色谱 ›› 2015, Vol. 33 ›› Issue (8): 856-863.DOI: 10.3724/SP.J.1123.2015.04011

• 研究论文 • 上一篇    下一篇

高效液相色谱-紫外检测法同时测定食品接触材料中7种苯多酸及其衍生物的特定总迁移量

王建玲, 肖晓峰, 陈彤, 刘艇飞, 何军, 邓弘毅, 杨娟娟   

  1. 台州出入境检验检疫局, 浙江 台州 318000
  • 收稿日期:2015-04-08 出版日期:2015-08-08 发布日期:2015-07-27
  • 通讯作者: 肖晓峰
  • 基金资助:

    国家质检总局科技计划项目(2013IK022).

Simultaneous determination of total specific migration limit of seven benzene polycarbonic acids and their derivatives in food simulants by high performance liquid chromatography-ultraviolet detection

WANG Jianling, XIAO Xiaofeng, CHEN Tong, LIU Tingfei, HE Jun, DENG Hongyi, YANG Juanjuan   

  1. Taizhou Entry-Exit Inspection and Quarantine Bureau, Taizhou 318000, China
  • Received:2015-04-08 Online:2015-08-08 Published:2015-07-27

摘要:

建立了高效液相色谱-紫外检测(HPLC-UV)同时测定5种食品模拟物(10%(v/v)乙醇、20%(v/v)乙醇、50%(v/v)乙醇、3%(w/v)乙酸和橄榄油)中偏苯三甲酸、偏苯三甲酸酐、间苯二甲酰氯、间苯二甲酸、对苯二甲酰氯、邻苯二甲酸、对苯二甲酸的特定总迁移量(SML(T))的方法。用食品模拟物浸泡待测样品,冷却至室温并混匀,水基食品模拟物经亲水性聚四氟乙酸针头过滤器过滤后进样;橄榄油用0.1%(w/v)乙酸铵水溶液提取后,下层清液用亲水性聚四氟乙烯针头过滤器过滤后进样。用Synergi Polar-RP色谱柱(250 mm×4.6 mm, 4 μm)分离,梯度洗脱,检测波长为232 nm。5种食品模拟物中的定量限为0.1~0.2 mg/kg;水基食品模拟物在0.5~12 mg/L、橄榄油食品模拟物在0.5~12 mg/kg范围内线性关系良好(r2 > 0.99991); 1.25、2.5、6.25 mg/kg水平的加标回收率为94.3%~105%,相对标准偏差为0.1%~2.3%。结果表明,该方法的色谱分离和线性关系较好,回收率和准确度高,完全满足欧盟(EU)No 10/2011法规附表2中7种苯多酸及其衍生物的SML(T)的限量要求,并已应用于实际样品的检测。

关键词: 对苯二甲酸, 高效液相色谱-紫外检测法, 间苯二甲酸, 邻苯二甲酸, 偏苯三甲酸, 特定总迁移量

Abstract:

A novel method for simultaneous determination of total specific migration limits (SML(T)) of trimellitic, isophthalic, terephthalic, phthalic acid and their derivatives (1,2,4-benzenetricarboxylic anhydride, isophthaloyl chloride and terephthaloyl chloride) in food simulants (10% (v/v) ethanol, 20% (v/v) ethanol, 50% (v/v) ethanol, 3% (w/v) acetic acid and olive oil) was developed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). After the migration test, the soaking solution was cooled down and vortexed. After the extraction of olive oil food simulants with 0.1% (w/v) ammonium acetate aqueous solution, the clear aqueous solution or other aqueous food simulants was filtered through a hydrophilic polytetrafluoroethylene filter with a disposable syringe before injection. The Synergi Polar-RP column (250 mm×4.6 mm, 4 μm) and gradient elution mode were selected. The variable wavelength detector was set at 232 nm. The limits of quantification were 0.1-0.2 mg/kg; the linearity of the method was good with r2>0.99991 over the range from 0.5 to 12 mg/L for aqueous food simulants or 0.5 to 12 mg/kg for olive oil food simulants. The recoveries of them were between 94.3% and 105% with the relative standard deviations between 0.1% and 2.3% at the levels of 1.25, 2.50, 6.25 mg/kg. The method shows the low limits of detection, good recoveries and accuracies, and meets the requirement of (EU)No 10/2011 regulation for the total specific migration limits of trimellitic, isophthalic, terephthalic, phthalic acids and their derivatives. The method has been applied to the analysis of food contact material samples.

Key words: high performance liquid chromatography-ultraviolet detection (HPLC-UV), isophthalic acid, phthalic acid, terephthalic acid, total specific migration limit (SML(T)), trimellitic acid

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