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    高效液相色谱法测定聚甲基丙烯酸酯食品材料中甲基丙烯酸酯及甲基丙烯酸向模拟食品液的迁移量

    Determination of Amounts of Methacrylates and Methacrylic Acid of Food-Containing Polymethacrylate Material Migrated Into Food Simulants by HPLC

    • 摘要: 以4%乙酸溶液和4种浓度(10%,20%,50%,95%)的乙醇溶液作为食品模拟液,将作为食品接触材料的聚甲基丙烯酸酯(PMA)塑料薄片分别浸泡于上述5种食品模拟液中。塑料片的测试面积(S)为0.3 dm2,模拟液的体积为50.0 mL。分别在3种条件下浸泡:1 70℃,2 h;2 40℃,10 d;3 60℃,2 h (95%乙醇溶液作为食品模拟液时)。浸泡后的模拟液经0.45 μm滤膜过滤后,滤液按仪器工作条件进行高效液相色谱分析。选择Shim Sen-VD C30色谱柱(250 mm×4.6 mm,3 μm)作为分离柱,柱温为35℃,以不同比例的(A)0.1%(体积分数)磷酸溶液和(B)甲醇的混合溶液作为流动相进行梯度洗脱,流动相的流量为0.5 mL·min-1,在此条件下,所测定的13种甲基丙烯酸及其羧酸酯可达到理想分离,并在波长210 nm处进行紫外检测。结果表明:13种化合物所测得的峰面积与相应的质量浓度之间的线性关系均为1~20 mg·L-1,其检出限(3S/N)为0.015~0.084 mg·L-1。分别对在上述5种食品模拟液中和3种浸泡条件下用标准加入法进行回收试验。结果表明:每一化合物的平均回收率均在85.0%以上,测定值的相对标准偏差(n=6)均小于6.0%。

       

      Abstract: Aqueous solutions (50.0 mL each) of 4% acetic acid and 10%, 20%, 50%, 95% ethanol were used separately as food simulants (abbrev. as FSs), and thin pieces of PMA plastic (with testing area of 0.3 dm2) were taken as the specimen to be soaked in the 5 FSs in the testing under 3 soaking conditions:1 70℃ for 2 h; 2 40℃ for 10 d and 3 60℃ for 2 h (95% ethanol solution). After soaking, the solution was filtered through 0.45 μm filtering membrane, and the filtrate was used for HPLC analysis under the working condition of the instrument. Shim Sen-VD C30(250 mm×4.6 mm, 3 μm) chromatographic column with column temperature at 35℃, and mixtures of (A) 0.1% (volume fraction) H3PO4 acid solution and (B) methanol in various ratios were selected for HPLC separation by gradient elution with flow-rate of 0.5 mL·min-1. 13 compounds of the methacrylates and methacrylic acid were well-separated and determined by UV-detector at the wavelength of 210 nm. As shown by the results, linearity ranges of the standard curves of the 13 compounds were found same between 1 to 20 mg·L-1. Detection limits (3S/N) found were in the range of 0.015 to 0.084 mg·L-1. Tests for recovery were made by standard addition method in 5 FS, and 3 soaking conditions separately, and as shown by the results, values of average recovery for the 13 compounds were all over 85%, and RSDs (n=6) all less than 6%.

       

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