Citation: LU Li, GONG Xu, FENG Youlong. Determination of 16 phthalate acid ester residues in health wine by gas chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(11): 1286-1292. doi: 10.3724/SP.J.1123.2014.07011 shu

Determination of 16 phthalate acid ester residues in health wine by gas chromatography-triple quadrupole mass spectrometry

1.
Jiangsu Institute for Food and Drug Control, Nanjing 210008, China

Received Date: 4 July 2014
Available Online: 22 August 2014
Fund Project: 中国食品药品检定研究院项目(2012BAK08B02). (2012BAK08B02)

A method for the analysis of sixteen phthalate acid ester (PAE) residues in health wine was developed using gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS). The health wine samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The samples were detected by GC-QQQ-MS with electron impact source (EI) in selected ion monitoring (SIM) mode after extraction. The separation was performed on an HP-5MS capillary column (30 m×0.25 mm×0.25 μm) with temperature programming. The retention time and the fragment ion abundance ratio were used to judge the qualitative results, and the quantitation was performed with standard curve method of the characteristic ion chromatographic peak area-concentration. Eighty-one batches of health wine samples were detected using the method. The results showed that the method had good linear relationships with correlation coefficients (r²) not less than 0.9959. The recoveries of fifteen PAEs ranged from 88.6% to 107.3% except dimethyl phthalate (DMP) which was 52.3%-58.7% in all the three spiked levels with the relative standard deviations of 0.1%-6.8%(RSD, n=6). The limits of detection were between 0.002 mg/L to 0.061 mg/L. The limits of quantification were between 0.005mg/L and 0.202 mg/L. The method is accurate, sensitive, proprietary and suitable for the simultaneous determination of the sixteen phthalate acid esters in health wine.
- gas chromatography-mass spectrometry (GC-MS),
- phthalate acid esters (PAEs),
- plasticizer,
- health wine
1. [1]
  [1] Tang X, Li X J, Xiong W M, et al. Chinese Journal of Analysis Laboratory (唐熙, 李小晶, 熊文明, 等. 分析试验室), 2013, 32(2): 31
2. [2]
  [2] Zhou X J, Zhao Y Q, Li W, et al. China Surfactant Detergent & Cosmetics (周相娟, 赵玉琪, 李伟, 等. 日用化学工业), 2010, 40(2): 148
3. [3]
  [3] Zhang Y, Zhang B B, Zhao Y G. Chinese Journal of Analysis Laboratory (章勇, 张蓓蓓, 赵永刚, 等. 分析试验室), 2014, 33(3): 303
4. [4]
  [4] Phthalate Esters. Baidu Encyclopedia (塑化剂. 百度百科).[2014-08-17]. http://baike.baidu.com/view/1651080.htm?fr=aladdin
5. [5]
  [5] Lü J X, Li J L, Hu Y B, et al (吕建霞, 李景林, 胡永彪, 等).[2014-08-17]. http://www.thermo.com.cn/Resources/201211/2315641328.pdf
6. [6]
  [6] Huang X D, Tao R, Xu Q. Food Science (黄晓东, 陶然, 徐强. 食品科学), 2012, 33(16): 237
7. [7]
  [7] Bai Z, Li H, Xie J, et al. Hubei Agricultural Sciences (白舟, 李颢, 谢佳, 等. 湖北农业科学), 2012, 51(4): 823
8. [8]
  [8] Xiao J, Huang Y, Wang M Y, et al. Chinese Journal of Chromatography (肖佳, 黄颖, 王敏毅, 等. 色谱), 2012, 30(9): 951
9. [9]
  [9] Ma Y L, Chen L X, Ding Y J, et al. Chinese Journal of Chromatography (马燕玲, 陈令新, 丁养军, 等. 色谱), 2013, 31(2): 155
10. [10]
  [10] Yang R J, Wei B W, Gao H, et al. Environmental Chemistry (杨荣静, 卫碧文, 高欢, 等. 环境化学), 2012, 31(6): 925
11. [11]
  [11] Li Y J, Xiong W M, Chen J W, et al. Journal of Instrumental Analysis (李拥军, 熊文明, 陈坚文, 等. 分析测试学报), 2012, 31(3): 278
12. [12]
  [12] Yuan Y T, Liu Z H, Li Y J, et al. Guangzhou Agricultural Sciences (袁永添, 刘正华, 李拥军, 等. 广州农业科学), 2012(6): 100
13. [13]
  [13] Liu P Y, Gao L, Shen J, et al. Chinese Journal of Chromatography (刘芃岩, 高丽, 申杰, 等. 色谱), 2010, 28(5): 517
14. [14]
  [14] Zheng X H, Lin L Y, Fang E H, et al. Chinese Journal of Chromatography (郑向华, 林立毅, 方恩华, 等. 色谱), 2012, 30(1): 27
15. [15]
  [15] Liang J, Zhuang W E, Wei D Q, et al. Chinese Journal of Chromatography (梁婧, 庄婉娥, 魏丹琦, 等. 色谱), 2012, 30(3): 273
16. [16]
  [16] Yang Y Y, Xie Y F, Tian F F, et al. Chinese Journal of Chromatography (杨悠悠, 谢云峰, 田菲菲, 等. 色谱), 2013, 31(7): 674
17. [17]
  [17] Zhang L, Shang C X, Sun C. Chinese Journal of Chromatography (张莉, 尚楚翔, 孙成. 色谱), 2014, 32(6): 653
18. [18]
  [18] GB/T 21911-2008
19. [19]
  [19] GB 9685-2008
20. [20]
  [20] Ministry of Health. Letter of General Office of the Ministry of Health Informed about Maximum Residue of Phthalic Acid Esters in Food and Food Additives (Sanitation Supervision Letter [2011] No. 551) (卫生部. 卫生部办公厅关于通报食品及食品添加剂邻苯二甲酸酯类物质最大残留量的函(卫办监督函[2011] 551号)).(2011-06-13)[2014-08-17]. http://www.foodmate.net/law/shipin/175051.html
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]
  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
4. [4]
  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
5. [5]
  Xiaowu Zhang , Pai Liu , Qishen Huang , Shufeng Pang , Zhiming Gao , Yunhong Zhang . Acid-Base Dissociation Equilibrium in Multiphase System: Effect of Gas. University Chemistry, 2024, 39(4): 387-394. doi: 10.3866/PKU.DXHX202310021
6. [6]
  Jiao CHEN , Yi LI , Yi XIE , Dandan DIAO , Qiang XIAO . Vapor-phase transport of MFI nanosheets for the fabrication of ultrathin b-axis oriented zeolite membranes. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 507-514. doi: 10.11862/CJIC.20230403
7. [7]
  Jingyu Cai , Xiaoyu Miao , Yulai Zhao , Longqiang Xiao . Exploratory Teaching Experiment Design of FeOOH-RGO Aerogel for Photocatalytic Benzene to Phenol. University Chemistry, 2024, 39(4): 169-177. doi: 10.3866/PKU.DXHX202311028
8. [8]
  Tianlong Zhang , Chenjia Song , Wenmin Zhao , Hongsheng Tang , Yan Li , Hua Li . Dream as a Horse, Poem “Liquor” while the Age. University Chemistry, 2024, 39(9): 48-54. doi: 10.12461/PKU.DXHX202403076
9. [9]
  Juntao Yan , Liang Wei . 2D S-Scheme Heterojunction Photocatalyst. Acta Physico-Chimica Sinica, 2024, 40(10): 2312024-. doi: 10.3866/PKU.WHXB202312024
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]
  Zhiquan Zhang , Baker Rhimi , Zheyang Liu , Min Zhou , Guowei Deng , Wei Wei , Liang Mao , Huaming Li , Zhifeng Jiang . Insights into the Development of Copper-based Photocatalysts for CO₂ Conversion. Acta Physico-Chimica Sinica, 2024, 40(12): 2406029-. doi: 10.3866/PKU.WHXB202406029
12. [12]
  Zhi Zhou , Yu-E Lian , Yuqing Li , Hui Gao , Wei Yi . New Insights into the Molecular Mechanism Behind Clinical Tragedies of “Cephalosporin with Alcohol”. University Chemistry, 2025, 40(3): 42-51. doi: 10.12461/PKU.DXHX202403104
13. [13]
  Liuyun Chen , Wenju Wang , Tairong Lu , Xuan Luo , Xinling Xie , Kelin Huang , Shanli Qin , Tongming Su , Zuzeng Qin , Hongbing Ji . 软模板法诱导Cu/Al₂O₃深孔道结构促进等离子催化CO₂加氢制二甲醚. Acta Physico-Chimica Sinica, 2025, 41(6): 100054-. doi: 10.1016/j.actphy.2025.100054
14. [14]
  Bing WEI , Jianfan ZHANG , Zhe CHEN . Research progress in fine tuning of bimetallic nanocatalysts for electrocatalytic carbon dioxide reduction. Chinese Journal of Inorganic Chemistry, 2025, 41(3): 425-439. doi: 10.11862/CJIC.20240201
15. [15]
  Liangzhen Hu , Li Ni , Ziyi Liu , Xiaohui Zhang , Bo Qin , Yan Xiong . A Green Chemistry Experiment on Electrochemical Synthesis of Benzophenone. University Chemistry, 2024, 39(6): 350-356. doi: 10.3866/PKU.DXHX202312001
16. [16]
  Gaoyan Chen , Chaoyue Wang , Juanjuan Gao , Junke Wang , Yingxiao Zong , Kin Shing Chan . Heart to Heart: Exploring Cardiac CT. University Chemistry, 2024, 39(9): 146-150. doi: 10.12461/PKU.DXHX202402011
17. [17]
  Xiaoling LUO , Pintian ZOU , Xiaoyan WANG , Zheng LIU , Xiangfei KONG , Qun TANG , Sheng WANG . Synthesis, crystal structures, and properties of lanthanide metal-organic frameworks based on 2, 5-dibromoterephthalic acid ligand. Chinese Journal of Inorganic Chemistry, 2024, 40(6): 1143-1150. doi: 10.11862/CJIC.20230271
18. [18]
  Lirui Shen , Kun Liu , Ying Yang , Dongwan Li , Wengui Chang . Synthesis and Application of Decanedioic Acid-N-Hydroxysuccinimide Ester: Exploration of Teaching Reform in Comprehensive Applied Chemistry Experiment. University Chemistry, 2024, 39(8): 212-220. doi: 10.3866/PKU.DXHX202312035
19. [19]
  Caixia Lin , Zhaojiang Shi , Yi Yu , Jianfeng Yan , Keyin Ye , Yaofeng Yuan . Ideological and Political Design for the Electrochemical Synthesis of Benzoxathiazine Dioxide Experiment. University Chemistry, 2024, 39(2): 61-66. doi: 10.3866/PKU.DXHX202309005
20. [20]
  Jingming Li , Bowen Ding , Nan Li , Nurgul . Application of Comparative Teaching Method in Experimental Project Design of Instrumental Analysis Course: A Case Study in Chromatography Experiment Teaching. University Chemistry, 2024, 39(8): 263-269. doi: 10.3866/PKU.DXHX202312078

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(353)
HTML views(111)

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