Citation: LI Rong, BO Yanna, LU Junwen, LIN Qinbao, HUANG Zhiqiang, CHEN Lisi. Determination of 28 phthalate esters in baked foods by gas chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, ;2016, 34(5): 502-511. doi: 10.3724/SP.J.1123.2015.12035 shu

Determination of 28 phthalate esters in baked foods by gas chromatography-triple quadrupole mass spectrometry

LI Rong ¹ ,
BO Yanna ^2,3 ,
LU Junwen ¹ ,
LIN Qinbao ³ ,
HUANG Zhiqiang ^2,, ,
CHEN Lisi ¹

1.
1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China;
2.
2. Hunan Academy of Inspection and Quarantine, Changsha 410004, China;
3.
3. Key Laboratory of Product Packaging and Logistics of Guangdong Higher Education Institutes, Institute of Packaging Engineering, Jinan University, Zhuhai 519070, China

Corresponding author: HUANG Zhiqiang,
Received Date: 23 December 2015

Fund Project: 国家科技支撑计划课题(2012BAK08B01) (2012BAK08B01)广东省省级科技计划项目(2014A040401011) (2014A040401011)国家质检总局科技计划项目(2015IK260) (2015IK260)中山市社会公益重大专项(2015B2295). (2015B2295)

An efficient method using gas chromatography-triple quadrupole mass spectrometry for the determination of 28 phthalate ester residues in bakery foods was established. The samples were extracted with ethyl acetate, and cleaned up with neutral alumina. The separation was performed on a TR-5MS capillary column (30 m×0.25 mm×0.25 μ m) by programmed temperature vaporization (PTV) with splitless mode. Meanwhile the identification and quantification were performed by GC-MS/MS in selected reaction monitoring (SRM) mode and using the internal standard method. The calibration curves of the 27 phthalate esters showed good linearities in the range of 0.05-10 mg/L, except diisononyl ortho-phthalate (DINP) which was in the range of 0.1-20 mg/L, with the correlation coefficients not less 0.9962. The limits of detection (LODs) were 0.1-9.8 μ g/kg and the limits of quantification (LOQs) were 0.4-32.6 μ g/kg. With the proposed method, the spiked recoveries were evaluated in four types of baked foods (bread, biscuits, cakes, stuffing) at low, medium and high concentrations. The results showed that the average recoveries of the 28 PAEs were in the range of 81.0%-117%, and the relative standard deviations (RSDs, n=6) were in the range of 1.3%-13.6%. The method was successfully applied in the investigation of the PAEs distribution in baked foods. The method is suitable for the determination of the 28 PAEs in baked foods with easy operation, high accuracy and precision.
- gas chromatography-tandem mass spectrometry (GC-MS/MS),
- phthalate eaters (PAEs),
- plasticizer,
- baked foods
1. [1]
  [1] Li X M, Wang J, Zhang Q H, et al. Chinese Journal of Chromatography, 2015, 33(11): 114 李晓敏, 王景, 张庆合, 等. 色谱, 2015, 33(11): 1147
2. [2]
  [2] Guo Y. Anal Bioanal Chem, 2012, 404(9): 2539
3. [3]
  [3] Wang X Y, Lin X T, Ke H M, et al. Journal of Environment and Health, 2007, 24(9): 736 王小逸, 林兴桃, 客慧明, 等. 环境与健康杂志, 2007, 24(9): 736
4. [4]
  [4] Liang J, Zhuang W E, Lin F, et al. Chinese Journal of Chromatography, 2014, 32(11): 1242 梁婧, 庄婉娥, 林芳, 等. 色谱, 2014, 32(11): 1242
5. [5]
  [5] Foster P M D. Inter J Andro, 2006, 29(1): 140
6. [6]
  [6] Zhao Y H, Wang X Y, Lin X T, et al. Journal of Environment and Health, 2010, 27(2): 184 赵雅辉, 王小逸, 林兴桃, 等. 环境与健康杂志, 2010, 27(2): 184
7. [7]
  [7] Li Y S, Chen T Y, Huang B L, et al. Food & Machinery, 2012, 28(1): 105 李艳松, 陈铁英, 黄宝临, 等. 食品与机械, 2012, 28(1): 105
8. [8]
  [8] Wang J, Li X M, Zhang Q H, et al. J Sep Sci, 2015, 38: 1700
9. [9]
  [9] Wu H Q, Zhu Z X, Huang X L, et al. Journal of Instrumental Analysis, 2011, 30(10): 1079 吴惠勤, 朱志鑫, 黄晓兰, 等. 分析测试学报, 2011, 30(10): 1079
10. [10]
  [10] Lo Turco V, Di Bella G, Potorti A G, et al. Eur Food Res Technol, 2015, 240: 451
11. [11]
  [11] Zheng X H, Lin L Y, Fang E H, et al. Chinese Journal of Chromatography, 2012, 30(1): 27 郑向华, 林立毅, 方恩华, 等. 色谱, 2012, 30(1): 27
12. [12]
  [12] Luo Y Z, Li Z Y, Liu Z H, et al. Journal of Analytical Science, 2014, 30(6): 890 罗跃中, 李忠英, 刘正华, 等. 分析科学学报, 2014, 30(6): 890
13. [13]
  [13] Li X Y, Yang Y C, Cui X, et al. Anal Lett, 2015, 48(16): 2544
14. [14]
  [14] Li Y Y, Ling Y, Guo H N, et al. Journal of Instrumental Analysis, 2013, 32(4): 408 李玉玉, 凌云, 郭浩楠, 等. 分析测试学报, 2013, 32(4): 408
15. [15]
  [15] Zhang F, Li Z H, Zhang Y, et al. Chinese Journal of Chromatography, 2014, 32(7): 735 张帆, 李忠海, 张莹, 等. 色谱, 2014, 32(7): 735
16. [16]
  [16] Zhu L P, Zhu T, Ma Y P, et al. Chinese Journal of Analytical Chemistry, 2013, 41(7): 1019 朱莉萍, 朱涛, 马运平, 等. 分析化学, 2013, 41(7): 1019
17. [17]
  [17] Lin J L, Chen W X, Zhu H C, et al. J Dairy Sci, 2015, 98(12): 8278
18. [18]
  [18] Sun X, Qi L, Qin Y T, et al. Chinese Journal of Chromatography, 2014, 32(11): 1260 孙欣, 齐莉, 秦延亭, 等. 色谱, 2014, 32(11): 1260
19. [19]
  [19] Lu L, Gong X, Feng Y L. Chinese Journal of Chromatography, 2014, 32(11): 1286 芦丽, 宫旭, 冯有龙. 色谱, 2014, 32(11): 1286
20. [20]
  [20] Zhang L, Shang C X, Sun C. Chinese Journal of Chromatography, 2014, 32(6): 653 张莉, 尚楚翔, 孙成. 色谱, 2014, 32(6): 653
21. [21]
  [21] Cariou R, Larvor F, Monteau F, et al. Food Chem, 2016, 196: 211
22. [22]
  [22] Shi Y M, Xu D M, Zhou Y, et al. Journal of Instrumental Analysis, 2011, 30(12): 1372 施雅梅, 徐敦明, 周昱, 等. 分析测试学报, 2011, 30(12): 1372
23. [23]
  [23] Wang J, Zhang L, Xin D Q, et al. J Food Sci, 2015, 80(11): 2452
24. [24]
  [24] Zhang C Y, Wang H, Zhang X H, et al. Chinese Journal of Chromatography, 2011, 29(12): 1236 张春雨, 王辉, 张晓辉, 等. 色谱, 2011, 29(12): 1236
25. [25]
  [25] Zhang L, Wu Q, Liang J H, et al. Food Science, 2012, 33(20): 184 张磊, 吴青, 梁健华, 等. 食品科学, 2012, 33(20): 184
26. [26]
  [26] Liu H H, Huang X Q, Wang H, et al. Modern Preventive Medicine, 2008, 35(1): 119 刘红河, 黄晓群, 王晖, 等. 现代预防医学, 2008, 35(1): 119
1. [1]
  Wei Shao , Wanqun Zhang , Pingping Zhu , Wanqun Hu , Qiang Zhou , Weiwei Li , Kaiping Yang , Xisheng Wang . Design and Practice of Ideological and Political Cases in the Course of Instrument Analysis Experiment: Taking the GC-MS Experiment as an Example. University Chemistry, 2024, 39(2): 147-154. doi: 10.3866/PKU.DXHX202309048
2. [2]
  Yanhui Zhong , Ran Wang , Zian Lin . Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry. University Chemistry, 2024, 39(11): 296-303. doi: 10.12461/PKU.DXHX202402017
3. [3]
  Shiyi Chen , Jialong Fu , Jianping Qiu , Guoju Chang , Shiyou Hao . Waste medical mask-derived carbon quantum dots enhance the photocatalytic degradation of polyethylene terephthalate (PET) over BiOBr/g-C₃N₄ S-scheme heterojunction. Acta Physico-Chimica Sinica, 2026, 42(1): 100135-0. doi: 10.1016/j.actphy.2025.100135
4. [4]
  Jianding LI , Junyang FENG , Huimin REN , Gang LI . Proton conductive properties of a Hf(Ⅳ)-based metal-organic framework built by 2,5-dibromophenyl-4,6-dicarboxylic acid. Chinese Journal of Inorganic Chemistry, 2025, 41(6): 1094-1100. doi: 10.11862/CJIC.20240464
5. [5]
  Lifang HE , Wenjie TANG , Yaoze LUO , Mingsheng LIANG , Jianxin TANG , Yuxuan WU , Fuxing ZHANG , Xiaoming ZHU . Synthesis, structure, and anticancer activity of two dialkyltin complexes constructed based on 2, 2′-bipyridin-6, 6′-dicarboxylic acid. Chinese Journal of Inorganic Chemistry, 2025, 41(8): 1601-1609. doi: 10.11862/CJIC.20250012
6. [6]
  Ling Liu , Haibin Wang , Genrong Qiang . Curriculum Ideological and Political Design for the Comprehensive Preparation Experiment of Ethyl Benzoate Synthesized from Benzyl Alcohol. University Chemistry, 2024, 39(2): 94-98. doi: 10.3866/PKU.DXHX202304080
7. [7]
  Linghua Chen . 基于双联动“三学”模式的食品专业分析化学教学改革. University Chemistry, 2025, 40(8): 78-91. doi: 10.12461/PKU.DXHX202409095
8. [8]
  Zunxiang Zeng , Yuling Hu , Yufei Hu , Hua Xiao . Analysis of Plant Essential Oils by Supercritical CO₂Extraction with Gas Chromatography-Mass Spectrometry: An Instrumental Analysis Comprehensive Experiment Teaching Reform. University Chemistry, 2024, 39(3): 274-282. doi: 10.3866/PKU.DXHX202309069
9. [9]
  Yanhui Guo , Li Wei , Zhonglin Wen , Chaorong Qi , Huanfeng Jiang . Recent Progress on Conversion of Carbon Dioxide into Carbamates. Acta Physico-Chimica Sinica, 2024, 40(4): 2307004-0. doi: 10.3866/PKU.WHXB202307004
10. [10]
  Xiuyun Wang , Jiashuo Cheng , Yiming Wang , Haoyu Wu , Yan Su , Yuzhuo Gao , Xiaoyu Liu , Mingyu Zhao , Chunyan Wang , Miao Cui , Wenfeng Jiang . Improvement of Sodium Ferric Ethylenediaminetetraacetate (NaFeEDTA) Iron Supplement Preparation Experiment. University Chemistry, 2024, 39(2): 340-346. doi: 10.3866/PKU.DXHX202308067
11. [11]
  Yajin Li , Huimin Liu , Lan Ma , Jiaxiong Liu , Dehua He . Photothermal Synthesis of Glycerol Carbonate via Glycerol Carbonylation with CO₂ over Au/Co₃O₄-ZnO Catalyst. Acta Physico-Chimica Sinica, 2024, 40(9): 2308005-0. doi: 10.3866/PKU.WHXB202308005
12. [12]
  Qianping Li , Hua Guan , Changfeng Wan , Yonghai Song , Jianwen Jiang . 大学有机化学复习课项目式教学——以“液晶化合物4-正戊基苯甲酸-4′-正戊基苯酯的合成路线设计与产品制备”为例. University Chemistry, 2025, 40(8): 100-116. doi: 10.12461/PKU.DXHX202410070
13. [13]
  Xichen YAO , Shuxian WANG , Yun WANG , Cheng WANG , Chuang ZHANG . Oxygen reduction performance of self?supported Fe/N/C three-dimensional aerogel catalyst layers. Chinese Journal of Inorganic Chemistry, 2025, 41(7): 1387-1396. doi: 10.11862/CJIC.20240384
14. [14]
  Zihan Cheng , Kai Jiang , Jun Jiang , Henggang Wang , Hengwei Lin . Achieving thermal-stimulus-responsive dynamic afterglow from carbon dots by singlet-triplet energy gap engineering through covalent fixation. Acta Physico-Chimica Sinica, 2026, 42(2): 100169-0. doi: 10.1016/j.actphy.2025.100169
15. [15]
  Mi Wen , Baoshuo Jia , Yongqi Chai , Tong Wang , Jianbo Liu , Hailong Wu . Improvement of Fluorescence Quantitative Analysis Experiment: Simultaneous Determination of Rhodamine 6G and Rhodamine 123 in Food Using Chemometrics-Assisted Three-Dimensional Fluorescence Method. University Chemistry, 2025, 40(4): 390-398. doi: 10.12461/PKU.DXHX202405147
16. [16]
  Ke Qiu , Fengmei Wang , Mochou Liao , Kerun Zhu , Jiawei Chen , Wei Zhang , Yongyao Xia , Xiaoli Dong , Fei Wang . A Fumed SiO₂-based Composite Hydrogel Polymer Electrolyte for Near-Neutral Zinc-Air Batteries. Acta Physico-Chimica Sinica, 2024, 40(3): 2304036-0. doi: 10.3866/PKU.WHXB202304036
17. [17]
  Shunü Peng , Huamin Li , Zhaobin Chen , Yiru Wang . Simultaneous Application of Multiple Quantitative Analysis Methods in Gas Chromatography for the Determination of Active Ingredients in Traditional Chinese Medicine Preparations. University Chemistry, 2025, 40(10): 243-249. doi: 10.12461/PKU.DXHX202412043
18. [18]
  Renxiao Liang , Zhe Zhong , Zhangling Jin , Lijuan Shi , Yixia Jia . A Palladium/Chiral Phosphoric Acid Relay Catalysis for the One-Pot Three-Step Synthesis of Chiral Tetrahydroquinoline. University Chemistry, 2024, 39(5): 209-217. doi: 10.3866/PKU.DXHX202311024
19. [19]
  Qi Wu , Changhua Wang , Yingying Li , Xintong Zhang . Enhanced photocatalytic synthesis of H₂O₂ by triplet electron transfer at g-C₃N₄@BN van der Waals heterojunction interface. Acta Physico-Chimica Sinica, 2025, 41(9): 100107-0. doi: 10.1016/j.actphy.2025.100107
20. [20]
  Juntao Yan , Liang Wei . 2D S-Scheme Heterojunction Photocatalyst. Acta Physico-Chimica Sinica, 2024, 40(10): 2312024-0. doi: 10.3866/PKU.WHXB202312024

Get Citation

PDF

XML

Metrics

PDF Downloads(1)
Abstract views(413)
HTML views(7)

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142