WANG Jincui, WANG Xirui. Simultaneous Determination of 22 Phthalate Esters in Milk Powder by GC-MS/MS[J]. Science and Technology of Food Industry, 2022, 43(5): 280−285. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021060214.
Citation: WANG Jincui, WANG Xirui. Simultaneous Determination of 22 Phthalate Esters in Milk Powder by GC-MS/MS[J]. Science and Technology of Food Industry, 2022, 43(5): 280−285. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021060214.

Simultaneous Determination of 22 Phthalate Esters in Milk Powder by GC-MS/MS

More Information
  • Received Date: June 23, 2021
  • Available Online: January 04, 2022
  • A suitable GC-MS/MS method was established for the determination of 22 phthalate esters (PAEs) in milk powder. The milk powder samples were dissolved in water, extracted by acetonitrile, salted out by NaCl, then quantitated by GC-MS/MS in multiple reaction monitoring mode (MRM). As a result, 22 PAEs possessed an excellent linear relation by using matrix-matched standard curve under 5~500 ng/mL, the correlation coefficients were all greater than 0.99, LODwas 1.0~5.0 μg/kg, LOQ was 3.0~15.0 μg/kg. The recoveries were 82.4%~111.4% at three spiked level with relative standard deviation (n=6) of 2.4%~9.5%. This analytical method is simple, quick, sensitive and stable, which can be used for a monitoring and screening analysis of 22 PAEs in milk powder.
  • [1]
    贺小敏, 施敏芳. 梁子湖水体和沉积物中邻苯二甲酸酯分布特征及生态健康[J]. 中国环境监测,2021,37(2):115−127. [HE Xiaomin, SHI Minfang. Distribution characteristics and ecological and health risk assessment of phthalic acid esters in surface water and sediment of Liangzi Lake, China[J]. Environmental Monitoring in China,2021,37(2):115−127.
    [2]
    任梦圆, 贾晓倩, 王盈, 等. 北京市海淀区孕妇膳食频率与头发中邻苯二甲酸酯水平的关联研究[J]. 中国生育健康杂志,2021,32(2):101−105. [REN Mengyuan, JIA Xiaoqian, WANG Ying, et al. Association between food frequency and hair concentration of phthalates among pregnant women in Haidian districe, Beijing[J]. Chinese Journal of Reproductive Health,2021,32(2):101−105.
    [3]
    CRINNION W J. Toxic effects of the easily avoidable phthalates and parabens[J]. Ahem Med Rev,2010,15(3):190−196.
    [4]
    XU C, WANG X, TANG S. Effets of DI-(2-ethylhexyl)phthalate on rat ovarian unction[J]. Journal of Medical Biochemistry,2011,30(4):309−316. doi: 10.2478/v10011-011-0026-2
    [5]
    马林, 马明月. 邻苯二甲酸酯类对生殖毒性的影响及其机制的研究进展[J]. 沈阳医学院学报,2017,19(4):359−363. [MA Lin, MA Mingyue. Research progress of effects of phthalates on reproductive toxicity and its mechanisms[J]. Journal of Shenyang Medical College,2017,19(4):359−363.
    [6]
    HARRIS T R, COLACINO J A, SCHECTER A. Dietary intake is associated with phthalate body burden in a nationally representative sample[J]. Environmental Health Perspectives,2010,118(7):998−1003. doi: 10.1289/ehp.0901712
    [7]
    范萍, 王丽. 气相色谱-三重四级杆质谱法测定肥胖儿童血清中6种邻苯二甲酸酯[J]. 现代预防医学,2017,44(18):3395−3398,3415. [FAN Ping, WANG Li. Determination of 6 phthalic acid esters (PAEs) in serum of obese children by gas chromatography-tandem quadrupole mass spectrometry[J]. Modern Preventive Medicine,2017,44(18):3395−3398,3415.
    [8]
    段晨晖, 房彦军, 梁俊, 等. 邻苯二甲酸酯类增塑剂的体外细胞毒性评价[J]. 生态毒理学报,2019,14(6):23−31. [DUAN C H, FANG Y J, LIANG J, et a1. In vitro cytotoxici W evaluation of phthalate plasticizets[J]. Asian Journal of Ecotoxicology,2019,14(6):23−31.
    [9]
    王笑妍, 薛燕波, 者东梅, 等. 邻苯二甲酸酯类增塑剂概况及法规标准现状[J]. 中国塑料,2019,33(6):95−105. [WANG Xiaoyan, XUE Yanbo, ZHE Dongmei, et a1. Overview of phthalate plasticizers, current regulations and standards[J]. China Plastics,2019,33(6):95−105.
    [10]
    BONINI M, ERRANI E, ZERBINATI G, et al. Extraction and gas chromatographic evaluation of plasticizers content in food packaging films[J]. Microchemical Journal,2008,90(1):31−36. doi: 10.1016/j.microc.2008.03.002
    [11]
    王楠, 胡长鹰, 程娟, 等. 纸质包装材料中邻苯二甲酸酯类物质向Tenax和奶粉的迁移[J]. 食品工业科技,2014,35(9):63−67. [WANG Nan, HU Changying, CHENG Juan, et a1. Migration of phthalate acid esters of paper-made food packaging into Tenax and milk powder[J]. Science and Technology of Food Industry,2014,35(9):63−67.
    [12]
    王守法, 周耀斌, 宁啸骏, 等. 气相色谱-质谱法测定婴幼儿乳粉中16种邻苯二甲酸酯类迁移物[J]. 包装与食品机械,2013,31(6):61−64. [WANG Shoufa, ZHOU Yaobin, NING Xiaojun, et a1. Determination of 16 phthalate esters migrants content in infant milk powder by GC-MS[J]. Packaging and Food Machinery,2013,31(6):61−64. doi: 10.3969/j.issn.1005-1295.2013.06.016
    [13]
    潘静静, 钟怀宁, 李丹, 等. 食品接触材料及制品中邻苯二甲酸酯类塑化剂的风险管控[J]. 中国油脂,2019,44(4):85−90. [PAN Jingjing, ZHONG Huaining, LI Dan, et al. Risk management of phthalate plasticizers in food contact materials and products[J]. China Oils and Fats,2019,44(4):85−90. doi: 10.3969/j.issn.1003-7969.2019.04.020
    [14]
    RUSSO M V, AVINO P, PERUGINI L, et al. Extraction and GC-MS analisis of phthalate esters in food matrices: A review[J]. Rsc Advances,2015,46(5):37023−37043.
    [15]
    YAN H, DU J, LIU B, et al. Simultaneous determination of four phthalate esters in bottled water using ultrasound-assisted dispersive liquid-liquid microextraction followed by GC-FID detection[J]. The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry,2010,135(10):2585−2590.
    [16]
    中华人民共和国国家标准. 食品中邻苯二甲酸酯的测定: GB 5009.271-2016[S]. 北京.

    National Standards of the People's Republic of China. Determination of phthalate esters in food: GB 5009.271-2016[S]. Beijing.
    [17]
    张玉环, 雷亚楠, 鲁皓, 等. 食品中邻苯二甲酸酯类塑化剂的检测技术研究进展[J]. 食品安全质量检测学报,2021,12(1):202−209. [ZHANG Yuhuan, LEI Yanan, LU Hao, et al. Research progress on the detection of phthalic acid ester plasticizers in food[J]. Journal of Food Safety & Quality,2021,12(1):202−209.
    [18]
    梁中秀. 邻苯二甲酸酯检测技术的研究进展[J]. 广东化工,2019,46(2):132−133. [LIANG Zhongxiu. The research progress of phthalate esters detection technology[J]. Guangdong Chemical Industry,2019,46(2):132−133. doi: 10.3969/j.issn.1007-1865.2019.02.055
    [19]
    张微. 邻苯二甲酸酯在食品检测中的研究进展[J]. 现代食品,2019(7):194−196. [ZHANG Wei. Progress of phthalate esters in food detection[J]. Modern Food,2019(7):194−196.
    [20]
    ZAATER M F, TAHBOUB Y R, Al SAYYED A N. Detemination of phthalates in jordanian bottled water using GC-MS and HPLC-UV: Environmental study[J]. Journal of Chromatographiv Science,2014,52(5):447−452. doi: 10.1093/chromsci/bmt059
    [21]
    阮小娇, 盛华栋, 周玮, 等. 固相萃取净化-气相色谱-三重四极杆串联质谱法同时测定奶粉中多氯联苯和邻苯二甲酸酯[J]. 质谱学报,2020,41(3):278−289. [RUAN Xiaojiao, SHENG Huadong, ZHOU Wei, et al. Determination of polychlorinated biphenyls and phthalate esters in milk powders by GC-MS/MS with solid phase extraction[J]. Journal of Chinese Mass Spectrometry Society,2020,41(3):278−289.
    [22]
    KRISHNA-KUMAR S, VIMALKUMAR K, POOPAL R K, et al. GC-MS determination of phthalate esters in human urine: A potential biomarker for phthalate bio-monitoring[J]. Journal of Chromatography, B Analytical Technologies in the Biomedical & Life Sciences,2018:107915−24.
    [23]
    张国民, 温素素. 气相色谱-质谱法测定食品中17种邻苯二甲酸酯类塑化剂的含量[J]. 理化检验 化学分册,2020,56:46−54. [ZHANG Guomin, WEN Susu. Determination of 17 phthalates plasticizers in food by gas chromatography-mass spectrometry[J]. Physical Testing and Chemical Analysis Part B: Chemical Analysis,2020,56:46−54.
    [24]
    REN R, JIN Q, HE H L, et al. Determination of 17 phthalate esters in infant milk powder and dairy products by GC-MS with 16 internal standards[J]. Chromatographia,2016,79(13/14):903−910.
    [25]
    黄海智, 叶兴乾, 盛华栋, 等. 食品中邻苯二甲酸酯的前处理及检测技术研究进展[J]. 分析试验室,2019,38(1):119−124. [HUANG Haizhi, YE Xingqian, SHENG Huadong, et al. Advances on the development of pretreatment and detection technigues for analysis of phthalate esters in food[J]. Chinese Journal of Analysis Laboratory,2019,38(1):119−124.
    [26]
    LENG G, CHEN W J, ZHANG M F, et al. Determination of phthalate esters in liquor samples by vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction followed by GC-MS[J]. Journal of Separation Science,2014,37(6):684−690. doi: 10.1002/jssc.201301033
    [27]
    王敬, 艾连峰, 马育松, 等. 气相色谱-三重四极杆质谱法测定液体乳及乳粉中的17种邻苯二甲酸酯类增塑剂[J]. 食品安全质量检测学报,2019,10(4):1009−1017. [WANG Jing, AI Lianfeng, MA Yusong, et al. Determination of 17 kinds of phthalic acid esters in milk and milk power by gas chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality,2019,10(4):1009−1017. doi: 10.3969/j.issn.2095-0381.2019.04.033
    [28]
    许文娟, 王振刚, 丁葵英, 等. QuEChERS/液相色谱-串联质谱法测定5种蔬菜中17种氨基甲酸酯类农药的基质效应研究[J]. 分析测试学报,2017,36(1):54−60. [XU Wenjuan, WANG Zhengang, DING Kuiying, et al. Detection of matrix effects of 17 carbamate pesticides in 5 vegetables by QuEChERS/LC-MS/MS method[J]. Journal of Instrumental Analysis,2017,36(1):54−60.
    [29]
    国家质量监督检验检疫总局. GB/T 27404-2008实验室质量控制规范 食品理化检测[S]. 北京:中国标准出版社,2008.

    General Administration of Quality Supervision, Inspection and Quarantine.GB/T 27404-2008 Criterion on quality control of laboratories-Chemical testing of food[S]. Beijing: China Standards Press, 2008.
  • Related Articles

    [1]MA Xiangjie, ZHAO Jiansheng, HUANG Qirui, WANG Qifan, CHEN Jie, ZENG Maomao. Effects of Thermal Reaction Conditions on Dicarbonyl Compounds and Flavor Substances in Glucose-Alanine Sweet-flavored Maillard Reaction Model System[J]. Science and Technology of Food Industry, 2024, 45(16): 114-120. DOI: 10.13386/j.issn1002-0306.2023100219
    [2]SUN Bingyu, ZHENG Xinru, LIU Linlin, LÜ Mingshou, HUANG Yuyang, ZHU Ying, QU Min, ZHU Xiuqing, SHI Yanguo. Research Progress on the Influence of Coagulants and Processing Conditions on the Formation and Quality of Tofu Gel[J]. Science and Technology of Food Industry, 2024, 45(3): 388-396. DOI: 10.13386/j.issn1002-0306.2023030178
    [3]CHEN Yang, LIAO Ziwei, TAO Juanjuan, JIANG Dan, SUN Daihua, CHEN Zhiyuan. Optimization of Ultrasonic Combined with Enzymatic Extraction Process of Total Alkaloids from Artemisia argyi Leaves and Its Antibacterial Activity[J]. Science and Technology of Food Industry, 2022, 43(12): 197-205. DOI: 10.13386/j.issn1002-0306.2021090016
    [4]GONG Pin, HAN Yewen, ZHAI Pengtao, CHEN Xuefeng, ZHAI Wenjun, ZHENG Benzhong, CHEN Fuxin. Active Components, Pharmacological Action and Application in Food Processing of Eucommia ulmoides Leaves[J]. Science and Technology of Food Industry, 2022, 43(10): 395-404. DOI: 10.13386/j.issn1002-0306.2021050082
    [5]SUN Xiyun, WANG Jingwen, TIAN Sihui, XU Zihan, LI Bin. Research Progress of the Effects of Food Matrix and Processing on Bioaccessibility of Polyphenols[J]. Science and Technology of Food Industry, 2021, 42(21): 400-407. DOI: 10.13386/j.issn1002-0306.2020080268
    [6]HUANG Zhiyu, SHEN Xueyu, CHEN Xunlin, GUO Zhuozhao, HUANG Wei. Isolation and Identification of Spoilage Fungi in the Fermentation Broth of Sanhua Plum, Evaluation of the Potency of Related Antibacterial Agents and Optimization of Fermentation Technology[J]. Science and Technology of Food Industry, 2021, 42(14): 113-120. DOI: 10.13386/j.issn1002-0306.2020110278
    [7]ZENG Yao-ying, SHAO Xiao-lu, CHENG Shu-jun, YU Qian. Combined Antibacterial Effect and Mechanism of Liangguoan and Garlic Oil[J]. Science and Technology of Food Industry, 2020, 41(10): 112-117. DOI: 10.13386/j.issn1002-0306.2020.10.019
    [8]LIU Ye, SU Hang, SONG Huan- lu, SU Ke- ran. Optimization of natto processing conditions based on nattokinase activity[J]. Science and Technology of Food Industry, 2016, (07): 170-175. DOI: 10.13386/j.issn1002-0306.2016.07.025
    [9]DONG Yi-wei, GUO Quan-you, LI Bao-guo, JIANG Chao-jun, GU Tian-sheng. Identification of dominated spoilage organisms and quality changes in lightly salted Mylopharyngodon piceus during processing and storage[J]. Science and Technology of Food Industry, 2015, (23): 306-310. DOI: 10.13386/j.issn1002-0306.2015.23.055
    [10]CHEN Xue-hong, QIN Wei-dong, MA Li-hua, DAI Xiao-juan. Effect of processing conditions on quality of fruit and vegetable juices[J]. Science and Technology of Food Industry, 2014, (01): 355-362. DOI: 10.13386/j.issn1002-0306.2014.01.046
  • Cited by

    Periodical cited type(18)

    1. 张帅奇,徐冉冉,王宝刚,周家华,王云香,梁丽雅. 四氢嘧啶对甜樱桃果实采后贮藏品质的影响. 保鲜与加工. 2025(02): 62-69 .
    2. 王天菊,沈庆庆,况世雪. 外源褪黑素对“红地球”葡萄采后贮藏品质的影响. 中国南方果树. 2024(01): 207-215 .
    3. 赵士粤,刘露露,崔克强,任瑞,何美美,杨明霞. 外源褪黑素对采后果实品质影响的研究进展. 中国果树. 2024(04): 17-22 .
    4. 肖鑫鑫,李佩艳,苏娇,马金金,罗登林. 褪黑素处理对金针菇贮藏品质和褐变的影响. 食品与发酵工业. 2024(07): 242-249 .
    5. 陈强,黄馨慧,张峥,张冲,柳叶飞. 褪黑素对薄皮甜瓜采后软化和乙烯合成的影响. 生物技术通报. 2024(04): 139-147 .
    6. 林育钊,冯梦棐,陈洪彬,蒋璇靓,郑金水,吴锦雯. 氧化白藜芦醇处理对黄皮果实贮藏特性和采后品质的影响. 热带作物学报. 2024(04): 804-812 .
    7. 张家铭,石浩,苏慧,钱鑫,赵野,马妍,周文化. 褪黑素及2, 4-表油菜素内酯复合处理对阳光玫瑰葡萄贮藏品质的影响. 食品与发酵工业. 2024(10): 141-148 .
    8. 申雪,陈娇,吕伟伟,司成伟,王纪忠. 外源褪黑素对常温货架期不同品种草莓果实贮藏品质的影响. 淮阴工学院学报. 2024(02): 40-49 .
    9. 董小盼,汤静,丁娇,金鹏,郑永华. 褪黑素处理对桃果实采后软腐病的影响及其机理. 食品科学. 2024(11): 243-249 .
    10. 宁娜,王懿,王晓茜,陈华红,南立军. 褪黑素结合PE包装对葡萄果梗褐变调控的研究. 北方园艺. 2024(17): 93-103 .
    11. 刘祯,陈贤柔,缪承杜,蓝碧锋,范智蕾,莫晓晴,王春越,刘袆帆,肖更生,王琴,刘东杰,马路凯. 褪黑素在果蔬采后品质劣变中的调控作用. 食品安全质量检测学报. 2023(02): 146-153 .
    12. 张海燕,康三江,曾朝珍,袁晶. 碱性钙对‘秦冠’苹果块贮藏品质及生理特性的影响. 食品安全质量检测学报. 2023(04): 41-49 .
    13. 张皓波,吴喜庆,杨蕊,林奇,包媛媛. 褪黑素结合气调包装处理对黄牛肝菌保鲜效果影响. 食用菌学报. 2023(03): 68-80 .
    14. 田甜,赵雅琦,王清,秦占军,潘媛,时文林,左进华,袁树枝,岳晓珍,封碧红. 不同贮藏期对鲜切菜山药和铁棍山药货架期品质的影响. 食品工业科技. 2023(18): 387-397 . 本站查看
    15. 赵朋飞,骆世超,许佩轩,孙晓峰,徐伟敏,马辉,许建锋,张海霞. 褪黑素处理对采后梨果实品质及相关生理指标的影响. 华北农学报. 2023(S1): 211-218 .
    16. 郜栀萍,田云芳,姜淑宁,尚泓奎,王银宵,杨秋梅. 外源褪黑素在果蔬保鲜中的作用研究进展. 现代农业科技. 2022(14): 171-174 .
    17. 吴敏,杜鹃,王曼,张健,阿塔吾拉·铁木尔,吴斌,吴忠红. 一氧化氮对无核白葡萄果梗贮藏品质和微观结构的影响. 食品工业科技. 2022(21): 350-359 . 本站查看
    18. 张妮,陶秋运,普莹莹,曹森,王瑞,吉宁. 不同地区玛瑙红樱桃品质差异分析. 食品工业科技. 2022(23): 95-102 . 本站查看

    Other cited types(14)

Catalog

    Article Metrics

    Article views (200) PDF downloads (24) Cited by(32)

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return