高效液相色谱–串联质谱法同时测定塑料食品接触材料中20种邻苯二甲酸酯迁移量  

Simultaneous Determination of the Migration of 20 Phthalates in Plastic Food Contact Materials by HPLC–MS–MS

作　　者：张子豪[1] 张海峰[1] 麦晓霞[1] 李全忠[1] 李丹[1] 刘莹峰[1] 蚁乐洲[1] 钟志光[1] 郑建国[1] 

机构地区：[1]广东出入境检验检疫局,广州510623

出　　处：《化学分析计量》2015年第6期6-10,共5页Chemical Analysis And Meterage

基　　金：国家质检总局科研项目(2015IK049;2013IK003);质检行业公益性科研专项(2012104020);广东检验检疫局科研项目(2014GDK52);广东省科技计划项目(2013B040402005)

摘　　要：采用高效液相色谱-串联质谱（LC-MS／MS）技术建立了食品接触材料中20种邻苯二甲酸酯类迁移量的测定方法。样品分别采用欧盟（Eu）No．10／2011法规中食品模拟液浸泡，橄榄油浸泡液用乙腈进行液-液萃取，水基浸泡液直接过滤，Cj8色谱柱（100mm×2．11mm，2．7μm）分离，以0．1％甲酸溶液-甲醇溶液为流动相，梯度洗脱，采用多反应监控（MRM）模式进行分析检测。20种邻苯二甲酸酯类化合物质量浓度在1-500ng／mL范围内与色谱峰面积呈线性关系。水溶液、3％乙酸食品模拟浸泡液、10％乙醇食品模拟浸泡液、20％乙醇食品模拟浸泡液、50％乙醇食品模拟浸泡液、橄榄油食品模拟浸泡液中方法定量限分别为0．20-9．81ng／mL，0．19-9．76ng／mL，0．25-12．3ng／mL，0．21—10．8ng／mL，0．19-11．7ng／mL，0．45～20-3ng／mL。样品加标回收率为85．8％-111．3％（3％乙酸浸泡液），79．4％-123．6％（橄榄油浸泡液），两种浸泡液中测定结果的相对标准偏差不大于8．48％（n=6）。该方法具有快速简便、灵敏度高及准确性好等特点，适用于塑料类食品接触材料中邻苯二甲酸酯类迁移量的检测。A high performance liquid chromatography-tandem mass spectrometry （HPLC-MS / MS） method was developed for the determination of migration of 20 phthalates in food contact materials. Samples were soaked in different kinds of food simulants according to （EU） No. 10/2011, the extractants from water-based simulants were directly filtered, while the extractant from olive oit simulant was extracted with acetonitrile. A C18 column （100 mm × 2.1 mm, 2.7 μm） was used to separate the target ingredients, and a system of 0.1% formylic acid solution-methanol was used as the mobile phases with a procedure of gradient elution. The phthalates were analyzed by multiple reaction monitoring mode. The linear range was 1-500 ng/ mL. The limits of quantification were 0.20-9.81 ng / mL in distilled water, 0.19-9.76 ng / mL in 3% acetic acid,0.25-12.3 ng/mL in 10% alcohol,0.21-10.8 ng/mL in 20% alcohol,0.19-11.7 ng/mL in 50% alcohol, and 0.45-20.3 ng/mL in olive oil. The recoveries was 85.8%-111.3%（3% acetic acid） and 79.4%-123.6%（olive oil）, and the relative standard deviations （RSDs） were not more than 8.48%（n=6）. This method was simple, sensitive, accurate and precise, and appropriate for the determination of phthalates in food contact plastic materials.

关 键 词：食品接触材料 邻苯二甲酸酯 迁移量 液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学]