% ~ 96. 4% 3. 0% ~ 9. 8% PAHs
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1 - * PAHs S /N = ~ 2. 0 μg /kg % ~ 96. 4% 3. 0% ~ 9. 8% PAHs - O A X 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 Province * 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 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 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 ECHA REACH 17 PAHs * wangchengyun2009@ 126. com 22 China Pulp & Paper Vol. 33No
2 PAHs 1. 2 a PAHs 0. 2 mg /kg PAHs 100 ml 1 mg /ml μg /ml μg /ml 3. 8 μg /ml μg /ml 2. 5 μg /ml 2. 4 μg /ml 8. 8 μg /ml 8. 7 μg /ml a 4. 8 μg /ml μg /ml b 4. 4 μg /ml k PAHs 4. 0 μg /ml j μg /ml a 8. 8 μg /ml e μg /ml cd μg /ml a h μg /ml PAHs g h i μg /ml PAHs g ml 150 ml min ml 26 PAHs 2. 0 ml ml 18 PAHs 2 /s 5. 0 ml ml μm Agilent 7890A-7000B 1. 4 Agilent SB DTD μl 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% cd 99. 6% 99. 8% a % AccuStandard Inc. Tedia 0. 1 g DB-EUPAH 20 m mm μm min /min /min h /min % 3. 5 min > % k 1. 2 ml /min EI ev 1. 5 ml /min 99. 8% % a 2. 2 ml /min MRM MRM % % b DB
3 1 MRM /min /m z - 1 /ms /V /m z - 1 /ms /V a b k j e a cd a h g h i MS DB-5MS DB-17 MS DB-35MS DB-225 MS HP-Innowax DB-EUPAH DB-EUPAH PAHs DB-EU- PAH 1 PAHs PAHs 1 MRM 1 PAHs MRM ml China Pulp & Paper Vol. 33No
4 min ml min ml min PAHs 3 2 Suplco LC-Florisil Supelclean LC-Si Anpelclean Agilent Bond Elut C18 Ac- cubond AccuBond Florisil Su ml min 2 /mg kg PAHs μg /ml 18 PAHs c 96. 4% PAHs A % 18 PAHs S /N = ~ 2. 0 μg /kg PAHs CNM Bond LC-C plco LC-C18 Agilent Chem Elut Waters Sep-Pak Vac μg /ml 18 PAHs 11 Supelclean LC-Si PAHs a 93. 0% PAHs % Supelclean LC-Si ml μg /ml 18 PAHs 2. 0 ml PAHs 5. 0 ml % PAHs 95% PAHs 5. 0 ml PAHs 90. 0% PAHs 5. 0 ml
5 3 18 PAHs /min /μg L - 1 r /μg kg A = c ~ A = 43. 9c ~ A = c ~ A = c ~ A = c ~ A = c ~ A = c ~ A = 29. 8c ~ a A = c ~ A = c ~ b A = c ~ k A = c ~ j A = 39. 9c ~ e A = c ~ a A = c ~ cd A = c ~ a h A = 77. 5c ~ g h i A = 41. 3c ~ RSD /ng /% /% RSD /ng /% /% RSD /ng /% /% a b k j e a cd a h g h i PAHs 3 PAHs 9 26 China Pulp & Paper Vol. 33No
6 mg /kg 2 - for polycyclic aromatic hydrocarbons in foodstuffs Text with EEA releance J. Official Journal of the European Union L XIE 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 PAHs J YIN 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 Generation J HUANG Chong-xingWANG Zhi-weiWANG Shuang-fei. Residual 420. contaminants in paper food packaging materials J. Packaging Engineering QIU 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 XU Jie-lingWANG BoXU Si-zhaoet al. Analysis of the harmful substances in paper-made food packaging materials J. Modern Food Science and Technology Spectroscopy Laboratory J FENG Jing-lanSHEN Jun-huiZHAI Meng-xiaoet al. Determi-. nation of polycyclic aromatic hydrocarbons in sediment using sonicate J extraction-high performance liquid chromatographyj. Journal of 3DONG Xiao-xue. Hygienic survey of paper food containers and packaging materials J. China Tropical Medicine YUE Qing-qing. Harmful substance in paper packaging materials and its status of migration study J. East China Pulp & Paper Industry J SHEN Song-meiCAO Xian-zhongSONG Yan-huiet al. The nature and the impacts of PAHs J. Guizhou Chemical Industry J Directive 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 Union2005L Commission Regulation EC No /2006 of 19 December 2006 setting maximum levels for certain contaminants in foodstuffs Text with EEA relevance J. Official Journal of the European Union 2006L Commission Regulation EC No. 835 /2011 of 19 August 2011 a- mending Regulation EC No /2006 as regards maximum levels Henan Normal University Natural Science Edition J
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