目的 建立食品塑料包装材料中4种替代型塑化剂（APs）的气相色谱-质谱测定方法。方法 优化前处理方法和气相色谱质谱条件,提高方法对4种APs的分离度和灵敏度。水基、酸性和酒精类（除95%乙醇）模拟物（V（正己烷）∶V（二氯甲烷）=1∶1）用超声提取,氮吹至近干复溶后测定,异辛烷和95%乙醇模拟物直接旋蒸近干复溶后测定。结果 4种APs在曲线范围内线性关系良好,相关系数大于0.99,检出限为0.02~0.3 mg/kg,定量限为0.05~1.0 mg/kg。空白食品模拟物的加标回收实验结果表明,4种APs的回收率范围为70.4%~117.8%,相对标准偏差（RSD）为0.8%~11.0%。结论 该方法前处理操作简单,灵敏度高,定量定性准确度好,为食品塑料包装材料中APs迁移量的测定和分析提供了参考。
Abstract
The work aims to establish a gas chromatography-mass spectrometry method for the determination of four alternative plasticizers (APs) in plastic food packaging materials. The pretreatment method and gas chromatography conditions were optimized to improve the separation and sensitivity of the four APs. For water-based, acidic and alcohol-based (except 95% ethanol) simulants, ultrasonic extraction was performed with n-hexane:dichloromethane = 1:1 (V/V), and the samples were concentrated by nitrogen blowing to near dryness and then re-dissolved for determination. For isooctane and 95% ethanol simulants, direct rotary evaporation to near dryness and re-dissolution were carried out for determination. The four APs showed good linear relationships within the curve range, with correlation coefficients > 0.99. The detection limits were 0.02-0.3 mg/kg, and the quantification limits were 0.05-1.0 mg/kg. The results of the spiked recovery experiments on blank food simulants indicated that the recovery rates of the four Aps were 70.4%-117.8%, and the relative standard deviations (RSD) were 0.8%-11.0%. The pretreatment operation of the method is simple, with high sensitivity and good accuracy in both quantitative and qualitative analysis, providing a reference for the determination and analysis of APs migration in plastic food packaging materials.
关键词
食品包装材料 /
塑料 /
替代型塑化剂 /
食品模拟物 /
迁移量
Key words
food packaging materials /
plastic /
alternative plasticizers /
food simulants /
migration
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参考文献
[1] 王欢, 杨静, 朱婷. 食品塑料包装导致的食品安全问题及对策分析[J]. 食品安全导刊, 2022(25): 31-33.
WANG H, YANG J, ZHU T.Analysis of Food Safety Problems Caused by Plastic Food Packaging and Countermeasures[J]. China Food Safety Magazine, 2022(25): 31-33.
[2] 李颖. 食品包装材料中邻苯二甲酸酯类塑化剂的检测探究[J]. 食品安全导刊, 2018(3): 65.
LI Y.Detection of Phthalate Plasticizers in Food Packaging Materials[J]. China Food Safety Magazine, 2018(3): 65.
[3] 张依, 范金旭, 李秋雨, 等. 食品中邻苯二甲酸酯类塑化剂的毒性危害及检测方法的研究进展[J]. 食品安全导刊, 2022(26): 190-192.
ZHANG Y, FAN J X, LI Q Y, et al.Research Progress on Toxicity and Detection Methods of Phthalic Acid Esters in Food[J]. China Food Safety Magazine, 2022(26): 190-192.
[4] 杨旭, 郭静. 食品中塑化剂的危害及检测方法研究[J]. 现代食品, 2023, 29(16): 176-178.
YANG X, GUO J.Study on the Harm and Detection Method of Plasticizer in Food[J]. Modern Food, 2023, 29(16): 176-178.
[5] 贾芳, 侯向昶, 谢文缄, 等. 食品包装材料中柠檬酸酯增塑剂的迁移研究[J]. 塑料科技, 2014, 42(10): 108-111.
JIA F, HOU X C, XIE W J, et al.Study on Migration of Citrate Plasticizers in Food Packaging Materials[J]. Plastics Science and Technology, 2014, 42(10): 108-111.
[6] 王杰, 黄佩硕, 谢艳姣, 等. 食品接触材料中非邻苯类塑化剂迁移及潜在危害的研究进展[J]. 食品安全导刊, 2024(21): 127-132.
WANG J, HUANG P S, XIE Y J, et al.Research Progress on the Migration and Potential Hazards of Non-Phthalate Plasticizers in Food Contact Materials[J]. China Food Safety Magazine, 2024(21): 127-132.
[7] 赵海娟, 张文洁, 郑美玲, 等. GC-MS法测定烟用包装材料中非邻苯酯类增塑剂[J]. 包装工程, 2019, 40(9): 59-65.
ZHAO H J, ZHANG W J, ZHENG M L, et al.Determination of Non-Phenyl Ester Plasticizers in Packaging Materials for Cigarettes by GC-MS[J]. Packaging Engineering, 2019, 40(9): 59-65.
[8] 于辉, 向军, 付成忠, 等. 尿液中邻苯二甲酸酯和替代型塑化剂代谢物同步分析方法的建立[J]. 环境化学, 2025, 44(4): 1370-1382.
YU H, XIANG J, FU C Z, et al.Development and Validation of an HPLC-MS/MS Method for the Simultaneous Analysis of Phthalate Ester and Alternative Plasticizer Metabolites in Human Urine[J]. Environmental Chemistry, 2025, 44(4): 1370-1382.
[9] 陈克云, 鞠香, 王艳丽, 等. 基于气相色谱-四极杆-飞行时间质谱高通量筛查芝麻油中54种替代型增塑剂[J]. 色谱, 2023, 41(11): 1010-1020.
CHEN K Y, JU X, WANG Y L, et al.High-Throughput Screening of 54 Alternative Plasticizers in Sesame Oil Using Gas Chromatography-Quadrupole Time-of-Flight Mass Spectrometry[J]. Chinese Journal of Chromatography, 2023, 41(11): 1010-1020.
[10] 杨诗嘉, 马玥玲, 钟慈平, 等. 白酒中42种非邻苯类塑化剂的测定方法研究及含量分析[J]. 食品科技, 2023, 48(8): 270-277.
YANG S J, MA Y L, ZHONG C P, et al.Simultaneously Detection and Content Analysis of 42 Non-Phthalate Esters Plasticizers in Chinese Liquor[J]. Food Science and Technology, 2023, 48(8): 270-277.
[11] 王腾, 余逸飞, 王睿, 等. 食品中邻苯二甲酸酯类塑化剂检测方法研究进展[J]. 生物技术进展, 2023, 13(1): 11-21.
WANG T, YU Y F, WANG R, et al.Research Progress on Detection Methods of Phthalates Plasticizers in Food[J]. Current Biotechnology, 2023, 13(1): 11-21.
[12] 范晓洁, 郭一凡, 张京伟, 等. 32种中国市售食品接触硅橡胶制品中邻苯二甲酸酯类塑化剂的研究[J]. 包装工程, 2023, 44(21): 187-195.
FAN X J, GUO Y F, ZHANG J W, et al.Phthalate Plasticisers in 32 Commercially Available Food Contact Silicone Rubber Products in China[J]. Packaging Engineering, 2023, 44(21): 187-195.
[13] 罗尔伦, 李芸, 王维茜, 等. 气相色谱-质谱联用法测定塑料食品接触材料中3种非邻苯塑化剂含量及其迁移量[J]. 食品科技, 2023, 48(11): 281-286.
LUO E L, LI Y, WANG W Q, et al.Determination of the Content and Migration of 3 Non-Phthalic Plasticizers in Plastic Food Contact Materials by GC-MS[J]. Food Science and Technology, 2023, 48(11): 281-286.
[14] 刘仕途, 曾铭, 陈湘颖, 等. 气相色谱-质谱法测定食品接触材料及制品中4种柠檬酸酯类化合物的迁移量[J]. 分析试验室, 2024, 43(4): 463-468.
LIU S T, ZENG M, CHEN X Y, et al.Determination of Migration of Four Citrate Compounds in Food Contact Materials and Products by Gas Chromatography-Mass Spectrometry Method[J]. Chinese Journal of Analysis Laboratory, 2024, 43(4): 463-468.
[15] 陈满英, 邹旭凤, 刘杏宜, 等. 食品及食品包装材料中塑化剂的检测研究进展[J]. 食品安全质量检测学报, 2017, 8(4): 1305-1311.
CHEN M Y, ZOU X F, LIU X Y, et al.Research Progress on Determination of Plasticizers in Food and Food Packaging Materials[J]. Journal of Food Safety & Quality, 2017, 8(4): 1305-1311.
基金
山东省市场监督管理局科研计划项目（sdscjgj2024sp08）; 山东省政府公派出国留学项目（2024）
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