclosiloxanes（D4－D9） to 50% ethanol，95% ethanol and isooctane in food contact silicone rubber products was developed based on gas chromatography－tandem mass spectrometry（GC－MS/MS），which was applied to the determination of 38 actual samples．2 mL of ,n,-hexane was used to extract D4－D9 from 10 mL of 50% ethanol obtained from the migration test¸ followed by filtration and detection．Meanwhile，the 95% ethanol and isooctane were simply determined after filtration．The analysis was carried out in multiple reaction monitoring mode using an HP－5 MS column for separation．The results showed that there were good linear relationships for D4－D9 in the range of 0.05－1.00 mg/L or 0.20－5.00 mg/L，with correlation coefficients（,r,2,） not less than 0.996 0．The limits of detection and limits of quantitation for each target were in the range of 0.02－0.07 mg/L and 0.05－0.20 mg/L，respectively．The recoveries ranged from 90.1% to 106%，with relative standard deviations not more than 13%．The method was used to determine the migration of D4－D9 in commercially available food contact silicone rubber products，and it was found that there was a migration risk of D4－D9 to 50% ethanol，while the migration risk of D4－D9 to 95% ethanol and isooctane was the highest as the detection rate for D4－D9 was 80%．The detection rate for the third migration of D4－D9 to 95% ethanol and isooctane was significantly greater than that for the first migration，while the detection rates for the first migration and the third migration to 50% ethanol were not significantly different.

关键词

食品接触用硅橡胶制品环硅氧烷食品模拟物迁移气相色谱－串联质谱（GC－MS/MS）

Keywords

food contact silicone rubbercyclosiloxanefood simulantmigrationgas chromatography－tandem mass spectrometry（GC－MS/MS）

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