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《化学分析计量》 2015年第06期
DOI:10.3969/j.issn.1008-6145.2015.06.002
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
张子豪,张海峰,麦晓霞,李全忠,李丹,刘莹峰,蚁乐洲,钟志光,郑建国
广东出入境检验检疫局,广州 510623 
Simultaneous Determination of the Migration of 20 Phthalates in Plastic Food Contact Materials by HPLC-MS-MS
张子豪,张海峰,麦晓霞,李全忠,李丹,刘莹峰,蚁乐洲,钟志光,郑建国
Guangdong Entry–Exit Inspection and Quarantine Bureau, Guangzhou, 510623, China 
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,C18色谱柱(100 mm×2.1 mm,2.7 μm)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1~500 ng/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0.20~9.81 ng/mL,0.19~9.76 ng/mL,0.25~12.3 ng/mL,0.21~10.8 ng/mL,0.19~11.7 ng/mL,0.45~20.3 ng/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。 
Abstract: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 oil 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 
Keywords:food contact materials; phthalates; migration; HPLC-MS-MS 
基金:国家质检总局科研项目 
本文引用格式:
张子豪,张海峰,麦晓霞,等.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[J].化学分析计量,2015,24(6):6-10 .
ZHANG Z H,ZHANG H F,MAI X X,et al.Simultaneous Determination of the Migration of 20 Phthalates in Plastic Food Contact Materials by HPLC-MS-MS[J]. Chemical analysis and meterage,2015,24(6):6-10. 

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