Determination of Five Phthalic Acid Esters Plasticizers in Food-Grade Lid Gasket by GC-FID

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1 . * 290 Journal of Xi an University of Technology 2011 Vol. 27 No GC-FID GC-FID 2- DEHP DINP DIDP BBP DBP ~ ~ 2. 9 μg /ml 5 h 86. 9% ~ % RSD 3. 75% DEHP 23. 3% 35. 5% O TS A Determination of Five Phthalic Acid Esters Plasticizers in Food-Grade Lid Gasket by GC-FID XIE Li 1 YU Jiang 1 LI Xia 1 ZHANG Guozhu 2 WANG Shibao 3 REN Penggang 1 1. Faculty of Printing and Packaging Engineering Xi an University of Technology Xi an China 2. Hanzhong Institute for Drug Control Hanzhong China 3. Hanzhong Vocational and Technical College Hanzhong China Abstract Gas chromatography-flame ionization detection GC-FID analysis method is used to determine contents of five phthalic acid esters PAEs plasticizers including di-2-ethylhexyl phthalate DE- HP di-isononyl phthalate DINP di-isodecyl phthalate DIDP butylbenzyl phthalate BBP and din-butyl phthalate DBP in four kinds of food packaging lid gaskets. The linear relation of this method is much better and the correlated coefficients of the compounds of five kinds are ~ and their detection limits are in the range of 0. 9 ~ 2. 9 μg /ml. The best extracting conditions for determining 5 kinds of phthalic acid esters are selected via experiments methylbenzene is adopted as the extracting solvent and the extraction time is 5 hours. The recovery rate of the five compounds is 86. 9% ~ % and the relative standard deviation RSD is 3. 75%. The results indicate in the four kinds of food packaging lid gasket the content of DEHP in alcoholic drinks packaging lid gasket and can packaging lid gasket is 23. 3% and 35. 5% respectively the five kinds of plasticizer are not detected in the rest of other two lid gaskets. Key words food-grade lid gasket gas chromatography-flame ionization detection GC-FID phthalic acid esters PAEs plasticizer * CAD /CAM xnxieli@ 126. com

2 GC-FID GC-2010 FID 1 BT25S 5 μl Human PVC PE No. 2 40% ~ 60% No. 3 No. 4 1 phthalic acid 1. 2 esters PAEs 1 Rtx % 30 m mm 25 μm 2 PAEs min 10 /min DEHP min N 2 2 DINP DIDP ml /min BBP DBP 2 FID % PVC 320 H 2 47 ml /min 400 PAEs ml /min μl 2007 /19 /EC PAEs 1. 3 DEHP DINP DIDP BBP DBP g g g g g 25 ml 25 ml DEHP DINP DIDP BBP DBP DEHP mg /ml mg /ml mg /ml mg /ml 40% mg /ml 1. 5 mg /kg ml 50 ml PAEs 50 ml ± g 3 mm 3 GC-FID mm PAEs 30 ml 50 ml GC-FID 2 2- DE- HP DINP DIDP BBP DBP 1 Fig. 1 Chromatogram of standards solution 10% 3 No. 1 r

3 S /N 3 PAEs PAEs S /N 3 Tab. 1 Regression equations relative coefficients r 4 and limits of detection S /N 3 of the five PAEs / / PAEs /% /min r μg /ml mg /ml /% DBP y = x DBP BBP y = x BBP DEHP y = x DEHP DINP y = x DINP DIDP y = x DIDP h 5 h 5 h Tab. 3 / / / /h mg mg % PAEs 86. 9% ~ % No No No ± g No PAEs - Tab. 4 Recovery rate No h 30 ml No. 1 2 h RSD 3. 75% 5 2 Tab. 5 Precision Tab. 2 Comparison of extraction rate in different solvents / DEHP /mg /mg /% RSD /% mg / μg /ml No h 3 h 4 h 5 h 6 h 7 h h 5 h 2 1 Y = C 50 W Y % C Comparison of extraction rate at different time μg /ml W g 6 Tab. 6 6 PAEs Contents of five PAEs in samples PAEs /% DBP BBP DEHP DINP DIDP No

4 GC-FID Fig. 2 Chromatograms of four samples 3 2. M r 3. J ~ ~ 2. 9 μg /ml Wang Yubang Wang Xinru. Toxicity of phthalic acid esters PAEs on reproductive endocrine J. Journal of En- 2 PAEs 86. 9% ~ % RSD 3. 75% vironmental & Occupational Medicine DEHP J % 35. 5% Wang Wei Wei Guanghui Deng Yongji et al. Histopathological changes of the cryptorchid testis and epididy- mis of mice exposed to DEHP J. National Journal of Andrology PAEs 5. PAEs Leydig J Song Xiaofeng Wei Guanghui Deng Yongji et al. Cytotoxicity of Di 2-ethylhexyl phthalate on leydig cells pri- 1. mary cultured from the fetal mice J. Chinese Journal of J Andrology Liao Yuwen Cao Guorong Xu Wencai et al. Discussion 6. PAEs on the food safety issue of the plasticizer in lid gasket J. J Packaging Engineering Li Mingyuan Hu Yinchuan. Current progress of the hazard

5 of PAEs migration in plastic package of food J. Journal of Food Science and Biotechnology Maurus Biedermann Katell Fiselier Koni Grob. Testing J migration from the PVC gaskets in metal closures into oily Li Liping Huang Lingyan Zhang Yan et al. Brain tissue damage male rat offspring induced by exposure to phthalate foods J. Food Science & Technology ethylhexyl ester during pregnancy and lactation J. Journal of Environment and Health J. Gu Jun Yu Wenjing. The research about HPLC analysis Wang Jing Cai Fengyun Zeng Qiang et al. The oxidative damage of lung cells induced by butylbenzyl phthalate in vitro J. Journal of Medical Research J Wang Li Yuan Jing Zhang Rong. Research advance in environmental exposure and health impact of Di 2-ethylhexyl phthalate J. Journal of Environment and Health Wang Meng Cai Fengyun Yang Xu. Suppression effect of Di-n-butyl phthalate in vitro on superoxide dismutase of various organs of mice J. Journal of Medical Research J He Peng. Simultaneous determination of 18 phthalate acid Wang Lixin Yang Xu. Research advance on toxicity and esters plasticizers in rubber and plastic materials by GC- health effect of phthalate review and perspective J. Journal of Environment and Health GB S. Wang Donghui Li Yirui Tian Yuping et al. Detection Anja Fankhauser-Noti Koni Grob. Migration of plasticizers from PVC gaskets of lids for glass jars into oily foods Amount of gasket material in food contact proportion of plasticizer migrating into food and compliance testing by simulation J. Food Science & Technology HPLC J way of biethylhexyl phthalate in food wrapper J. Journal of Suzhou University Natural Science PVC J Wang Xiangyang Shi Qinghong. Study on the migration of Di 2-ethylhexyl phthalate in PVC film to food J. Food Science and Technology J Liu Jun Zhu Ran Tian Yanhe et al. Determination of SOD J. residual fourteen kinds of phthalates and five kinds of adipates in food packaging materials by gas chromatographymass spectrometry J. Journal of Instrumental Analysis J MS J. China Plastics Industry J of eight phthalic acid esters in food packaging plastic J. Amino Acids & Biotic Resources

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