. * 290 Journal of Xi an University of Technology 2011 Vol. 27 No. 3 1006-4710 2011 03-0290-05 GC-FID 1 1 1 2 3 1 1. 710048 2. 723000 3. 723000 GC-FID 2- DEHP DINP DIDP BBP DBP 0. 998 1 ~ 0. 999 8 0. 9 ~ 2. 9 μg /ml 5 h 86. 9% ~ 103. 1% RSD 3. 75% DEHP 23. 3% 35. 5% O657. 7 TS206. 4 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 710048 China 2. Hanzhong Institute for Drug Control Hanzhong 723000 China 3. Hanzhong Vocational and Technical College Hanzhong 723000 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 0. 998 1 ~ 0. 999 8 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% ~ 103. 1% 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 * 2011-03-20 51073128 1968- CAD /CAM E-mail xnxieli@ 126. com
GC-FID 291 1 2 1. 1 2. 1 1 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 -50 80% 30 m 0. 32 mm 25 μm 2 PAEs 2-270 250 1 min 10 /min DEHP 290 12 min N 2 2 DINP DIDP ml /min BBP DBP 2 FID 300 60% PVC 320 H 2 47 ml /min 400 PAEs ml /min 3-11 2007 3 30 30 1 3 μl 2007 /19 /EC PAEs 1. 3 DEHP DINP DIDP BBP DBP 1. 021 g 1. 016 g 1. 023 g 1. 025 g 1. 019 g 25 ml 25 ml DEHP DINP DIDP BBP DBP 40. 84 DEHP mg /ml 40. 64 mg /ml 40. 92 mg /ml 41. 00 mg /ml 40% 40. 76 mg /ml 1. 5 mg /kg 12 0 1 2 3 4 5 ml 50 ml PAEs 50 ml 13-19 - 1. 4 0. 5 ± 0. 01 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 0. 998 1
292 2011 27 3 0. 999 8 3 S /N 3 PAEs 4 1 1 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 5. 19 y = 15. 41x + 355. 80 0. 998 1 2. 7 DBP 0. 815 2 89. 6 106. 7 83. 5 93. 3 BBP 7. 45 y = 15. 76x + 320. 40 0. 999 5 2. 9 BBP 0. 820 0 83. 1 90. 5 89. 4 87. 7 DEHP 8. 52 y = 26. 45x - 64. 22 0. 999 8 1. 5 DEHP 0. 816 8 85. 7 90. 6 84. 5 86. 9 DINP 10. 26 y = 23. 99x - 730. 22 0. 998 9 1. 4 DINP 0. 818 4 101. 5 89. 7 92. 4 94. 5 DIDP 10. 94 y = 15. 92x - 363. 39 0. 999 7 0. 9 DIDP 0. 812 8 103. 2 98. 4 107. 8 103. 1 5 h 5 h 5 h Tab. 3 / / / /h mg mg % 2 500. 2 16 560 62. 83 12. 56 3 499. 6 24 937 94. 22 18. 86 4 500. 3 27 290 103. 36 20. 66 5 499. 8 30 129 114. 4 22. 89 6 499. 5 29 461 111. 74 22. 37 7 500. 4 28 876 109. 33 21. 85 PAEs 86. 9% ~ 103. 1% No. 2 - - - - - 2. 4 No. 3 - - - - - No. 1 0. 5 ± 0. 01 g No. 4 - - 35. 5 - - PAEs - Tab. 4 Recovery rate 2. 5 2. 2 No. 1 6 5 h 30 ml No. 1 2 h 2 5 2 RSD 3. 75% 5 2 Tab. 5 Precision Tab. 2 Comparison of extraction rate in different solvents / DEHP /mg /mg /% RSD /% mg / μg /ml 501. 2 17 769 67. 26 13. 42 499. 8 669. 658 6 17 648. 251 8 499. 8 13 174 50. 07 10. 02 520. 2 729. 107 0 19 220. 662 7 500. 5 11 098 42. 16 8. 42 515. 8 716. 848 7 18 896. 428 9 499. 2 5 949 22. 77 4. 56 3. 75 501. 3 677. 187 4 17 847. 386 6 2. 3 No. 1 498. 8 670. 463 3 17 669. 534 4 513. 7 708. 274 6 18 669. 642 1 2 h 3 h 4 h 5 h 6 h 7 h 2. 6 3 3 2 h 5 h 2 1 Y = C 50 W 10 100 1 6 3 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. 1 - - 23. 3 - -
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