超高效液相色谱—串联质谱法测定聚酰胺厨具中23种初级芳香胺的迁移量

Determination of Migrations of 23 Primary Aromatic Amines in Polyamide Kitchenware by Ultra-High Performance Liquid Chromatography-Tadem Mass Spectrometry

将表面积为0.6 dm~2聚酰胺厨具样品浸泡在100 mL 3%(质量分数)乙酸溶液中,于(100±3)℃加热2 h,再重复浸泡两次。收集各浸泡液1 mL,用0.22μm针式滤膜过滤,滤液供优化的仪器工作条件测定。以CORTECS T3色谱柱(100 mm×2.1 mm, 2.7μm)为固定相,以不同体积比的含0.1%(体积分数)甲酸的甲醇溶液和水的混合溶液为流动相进行梯度洗脱,分离后的初级芳香胺(PAAs)在电喷雾离子源正离子(ESI~+)模式以及多反应监测(MRM)模式下用串联质谱法(MS/MS)检测。结果显示:23种PAAs的质量浓度均在1~20μg·L^(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.04~0.5μg·L^(-1);对阴性样品进行3个浓度水平的加标回收试验,所得回收率为90.9%~107%,测定值的相对标准偏差(n=6)为0.40%~7.3%。方法用于10种聚酰胺厨具的分析,仅在平底铲、饭勺、薯压、汤勺等4款厨具中检出了4,4′-二氨基二苯甲烷(4,4′-MDA)、4-氯邻甲苯胺(4-CoT)和对氯苯胺(4-CA),检出量(0.4~1.3μg·kg^(-1))随浸泡次数的增加而降低。

The sample with surface area of 0.6 dm~2 of polyamide kitchenware was immersed in 100 mL of 3%(mass fraction) acetic acid solution, and the mixture was heated at(100±3)℃ for 2 h. After the immersing process was repeated twice, each immersing solution was collected, and an aliquot(1 mL) was filtered with a 0.22 μm needle filter membrane. The filtrate was used for determination under optimized instrument working conditions. CORTECS T3 column(100 mm×2.1 mm, 2.7 μm) was used as the stationary phase, and methanol containing 0.1%(volume fraction) formic acid-water mixed solution at various volume ratios was used as the mobile phase for gradient elution. The primary aromatic amines(PAAs) separated were detected by MS/MS with an electrospray ion source in positive mode under multiple reaction monitoring mode. As shown by results that the mass concentrations of 23 PAAs were all linearly related with their corresponding peak areas in the range of 1-20 μg·L^(-1), with detection limits(3 S/N) in the range of 0.04-0.5 μg·L^(-1). Test for recovery was made on the negative samples by standard addition method, giving values of recovery in the range of 90.9%-107%, and RSDs(n=6) of the determined values ranged from 0.40% to 7.3%. The proposed method was applied to the analysis of 10 kinds of polyamide kitchenware, and 4,4′-MDA, 4-CoT and 4-CA were detected in the 4 types of kitchenware, including flat spatula, rice spoon, potato pressure and soup spoon, and the detection amounts(0.4-1.3 μg·kg^(-1)) decreased with the increase of immersing times.