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，4μm）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。
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 simu-lants(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 vari-able 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. 999 91 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 to-tal specific migration limits of trimellitic,isophthalic,terephthalic,phthalic acids and their de-rivatives. The method has been applied to the analysis of food contact material samples.
参考文献
| [1] | Berthet, A.;Berode, M.;Bouchard, M..Gas-chromatography mass-spectrometry determination of phthalic acid in human urine as a biomarker of folpet exposure[J].Analytical and bioanalytical chemistry,20112(2):493-502. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%