摘要
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×1.8μm)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(R^2)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(G C)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 with0.22^m microfiltration membrane.The residual toluene diisocyanate was separated on a DB-624capillary column using temperature programming.The flame ionization detector(FID)was used at250U h e inlet temperature was180t with nitrogen as carrier gas.The linear range was10-200mg/L(及2=0.9989)for TDI.The average recovery ranged from80.5%to91.6%with RSD not more than7.9%(n=6).The limit of detection(LOD)and limit of quantification(LOQ)were10mg/kg and100mg/k g,respectively.The developed method was then utilized to analyse the100batches 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.
作者
王爱霞
叶平
黄楠
陈妍
李兴根
WANG Aixia;YE Ping;HUANG Nan;CHEN Yan;LI Xinggen(Product Quality Supervising and Inspecting Center of Taizhou City,China National Supervision & Testing Center of Fine Chemicals,Taizhou 225300,China)
出处
《色谱》
CAS
CSCD
北大核心
2017年第6期665-668,共4页
Chinese Journal of Chromatography
基金
江苏省质量技术监督局风险监测项目(322015120013)~~
关键词
气相色谱
内标法
甲苯二异氰酸酯
海绵文胸
gas chromatography ( G C )
internal standard method
toluene diisocyanate (TDI)
sponge bra
