建立了气相色谱-内标法测定海绵文胸中的甲苯二异氰酸酯(TDI)残留量.样品经均质处理后,用经脱水处理的乙酸乙酯超声萃取25 min,过滤净化后,采用Agilent DB-624色谱柱(30 m×0.32 mm×1.8 μm)分析,柱温采用程序升温,检测器为氢火焰离子化检测器,检测器温度为250 ℃,进样口温度为180 ℃,载气为氮气.结果表明:甲苯二异氰酸酯在10~200 mg/L范围内峰面积与质量浓度线性关系良好,线性相关系数(R2)为0.998.9,平均回收率为80.5%~91.6%,RSD不大于7.9%(n=6),方法的检出限和定量限分别为10 mg/kg和100 mg/kg.在优化条件下,对生产企业、实体店和电商平台采购的100批次样品进行了检测.该方法操作简单、耗时短、灵敏度高、稳定性好,应用于日常检测可大大降低检测成本,缩短检测周期,具有实际应用价值.
A gas chromatography (GC) with internal standard method was developed for the determination of residual toluene diisocyanate (TDI) in sponge bra.The samples were extracted with ethyl acetate dehydrated,and cleaned up with 0.22 μm microfiltration membrane.The residual toluene diisocyanate was separated on a DB-624 capillary column using temperature programming.The flame ionization detector (FID) was used at 250 ℃.The inlet temperature was 180 ℃ with nitrogen as carrier gas.The linear range was 10-200 mg/L (R2=0.9989) for TDI.The average recovery ranged from 80.5% to 91.6% with RSD not more than 7.9%(n=6).The limit of detection (LOD) and limit of quantification (LOQ) were 10 mg/kg and 100 mg/kg,respectively.The developed method was then utilized to analyse the 100 batches of sponge bra samples from the manufacturing enterprises,the entity shops and electric business platforms.The method is simple,time-saving and environment friendly with high sensitivity and good reproducibility,and has practical application value due to its low-cost and short-circle.
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