PVC医疗器械中非邻苯二甲酸酯类增塑剂DINCH的含量和迁移量的检测方法研究

目的：采用气相色谱质谱联用法测定聚氯乙烯（PVC）医疗器械中非邻苯二甲酸酯类增塑剂环己烷1，2-二甲酸二异壬基酯（diisononyl cyclohexane-1，2-dicarboxylate，DINCH）的含量和迁移量。 方法：分别用乙醚加热回流法提取PVC医疗器械中DINCH，以脂肪乳为浸提液评价DINCH的迁移量，并建立GCMS方法检测测试液中DINCH的含量。 结果：该方法线性范围为50~800 μg·mL^-1，r=0.9999，在提取试验和迁移试验中，DINCH的回收率为81.7%~101.5%，RSD均小于5.0%。 结论：本文建立的方法可用于PVC医疗器械中DINCH含量和迁移量的评价。

Objective: Determination of the content and migration of non-phthalate plasticizers diisononyl cyclohexane-1,2-dicarboxylate( DINCH) in PVC medical devices by GC-MS. Methods: The content of DINCH was detected by ether reflux and the migration of DINCH was evaluated using fat emulsion as extracts.GCMS analysis method was developed to detect DINCH.The DB-5MS capillary column (30 m×0.25 mm×0.25 μm) was adopted with the vaporization temperature of 290℃.Heating program: the initial temperature was 200℃, kept for 2 min, and then increased at a rate of 10℃·min^-1 to 300℃, and finally the temperature was maintained for 2 min.The electron impact(EI) ion source was selected and the temperature of ion source was 200℃. Results: The results showed that the linear range was 50-800 μg·mL^-1, r=0.9999.The recovery rate of DINCH was between 81.7% and 101.5%, and RSD was less than 5.0% in both the extraction and migration experiments. Conclusion: The method established could be used for the evaluation of the content and migration of DINCH in PVC medical devices.

[1] JIN Qiu-mei(靳秋梅), SUN Zeng-rong(孙增荣). Reproductive and developmental toxicity of phthalates(邻苯二甲酸酯类化合物的生殖发育毒性)[J].J Tianjin Med Univ(天津医科大学学报), 2004,10(Supplement):15
[2] CAO Guo-zhou(曹国洲), XIAO Dao-qing(肖道清), ZHU Xiao-yan(朱晓艳).Risk assessment of phthalate plasticizers in food contact products(食品接触制品中邻苯二甲酸酯类增塑剂的风险评估)[J].Food Sci(食品科学),2010,31(5): 325
[3] Directive 2005/84/EC, Amending for the 22nd Time Council Directive 76/769/EEC on the Approximation of the Laws, Regulations and Administrative Provisions of the Member States Relating to Restrictions on the Marketing and Use of Certain Dangerous Substances and Preparations (Phthalates in Toys and Childcare Articles)[S].2005
[4] Directive 2007/19/EC, Amending Directive 2002/72/EC Relating to Plastic Materials and Articles Intended to Come into Contact with Food and Council Directive 85/572/EE Claying down the List of Simulants to Be Used for Testing Migration of Constituents of Plastic Materials and Articles Intended to Come into Contact with Foodstuffs [S].2007
[5] Otter R,Goth H.Hexamoll^© DINCH-our response to the plasticiser challenge[R].Brussels:the Conference Plasticisers, 2004:9
[6] Opinion of the Scientific Panel on food additives, flavourings, processing aids and materials in contact with food (AFC) on a request related to a 12th list of substances for food contact materials[J].EFSA J, 2006,9:395
[7] NICNAS.1,2-Cyclohexanedicarboxylic acid, 1,2-diisononyl ester ('Hexamoll DINCH')[R].Australia:Health and Ageing, 2011:9
[8] Directive 2002/72/EC, Relating to Plastic Materials and Articles Intended to Come into Contact with Foodstuffs [S].2002
[9] Nair CSB, Vidba R, Ashalatha PM.Hexamoll DINCH plasticised PVC containers for the storage of platelets[J].Asian J Transfus Sci, 2011, 5(1): 18
[10] Nagorka R, Conrad A, Scheller C, et al.Diisononyl 1, 2-cyclohexanedicarboxylic acid (DINCH) and di (2-ethylhexyl) terephthalate (DEHT) in indoor dust samples: concentration and analytical problems[J].Int J Hyg Environ Health, 2011, 214(1):26
[11] European Commission.Opinion on the results of a second risk assessment of DEHP human health part[R].Brussels: European Commission, 2004