橄榄油食品模拟物中14种紫外线吸收剂迁移量的测定

史红兰; 翁江赉; 勾新磊; 朱晓艳; 张梅; 童嘉琦

doi:10.19554/j.cnki.1001-3563.2025.15.013

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包装工程（技术栏目） ›› 2025, Vol. 46 ›› Issue (15) : 122-131. DOI: 10.19554/j.cnki.1001-3563.2025.15.013

食品接触材料安全与检测

橄榄油食品模拟物中14种紫外线吸收剂迁移量的测定

史红兰², 翁江赉², 勾新磊³, 朱晓艳¹, 张梅³, 童嘉琦^1*

作者信息 +

Determination of Migration of 14 Ultraviolet Absorbers in Olive Oil Simulant

SHI Honglan², WENG Jianglai², GOU Xinlei³, ZHU Xiaoyan¹, ZHANG Mei³, TONG Jiaqi^1*

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文章历史 +

摘要

目的基于液相色谱-串联质谱仪,测定食品接触材料及制品中14种紫外线吸收剂在橄榄油食品模拟物中的迁移量。方法迁移到橄榄油中的UV-71、UV-326、UV-327、UV-328、UV-329和UV-360等紫外线吸收剂经四氢呋喃稀释,UV-3030、UV-3035、UV-3039、UV-312和UV-3638经乙腈提取后用C18填料固相萃取小柱净化,UV-234、UV-1164和UV-1577经皂化和正己烷提取后用硅胶填料固相萃取小柱净化。选用C18色谱柱分离,以甲醇和含有甲酸及甲酸铵的水溶液为流动相,梯度洗脱。液相色谱-三重四极杆串联质谱检测,外标法定量。结果 14种目标物在0.005~0.1 mg/L线性范围内相关系数达到0.998以上。8种紫外线吸收剂的检出限可达0.001 5 mg/kg,定量限可达0.005 mg/kg;6种紫外线吸收剂可分别达到3 mg/kg和10 mg/kg。在3种浓度的加标水平下,加标回收率为85.9%~108.1%,相对标准偏差不大于9.5%。结论该方法灵敏度高、准确性好,可用于检测橄榄油中14种紫外线吸收剂的迁移量。

Abstract

The work aims to determine the migration of 14 ultraviolet absorbers from food contact materials and articles into olive oil simulant based on liquid chromatography-tandem mass spectrometry (LC-MS/MS). UV-71, UV-326, UV-327, UV-328, UV-329 and UV-360 in the olive oil were diluted with tetrahydrofuran. UV-3030, UV-3035, UV-3039, UV-312 and UV-3638 were extracted with acetonitrile and cleaned up by C18 solid-phase extraction column. UV-234, UV-1164 and UV-1577 were extracted with hexane after saponification, and cleaned up by silica solid-phase extraction column. The separation was carried out on a C18 column selected for gradient elution with methanol and aqueous solution containing formic acid and ammonium formate as mobile phases. The analytes were detected by triple quadrupole tandem mass spectrometry and quantified by external standard method. The correlation coefficients of the 14 target compounds reached more than 0.998 in the linear range of 0.005-0.10 mg/L. The limits of detection for eight UV absorbers were up to 0.001 5 mg/kg, and the limits of quantification were up to 0.005 mg/kg and those for six UV absorbers were up to 3 mg/kg and 10 mg/kg, respectively. The recoveries ranged from 85.9% to 108.1% at 3 different concentrations, with the relative standard deviations no more than 9.5%. The method is sensitive, accurate and can be used for the determination of the migration of 14 ultraviolet absorbers in olive oil.

导出引用

史红兰, 翁江赉, 勾新磊, 朱晓艳, 张梅, 童嘉琦. 橄榄油食品模拟物中14种紫外线吸收剂迁移量的测定[J]. 包装工程（技术栏目）. 2025, 46(15): 122-131 https://doi.org/10.19554/j.cnki.1001-3563.2025.15.013

SHI Honglan, WENG Jianglai, GOU Xinlei, ZHU Xiaoyan, ZHANG Mei, TONG Jiaqi. Determination of Migration of 14 Ultraviolet Absorbers in Olive Oil Simulant[J]. Packaging Engineering. 2025, 46(15): 122-131 https://doi.org/10.19554/j.cnki.1001-3563.2025.15.013

中图分类号： TB324 O652.6

参考文献

[1] 曹瑜, 钟泽辉, 唐聪. 食品接触材料中有害物质迁移的研究进展[J]. 包装工程, 2023, 44(15): 112-121.
CAO Y, ZHONG Z H, TANG C.Research Progress on the Migration of Harmful Substances in Food Contact Materials[J]. Packaging Engineering, 2023, 44(15): 112-121.
[2] ZHANG Q, HUO Y X, YANG Q L, et al.Migration of Chemical Substances from Packaging Materials to Food[J]. Food Chemistry, 2025, 485: 144544.
[3] 寇筱雪, 黄华军, 蔡汶静, 等. 食品接触材料检测技术新进展[J]. 分析测试学报, 2022, 41(3): 409-417.
KOU X X, HUANG H J, CAI W J, et al.New Progress on Detection Techniques for Food Contact Materials[J]. Journal of Instrumental Analysis, 2022, 41(3): 409-417.
[4] FREITAS F, BRINCO J, CABRITA M J, et al.Analysis of Plasticizer Contamination Throughout Olive Oil Production[J]. Molecules, 2024, 29(24): 6013.
[5] 国家卫生和计划生育委员会. 食品安全国家标准食品接触材料及制品用添加剂使用标准: GB 9685— 2016[S]. 北京: 中国标准出版社, 2017.
National Health and Family Planning Commission. National Food Safety Standard-Standard for Uses of Additives in Food Contact Materials or Articles: GB 9685-2016[S]. Beijing: Standards Press of China, 2017.
[6] TRIPATHI S, KUMAR L, DESHMUKH R K, et al.Ultraviolet Blocking Films for Food Packaging Applications[J]. Food and Bioprocess Technology, 2024, 17(6): 1563-1582.
[7] NGUYEN T M, LIM Y W, JANA S, et al.Low-Migration Macromolecular Benzophenones as UV Absorbers for Food Packaging Polymers[J]. ACS Applied Polymer Materials, 2023, 5(9): 6932-6940.
[8] AKINBOYE A J, KIM K, PARK J, et al.Contamination of Ultraviolet Absorbers in Food: Toxicity, Analytical Methods, Occurrence and Risk Assessments[J]. Food Science and Biotechnology, 2024, 33(8): 1805-1824.
[9] TIAN L W, WU Y N, JIA Y K, et al.Understanding of Benzophenone UV Absorber-Induced Damage and Apoptosis in Human Hepatoma Cells[J]. International Journal of Molecular Sciences, 2025, 26(7): 2990.
[10] 国家卫生健康委员会, 国家市场监督管理总局. 食品安全国家标准食品接触材料及制品迁移试验通则: GB 31604.1—2023[S]. 北京: 中国标准出版社, 2023.
National Health Commission, State Administration for Market Regulation. National Food Safety Standard-General Principles for Migration Test of Food Contact Materials or Articles: GB 31604.1-2023[S]. Beijing: Standards Press of China, 2023.
[11] ZHAO M L, CHEN Y, YANG G P, et al.Simultaneous Determination of Benzothiazoles, Benzotriazoles, and Benzotriazole UV Absorbers by Solid-Phase Extraction-Gas Chromatography-Mass Spectrometry[J]. Environmental Science and Pollution Research, 2023, 30(15): 45315-45330.
[12] MARTÍN-POZO L, DEL CARMEN GÓMEZ-REGALADO M, MOSCOSO-RUIZ I, et al. Analytical Methods for the Determination of Endocrine Disrupting Chemicals in Cosmetics and Personal Care Products: A Review[J]. Talanta, 2021, 234: 122642.
[13] 李成发, 陈麒宇, 李英, 等. Py-GC-MS快速测定食品接触材料中抗氧化剂和紫外吸收剂[J]. 塑料科技, 2022, 50(7): 86-91.
LI C F, CHEN Q Y, LI Y, et al.Rapid Determination of Antioxidants and UV Absorbers in Food Contact Materials by Py-GC-MS Method[J]. Plastics Science and Technology, 2022, 50(7): 86-91.
[14] LI C F, LI Y, CHEN Z N, et al.Simultaneous Determination of Antioxidants and Ultraviolet Absorbers by Ultra-Performance Liquid Chromatography in Food Simulants[J]. Food Analytical Methods, 2014, 7(9): 1755-1762.
[15] 肖晓峰, 王建玲, 陈彤, 等. 高效液相色谱-串联质谱法检测塑料类食品接触材料中9种紫外吸收剂的特定总迁移量[J]. 分析测试学报, 2015, 34(9): 1021-1026.
XIAO X F, WANG J L, CHEN T, et al.Simultaneous Determination of Total Specific Migration Limit of 9 Types of Ultraviolet Absorbers in Food Simulants by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Instrumental Analysis, 2015, 34(9): 1021-1026.
[16] 林睿, 赖莺, 林伟靖, 等. 食品接触材料中19种紫外光吸收剂迁移量的测定及迁移规律研究[J]. 分析测试学报, 2015, 34(1): 20-27.
LIN R, LAI Y, LIN W J, et al.Investigation on Determination of 19 UV Absorbers in Food Contact Materials and Their Migration Regularity[J]. Journal of Instrumental Analysis, 2015, 34(1): 20-27.
[17] 李成发, 李英, 陈枝楠, 等. 高效液相色谱法同时测定食品接触材料中抗氧化剂和紫外吸收剂的迁移量[J]. 色谱, 2014, 32(6): 616-622.
LI C F, LI Y, CHEN Z N, et al.Simultaneous Determination of Migration Amounts of Antioxidants and Ultraviolet Absorbents by High Performance Liquid Chromatography in Food Contact Materials[J]. Chinese Journal of Chromatography, 2014, 32(6): 616-622.
[18] 国家卫生和计划生育委员会. 食品安全国家标准食品接触材料及制品迁移试验预处理方法通则: GB 5009.156—2016[S]. 北京: 中国标准出版社, 2017.
National Health and Family Planning Commission. National Food Safety Standard-General Principles for Pretreatment Methods for Migration Test of Food Contact Materials and Products: GB 5009.156—2016[S]. Beijing: Standards Press of China, 2017.
[19] BHOGAL S, GROVER A, MOHIUDDIN I.A Review of the Analysis of Phthalates by Gas Chromatography in Aqueous and Food Matrices[J]. Critical Reviews in Analytical Chemistry, 2024, 54(8): 3428-3452.
[20] WANG H L, LIU X T, TU M L, et al.Current Sample Preparation Methods and Analytical Techniques for the Determination of Synthetic Antioxidants in Edible Oils[J]. Journal of Separation Science, 2022, 45(20): 3874-3886.
[21] 国家卫生健康委员会, 国家市场监督管理总局. 食品安全国家标准食品中维生素D的测定: GB 5009.296—2023[S]. 北京: 中国标准出版社, 2023.
National Health Commission, State Administration for Market Regulation. National Food Safety Standard-Determination of Vitamin D in Foods: GB 5009.296-2023[S]. Beijing: Standards Press of China, 2023.
[22] 陈小华. 固相萃取技术与应用[M]. 2版. 北京: 科学出版社, 2019: 129-146.
CHEN X H.Solid Phase Extraction Technology and Its Application[M]. 2nd ed. Beijing: Science Press, 2019: 129-146.
[23] 肖晓峰, 何军, 刘艇飞, 等. 有机相阴离子交换固相萃取HPLC-UV法快速测定食品接触材料中4种尼泊金酯的特定迁移量[J]. 分析测试学报, 2018, 37(4): 471-476.
XIAO X F, HE J, LIU T F, et al.Rapid Determination of Specific Migration of Four Parabens in Food Simulants by HPLC-UV Detection with Organic Phase Anion Exchange Solid Phase Extraction[J]. Journal of Instrumental Analysis, 2018, 37(4): 471-476.
[24] 唐吉旺, 袁列江, 肖泳, 等. 高效液相色谱-串联质谱法测定食品塑料包装材料中双酚A和壬基酚[J]. 食品与机械, 2023, 39(1): 37-41.
TANG J W, YUAN L J, XIAO Y, et al.Determination of Bisphenol a and Nonylphenol in Food Packaging Material by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Food & Machinery, 2023, 39(1): 37-41.
[25] ALAGARSAMY V, MURUGANANTHAN G, VENKATESHPERUMAL R. Synthesis, Analgesic, Anti-Inflammatory and Antibacterial Activities of Some Novel 2-Methyl-3-Substituted Quinazolin-4-(3H)-Ones[J]. Biological & Pharmaceutical Bulletin, 2003, 26(12): 1711-1714.
[26] AJANI O O, AUDU O Y, GERMANN M W, et al.Expeditious Synthesis and Spectroscopic Characterization of 2-Methyl-3-Substituted-Quinazolin-4(3H)-One Derivatives[J]. Oriental Journal of Chemistry, 2017, 33(2): 562-574.
[27] WANG H, LI X, SHAO M Y, et al.Simultaneous Determination of 9 Environmental Pollutants Including Bisphenol a in Vegetable Oil by Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry[J]. Analytical Methods, 2021, 13(31): 3527-3534.
[28] 国家卫生健康委员会, 国家市场监督管理总局. 食品安全国家标准食品接触材料及制品化学分析方法验证通则: GB 31604.59—2023[S]. 北京: 中国标准出版社, 2023.
National Health Commission, State Administration for Market Regulation. National Food Safety Standard-Food Contact Materials or Articles-General Principles for Validation of Chemical Analysis Methods: GB 31604.59-2023[S]. Beijing: Standards Press of China, 2023.