有机相阴离子交换固相萃取HPLC-UV法快速测定食品接触材料中4种尼泊金酯的特定迁移量

Rapid Determination of Specific Migration of Four Parabens in Food Simulants by HPLC-UV Detection with Organic Phase Anion Exchange Solid Phase Extraction

建立了有机相阴离子交换固相萃取/高效液相色谱紫外法(HPLC-UV)快速测定10%乙醇、3%乙酸、20%乙醇、50%乙醇和橄榄油食品模拟物中尼泊金甲酯、尼泊金乙酯、尼泊金异丙酯和尼泊金丙酯的特定迁移量(SM)。橄榄油食品模拟物样品采用有机相阴离子交换固相萃取法净化,水基食品模拟物样品经亲水性聚四氟乙烯针式过滤器过滤后直接进样。以甲醇和纯水为流动相,4种尼泊金酯在ZORBAX SB-Phenyl柱上等度洗脱,12.5 min内达到基线分离;紫外外标校准曲线法定量。4种尼泊金酯在0.5~100 mg/L范围内线性关系良好(r2≥0.999 8),在10、50、100 mg/kg 3个浓度水平下的加标回收率为97.9%~103%,相对标准偏差为0.02%~2.2%,在5种食品模拟物中的定量下限为0.1~0.5 mg/kg。结果表明,该方法的色谱分离和线性关系好,回收率和准确度高,满足欧盟(EU)NO 10/2011法规附表1中4种尼泊金酯SM的限量要求,并已应用于实际样品的检测。

A method for the rapid determination of specific migration （SM ） of methylparaben,ethylparaben,isopropylparaben and propylparaben in food simulants （10 % ethanol,3 % acetic acid,20 % ethanol,50 % ethanol and olive oil ） was developed by HPLC-UV detection with organic phase anion exchange （OPAE ） solid phase extraction （SPE ）.After the migration test,the soaking solution was cooled down,and vortexed.The olive oil food simulant sample was pretreated by organic phase anion exchange solid phase extraction before injection,while the aqueous food simulant （10 % ethanol,3 % acetic acid,20 % ethanol or 50 % ethanol solution ） sample was just filtered through a polytetrafluoroethylene filter with a disposable syringe before injection.The baseline separations for four parabens were achieved within 12.5 min on a phehyl column.The external standard method for calibration curve was adopted via ultraviolet detector.The linearities of the method for 4 parabens were good with r 2≥0.999 8 over the concentration range of 0.5-100 mg/L.The recoveries for 4 parabens in 5 types of food simulants at spiked levels of 10,50,100 mg/kg were between 97.9 % and 103 % with relative standard deviations of 0.02 % -2.2 % .The limits of quantitation of the method were between 0.1 mg/kg and 0.5 mg/kg. With the low limits of quantitation,good recoveries and accuracies,the method could meet the requirements of （EU ）NO 10/2011 regulation for the specific migration limit of four parabens.The method was applied in the analysis of food contact material samples.