Determination of Migration of Spiroglycol in Modified Copolyester Products for Food Contact by Gas Chromatography

WEI Cunqian; SUN Duozhi; WU Yaping

doi:10.19554/j.cnki.1001-3563.2026.17.008

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Packaging Engineering ›› 2026, Vol. 47 ›› Issue (17) : 76-82. DOI: 10.19554/j.cnki.1001-3563.2026.17.008

Special Topic on Sustainable Design and Systemic Transformation of Plastic Packaging for Liquid Foods

Determination of Migration of Spiroglycol in Modified Copolyester Products for Food Contact by Gas Chromatography

WEI Cunqian, SUN Duozhi^*, WU Yaping

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Abstract

The work aims to establish an analytical method using gas chromatography with a flame ionization detector (GC-FID) for determining the migration level of spiroglycol in modified copolyester products for food contact. Food simulants or chemical alternative solvents (e.g., 95% ethanol) were used for migration testing, with optimized sample pretreatment procedures for different simulant types: water and ethanol-containing simulants were directly injected after methanol dilution, acidic simulants required neutralization with sodium hydroxide followed by dichloromethane extraction and fat-based simulants (represented by corn oil) were extracted with a methanol-acetonitrile mixed solution. Gas chromatography involved qualification by retention time and quantification by the external standard method. Spiroglycol exhibited a good linear relationship with peak area within the concentration range of 2.0-10 mg/L. The detection limit (based on a signal-to-noise ratio of 3∶1) was 1.0 mg/kg. Spike recovery tests demonstrated method accuracy, with recoveries ranging from 83.5% to 109.2%, and the relative standard deviations (RSD) for seven parallel determinations were all below 2.5%, indicating good reproducibility. This method addresses the gap in existing standards for detecting spiroglycol migration levels. It fully meets the compliance testing requirements specified in Announcement No.1 of 2025 by the National Health Commission for the migration limit of spiroglycol (≤5 mg/kg) in poly(cyclohexanedimethylene naphthalate) (PCN) materials, providing reliable technical support for industry quality control and government regulation.

Key words

gas chromatography / food contact / modified copolyester / spiroglycol / migration

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WEI Cunqian, SUN Duozhi, WU Yaping. Determination of Migration of Spiroglycol in Modified Copolyester Products for Food Contact by Gas Chromatography[J]. Packaging Engineering. 2026, 47(17): 76-82 https://doi.org/10.19554/j.cnki.1001-3563.2026.17.008

References

[1] 孙中华, 周兴, 陈圣春, 等. 一种改性聚萘二甲酸乙二醇酯及其制备方法和应用: CN202311432467.9[P].2024-03-19.
SUN Z H, ZHOU X, CHEN S C, et al. Modified Polyethylene Naphthalate and Preparation Method and Application Thereof: CN202311432467.9[P].2024-03-19.
[2] 胡晗, 张若愚, 王静刚, 等. 基于螺环乙二醇的共聚酯及其制备方法、制品: CN201911188329.4[P].2020-04-28.
HU H, ZHANG R Y, WANG J G, et al. Spiroglycol-based Copolyester, Preparation Method and Article Thereof: CN201911188329.4[P].2020-04-28.
[3] 凌昊鹏, 凌海鲲, 宋厚春. 一种高透明、高抗冲非晶共聚酯及其制备方法: CN202511559557.3[P].2025-12-16.
LING H P, LING H K, SONG H C. High-transparency and High-impact Amorphous Copolyester and Preparation Method Thereof: CN202511559557.3[P].2025-12-16.
[4] LEE T H, LIU H Z, FORRESTER M J, et al.Next-Generation High-Performance Biobased Naphthalate-Modified PET for Sustainable Food Packaging Applications[J]. Macromolecules, 2022, 55(17): 7785-7797.
[5] 国家卫生健康委员会. 关于4-α-糖基转移酶等28种“三新食品”的公告(2021年第6号)[EB/OL]. (2021-07-15) [2026-03-10]. https://zwfw.nhc.gov.cn/kzx/tzgg/sptjjxpzsp_224/202107/t20210727_2160.html.
National Health Commission of the People's Republic of China. Announcement on 28 New Types of Food-related Products Including 4-α-Glycosyltransferase (No.6, 2021) [EB/OL]. (2021-07-15) [2026-03-10]. https://zwfw.nhc.gov.cn/kzx/tzgg/sptjjxpzsp_224/202107/t20210727_2160.html.
[6] 国家卫生健康委员会. 关于甜叶菊多酚等20种“三新食品”的公告[EB/OL]. (2025-02-10) [2026-03-10]. https://zwfw.nhc.gov.cn/kzx/tzgg/sptjjxpzsp_224/202502/t20250212_2998.html.
National Health Commission of the People's Republic of China. Announcement on 20 New Types of Food-related Products Including Stevia Polyphenols (No.1, 2025)[EB/OL]. (2025-02-10) [2026-03-10]. https://zwfw.nhc.gov.cn/kzx/tzgg/sptjjxpzsp_224/202502/t20250212_2998.html.
[7] 国家卫生健康委员会. 解读《关于甜叶菊多酚等20种“三新食品”的公告》(2025年第1号)[EB/OL]. (2025-02-01) [2026-03-10]. http://www.nhc.gov.cn/sps/c100087/202502/51c9c331c7dc4422b2da408f9886b509.shtml.
National Health Commission of the People's Republic of China. Interpretation of Announcement No.1 of 2025 on 20 New Food-related Substances Including Stevia Polyphenols[EB/OL]. (2025-02-01) [2026-03-10]. http://www.nhc.gov.cn/sps/c100087/202502/51c9c331c7dc4422b2da408f9886b509.shtml.
[8] 张育川. 螺环乙二醇(SPG)[J]. 精细与专用化学品, 2002, 10(7): 23.
ZHANG Y C.Spiroglycol(SPG)[J]. Fine and Specialty Chemicals, 2002, 10(7): 23.
[9] 丁珂. 高纯度大粒径螺二醇的合成、表征及晶体结构[D]. 青岛: 青岛科技大学, 2006.
DING K.Synthesis, Characterization and Crystal Structure of Spiroglycol with High Purity and Large Particle Size[D]. Qingdao: Qingdao University of Science & Technology, 2006.
[10] 李刚. 一锅法合成螺二醇的研究[C]// 河南省化学会2010年学术年会论文摘要集. 安阳师范学院化学化工学院, 2010: 520.
LI G.Study on One-Pot Synthesis of Spiroglycol[C]// Abstracts of the 2010 Annual Academic Conference of Henan Chemical Society. Anyang: School of Chemistry and Chemical Engineering, Anyang Normal University, 2010: 520.
[11] 叶庆国, 梁荣宁. 循环一锅法合成高纯度大粒径螺二醇[J]. 化学工业与工程技术, 2008, 29(1): 4-6.
YE Q G, LIANG R N.Circulating One-Pot Synthesis of Spiroglycol with Large Particle Size and High Purity[J]. Journal of Chemical Industry & Engineering, 2008, 29(1): 4-6.
[12] 徐俊明, 刘福胜, 于世涛. 一锅法合成螺环二醇[J]. 精细石油化工进展, 2006, 7(12): 42-45.
XU J M, LIU F S, YU S T.Synthesis of Spiroglycol by One-Pot Method[J]. Advances in Fine Petrochemicals, 2006, 7(12): 42-45.
[13] 朱坚, 尚小愉, 王滢, 等. 螺环二醇改性PET共聚酯的合成及性能[J]. 化工进展, 2022, 41(11): 6003-6010.
ZHU J, SHANG X Y, WANG Y, et al.Synthesis and Properties of PET Copolyester Modified by Spirocyclodiol[J]. Chemical Industry and Engineering Progress, 2022, 41(11): 6003-6010.
[14] 赵永涛, 董武卿. 螺环二醇的合成研究[J]. 安徽化工, 2012, 38(6): 31-33.
ZHAO Y T, DONG W Q.Research of Synthesis of Spiroglycol[J]. Anhui Chemical Industry, 2012, 38(6): 31-33.
[15] 赵永涛, 董武卿. 螺环二醇的合成[C]// 全国第18届有机和精细化工中间体学术交流会论文集. 大连: 大连化工研究设计院, 2012: 126-129.
ZHAO Y T, DONG W Q.Synthesis of Spiroglycol[C]// Fine Chemicals Professional Committee of Chemical Industry and Engineering Society of China. Proceedings of the 18th National Symposium on Organic and Fine Chemical Intermediates. Dalian: Dalian Chemical Research and Design Institute, 2012: 126-129.
[16] 朱坚. 生物基螺环结构PET共聚酯的合成与性能研究[D]. 杭州: 浙江理工大学, 2022.
ZHU J.Synthesis and Properties of Bio-based Spiro-structured PET Copolyester[D]. Hangzhou: Zhejiang Sci-Tech University, 2022.
[17] 乔海清, 王光英, 翟钰, 等. 食品塑料包装材料中二元醇迁移量的测定[J]. 分析仪器, 2023(2): 52-56.
QIAO H Q, WANG G Y, ZHAI Y, et al.Determination of Migration of Dihydric Alcohol in Food Plastic Packaging Materials[J]. Analytical Instrumentation, 2023(2): 52-56.
[18] 王绮, 林武, 王衍添. 气相色谱法测定食品接触塑料制品中1, 4-丁二醇迁移量的不确定度评定[J]. 化学分析计量, 2025, 34(6): 131-136.
WANG Q, LIN W, WANG Y T.Evaluation of Uncertainty in Measurement of 1, 4-Butanediol Migration Volume in Food-Contact Pastic Products by Gas Chromatography[J]. Chemical Analysis and Meterage, 2025, 34(6): 131-136.
[19] 赵镭, 孙多志, 左莹. 气相色谱法测定食品接触用共聚酯制品中2, 2, 4, 4-四甲基-1, 3-环丁二醇迁移量[J]. 化学分析计量, 2021, 30(9): 26-29.
ZHAO L, SUN D Z, ZUO Y.Determination of Migration of 2, 2, 4, 4-Tetramethyl-1, 3-Cyclobutanediol in Tritan Copolyester Products for Food Contact by Gas Chromatography[J]. Chemical Analysis and Meterage, 2021, 30(9): 26-29.
[20] 上海市食品接触材料协会. T/SAFCM 050-2026食品接触材料及制品螺环乙二醇迁移量的测定[S]. 上海: 上海市食品接触材料协会, 2026.
Shanghai Food Contact Materials Association. T/SAFCM 050-2026 Determination of Migration of Spiroglycol in Food Contact Materials and Articles[S]. Shanghai: Shanghai Food Contact Materials Association, 2026.