% ~ 96. 4% 3. 0% ~ 9. 8% PAHs

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- * 518067-18 PAHs - 1 1 40. 0 - S /N = 10 0. 1 ~ 2. 0 μg /kg 0. 998 57. 5% ~ 96. 4% 3. 0% ~ 9. 8% PAHs - O657. 72 A 0254-508X 2014 04-0022-07 Determination of PAHs in the Paper Packaging Materials Using Gas Chromatography-Tandem Mass Spectrometry Combined with Ultrasonic Extraction YANG Zuo-jun WANG Cheng-yun * TONG Chang-fei YUN Peng GU Hao-fei XU Rong The Testing and Technology Center for Industrial ProductsShenzhen Entry-Exit Inspection and Quarantine Bureau ShenzhenGuangdong Province518067 * E-mail wangchengyun2009@ 126. com Abstract An effective method was established for the simultaneous determination of 18 kinds of banned polycyclic aromatic hydrocarbons PAHs in paper packaging materials which were intended to be used to contact with foodstuffs. PAHs in paper packaging materials were ultrasonically extracted with acetone-hexane 1 1 as the extraction solvent at 40. 0 the extractive was purified by silica solid phase extraction column. The extractive was analyzed by gas chromatography-tandem mass spectrometry and the contents of each analytes were calibrated by external standard method. The limits of quantitation LOQ changed from 0. 1 μg /kg to 2. 0 μg /kg at the condition of signal /noise S / N of 10. At the same time the correlation coefficients were all higher than 0. 998. The spiked average recoveries varied from 57. 5% to 96. 4% while the relative standard deviation RSD changed from 3. 0% to 9. 8%. The method was rapidsimpleaccurate and sensitive which could satisfy completely the demand of the analysis of PAHs in paper packaging materials which were intended to contact with foodstuffs. Key words polycyclic aromatic hydrocarbons paper packaging materials gas chromatography-tandem mass spectrometry ultrasonic extraction 6-8 PAHs 18 2008 10 28 ECHA 2012 1-4 10 31 REACH 17 PAHs 5 2013-10-21 31170548 * E-mail wangchengyun2009@ 126. com 22 China Pulp & Paper Vol. 33No. 42014

PAHs 1. 2 a PAHs 0. 2 mg /kg PAHs 100 ml 1 mg /ml 9 10 11 12 13 14 4. 1 μg /ml 92. 5 μg /ml 3. 8 μg /ml 15-16 17-18 5. 0 μg /ml 2. 5 μg /ml 2. 4 μg /ml 8. 8 μg /ml 8. 7 μg /ml a 4. 8 μg /ml 19-24 4. 9 μg /ml b 4. 4 μg /ml k PAHs 4. 0 μg /ml j 10. 4 μg /ml a 8. 8 μg /ml e 10. 6 μg /ml 1 2 3 -cd 23. 5 μg /ml a h 22. 8 μg /ml PAHs g h i 25. 0 μg /ml PAHs 1. 3 1. 0 g 25. 0 ml 150 ml 25-40. 0 35. 0 min 25. 0 ml 26 PAHs 2. 0 ml - 5. 0 ml 18 PAHs 2 /s 5. 0 ml - 3 2 1 2. 0 ml 0. 45 μm 1. 1 - Agilent 7890A-7000B 1. 4 Agilent SB 25-12 DTD 50 1 1. 0 μl 260. 0 280. 0 0. 45 μm Membrane Heidolph 4003 Heidolph 97. 2% j 98. 0% a 99. 0% e 99. 2% 99. 3% 97. 5% 99. 5% 99. 5% g h i 99. 6% 99. 6% 1 2 3-cd 99. 6% 99. 8% a 100. 0% AccuStandard Inc. Tedia 0. 1 g DB-EUPAH 20 m 0. 18 mm 0. 14 μm 50. 0 1. 0 min 25. 0 /min 200. 0 8. 0 /min h 260. 0 5. 0 /min 320. 0 99. 0% 3. 5 min > 99. 999% k 1. 2 ml /min 300. 0 150. 0 EI 70. 0 ev 1. 5 ml /min 99. 8% 100. 0% a 2. 2 ml /min MRM MRM 100. 0% 100. 0% b 1 2 2. 1 - DB-1 2014 33 4 23

1 MRM /min /m z - 1 /ms /V /m z - 1 /ms /V 1 4. 941 128 78 150 25 128 102 150 25 2 6. 627 152 148 50 45 152 149 50 45 3 6. 751 154 152 50 40 154 153 50 20 4 7. 251 166 166 50 5 166 163 50 50 5 8. 658 178 178 60 5 178 176 60 40 6 8. 699 178 178 60 5 178 176 60 35 7 11. 003 202 198 150 50 202 200 150 45 8 11. 661 202 200 150 45 202 198 150 50 9 a 14. 801 228 228 100 5 228 226 100 45 10 15. 036 228 228 100 5 228 226 100 45 11 b 18. 258 252 252 100 15 252 250 100 45 12 k 18. 334 252 252 100 15 252 250 100 45 13 j 18. 441 252 252 100 15 252 251 100 25 14 e 19. 441 252 252 150 15 252 250 150 45 15 a 19. 618 252 252 150 15 252 250 150 45 16 1 2 3 - cd 23. 275 276 276 75 15 276 275 75 25 17 a h 23. 341 278 275 75 50 278 276 75 45 18 g h i 24. 335 276 276 75 15 276 275 75 25 MS DB-5MS DB-17 MS DB-35MS DB-225 MS HP-Innowax DB-EUPAH DB-EUPAH PAHs DB-EU- PAH 1 PAHs 2. 2-1 1 PAHs 1 MRM 1 PAHs MRM 25. 0 ml 1 35. 0 24 China Pulp & Paper Vol. 33No. 42014

1-35. 0 min 2-3 3 20. 0 3 25. 0 30. 0 ml 30. 0 35. 0 2 40. 0 30. 0 35. 0 40. 0 min 1 3 25. 0 ml 40. 0 35. 0 min PAHs 3 2 Suplco LC-Florisil Supelclean LC-Si Anpelclean Agilent Bond Elut C18 Ac- cubond AccuBond Florisil Su- - 2 1-1 1-1 1 25. 0 ml - 1 1 40. 0 35. 0 min 2 /mg kg - 1 1-1 1 161. 1 2 191. 6 3 116. 3 4-1 1 160. 2 5 175. 9 6-2 1 134. 1 7 187. 6 8 165. 4 9-1 1 217. 6 10 152. 5 11 192. 8 2. 3 2. 4 PAHs 10. 0 μg /ml 18 PAHs c 96. 4% PAHs A 3 3 98. 5% 18 PAHs S /N = 10 3 0. 1 ~ 2. 0 μg /kg PAHs CNM Bond LC-C18-1 1 plco LC-C18 Agilent Chem Elut Waters Sep-Pak Vac 10 10. 0 μg /ml 18 PAHs 11 Supelclean LC-Si PAHs a 93. 0% PAHs 2 2-95. 0% Supelclean LC-Si 1 1 5. 0 ml 10. 0 μg /ml 18 PAHs 2. 0 ml PAHs 5. 0 ml - 3 2-3 1-1 1-1 2-1 3-2 1-2 3-2 3 92% PAHs 95% - 2 3 PAHs 5. 0 ml PAHs 90. 0% PAHs 5. 0 ml 2014 33 4 25

3 18 PAHs /min /μg L - 1 r /μg kg - 1 4. 941 A = 1699. 8c - 365. 9 0. 4 ~ 81. 6 0. 99990 0. 2 6. 627 A = 43. 9c - 1265. 7 4. 6 ~ 924. 8 0. 99995 2. 0 6. 751 A = 2864. 5c - 1682. 5 0. 4 ~ 75. 6 0. 99965 0. 2 7. 251 A = 304. 3c - 266. 4 0. 5 ~ 99. 1 0. 99935 0. 2 8. 658 A = 723. 4c - 71. 1 0. 2 ~ 24. 6 0. 99970 0. 1 8. 699 A = 607. 7c - 352. 9 0. 2 ~ 48. 0 0. 99895 0. 1 11. 003 A = 826. 9c - 2874. 8 0. 9 ~ 175. 8 0. 99810 0. 5 11. 661 A = 29. 8c - 47. 0 0. 9 ~ 174. 2 0. 99960 0. 5 a 14. 801 A = 483. 4c + 32. 5 0. 5 ~ 48. 0 0. 99945 0. 2 15. 036 A = 712. 81c - 192. 5 0. 5 ~ 49. 3 0. 99945 0. 2 b 18. 258 A = 347. 0c - 1143. 8 0. 4 ~ 44. 0 0. 99965 0. 2 k 18. 334 A = 164. 0c - 59. 9 0. 4 ~ 80. 0 0. 99990 0. 2 j 18. 441 A = 39. 9c - 144. 1 1. 0 ~ 208. 8 0. 99910 0. 5 e 19. 441 A = 212. 7c - 149. 0 1. 1 ~ 105. 6 0. 99995 0. 5 a 19. 618 A = 275. 1c - 689. 2 0. 9 ~ 176. 0 0. 99915 0. 5 1 2 3-cd 23. 275 A = 135. 3c - 817. 7 2. 4 ~ 470. 4 0. 99955 1. 0 a h 23. 341 A = 77. 5c - 651. 3 2. 3 ~ 456. 0 0. 99910 1. 0 g h i 24. 335 A = 41. 3c - 434. 9 2. 5 ~ 499. 2 0. 99880 1. 0 4 RSD /ng /% /% RSD /ng /% /% RSD /ng /% /% 2. 0 57. 5 9. 5 8. 2 59. 3 8. 2 20. 4 61. 0 6. 5 46. 2 70. 8 8. 0 185. 0 70. 9 8. 0 462. 4 72. 5 7. 7 1. 9 70. 2 9. 8 7. 6 69. 8 7. 2 18. 9 70. 9 6. 3 2. 5 81. 2 7. 8 9. 9 81. 2 5. 9 24. 8 81. 9 5. 3 2. 2 90. 8 8. 2 8. 9 93. 1 6. 2 22. 3 94. 6 3. 5 1. 2 89. 9 9. 3 4. 8 91. 4 7. 0 12. 0 90. 7 4. 7 4. 4 92. 1 6. 2 17. 6 91. 9 5. 2 44. 0 92. 5 3. 0 4. 4 80. 2 6. 5 17. 4 81. 2 6. 2 43. 5 81. 3 5. 5 a 2. 4 92. 3 8. 9 9. 6 92. 8 6. 1 24. 0 93. 4 3. 0 2. 5 94. 9 7. 8 9. 9 94. 4 6. 2 24. 6 92. 2 3. 7 b 2. 2 96. 4 7. 7 8. 8 95. 9 5. 4 22. 0 94. 9 3. 4 k 2. 0 88. 9 8. 4 8. 0 92. 2 5. 8 20. 0 89. 8 4. 4 j 5. 2 90. 2 5. 6 20. 9 89. 2 4. 8 52. 2 90. 2 3. 0 e 5. 3 91. 4 5. 7 21. 1 92. 4 4. 4 52. 8 94. 1 4. 3 a 4. 4 90. 3 6. 8 17. 6 90. 2 5. 6 44. 0 92. 2 5. 0 1 2 3-cd 11. 8 93. 2 5. 7 47. 0 94. 1 5. 0 117. 6 92. 4 4. 6 a h 11. 4 89. 3 5. 7 45. 6 91. 2 4. 5 114. 0 92. 4 4. 0 g h i 12. 5 88. 9 6. 2 49. 9 90. 2 4. 3 124. 8 90. 6 3. 5 2. 5 4 2. 6 20 PAHs 3 PAHs 9 26 China Pulp & Paper Vol. 33No. 42014

3 2-217. 6 mg /kg 2 - for polycyclic aromatic hydrocarbons in foodstuffs Text with EEA releance J. Official Journal of the European Union2011 3 L254 4. 9XIE Yun-feiWANG XuRUAN Wei-donget al. Application of 18 surface-enhanced Raman spectroscopy to detection of polycyclic aro- hydrocarbons J. Spectroscopy and Spectral Analysis2011 PAHs -matic - 1 1 31 92319.. 40. 0 PAHs J. 201131 92319. - 10YIN Xue-fengLI Xiao-dongYOU Xiao-fanget al. Analysis of polycyclic aromatic hydrocarbon in pyrolysis products for combustion PAHs of polyethylene by using Fourier infrared spectroscopyj. Thermal Power Generation200534 420.. J. 200534 1HUANG Chong-xingWANG Zhi-weiWANG Shuang-fei. Residual 420. contaminants in paper food packaging materials J. Packaging Engineering200728 712. 11QIU Ru-binZHANG Ru-pingLIN Shui-donget al. Determination of polycyclic aromatic hydrocarbons in edible oils by constant-. energy synchronous fluorescene spectrometry J. Chinese Journal of J. 200728 712. 2XU Jie-lingWANG BoXU Si-zhaoet al. Analysis of the harmful substances in paper-made food packaging materials J. Modern Food Science and Technology200925 91083. Spectroscopy Laboratory201128 2777.. J. 201128 2777. 12FENG Jing-lanSHEN Jun-huiZHAI Meng-xiaoet al. Determi-. nation of polycyclic aromatic hydrocarbons in sediment using sonicate J. 200925 91083. extraction-high performance liquid chromatographyj. Journal of 3DONG Xiao-xue. Hygienic survey of paper food containers and packaging materials J. China Tropical Medicine20088 4694. 20088 4694. 4YUE Qing-qing. Harmful substance in paper packaging materials and its status of migration study J. East China Pulp & Paper Industry 201142 461.. J. 201142 461. 5SHEN Song-meiCAO Xian-zhongSONG Yan-huiet al. The nature and the impacts of PAHs J. Guizhou Chemical Industry 2008 33 361.. J. 200833 361. 6Directive 2005 /69 /EC of the European Parliament and of the Council of 16 November 2005 amending for the 27th time Council Directive 76 /769 /EEC on the approximation of the laws regulation and administrative provisions of the Member States relating to restrictions on the marketing and use of certain dangerous substances and preparation polycyclic aromatic hydrocarbons in extender oils and tyres J. Official Journal of the European Union2005L323 51. 7Commission Regulation EC No. 1881 /2006 of 19 December 2006 setting maximum levels for certain contaminants in foodstuffs Text with EEA relevance J. Official Journal of the European Union 2006L364 1. 8Commission Regulation EC No. 835 /2011 of 19 August 2011 a- mending Regulation EC No. 1881 /2006 as regards maximum levels Henan Normal University Natural Science Edition 201139 688.. J.. - 2014 33 4 27

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