摘要
建立了超声提取-硅烷化气相色谱-质谱测定电子产品中四溴双酚A的方法。样品用正己烷/丙酮作提取剂,浸泡后超声提取,经N,O-双三甲基硅烷三氟乙酰胺(BSTFA)+1%三甲基氯硅烷(TMCS)衍生化,利用气相色谱-质谱仪进行定性定量分析。讨论了浸泡时间对提取效率的影响,优化衍生温度和衍生时间。结果表明:标样衍生后在0.4～4.0μg/mL范围内具有良好的线性。加标回收率范围在61%～93%之间,平行测定的相对标准偏差小于5%。方法的检出限为1.25 mg/kg,定量限为3.75 mg/kg。
A method for the determination of tetrabromobisphenol A in electronics using ultrasonic extraction and derivatisation by Gas Chromatography-Mass spectrometry was established.Samples were extracted with hexane and acetone mixtures.A derivatisation step was carried out with BSTFA＋TMCS as derivatisation reagents.Effect of experiment conditions,such as derivative volume,derivatisation time and temperature were investigated.Under the optimized conditions,the calibration curve showed good linearity between 0.4 μg/mL and 4.0 μg/mL.The results showed that the recoveries of samples were 61.2%~93%.The relative standard deviation was less than 5%.The limit of detection was 1.25 mg/kg,and the limit of quantity was 3.75 mg/kg.
出处
《分析试验室》
CAS
CSCD
北大核心
2011年第4期62-64,共3页
Chinese Journal of Analysis Laboratory
基金
北京市科学技术研究院萌芽计划项目(2008)资助
