摘要
建立了气相色谱-质谱（ GC-MS）联用法快速测定儿童产品中2种有机磷阻燃剂，磷酸苯基（二叔丁基苯基）酯（DBPP）和2，2-双氯甲基-三亚甲基-双[双（2-氯乙基）磷酸脂（V6）的分析方法。考察了不同萃取方法，不同萃取溶液，不同极性色谱柱对DBPP和V6分离检测的影响。采用丙酮作为萃取溶剂，超声萃取样品中DBPP和V6，选用DB-5MS色谱柱进行目标物分离，质谱定量检测。结果显示，DBPP在0．01～10 mg／kg内，线性关系良好（R2＞0．9991），重现性良好。 V6在1～30 mg／kg内，线性关系良好（R2＞0．9993），重现性良好。在0．01～10 mg／kg添加水平内DBPP的平均回收率为89．3％～94．2％，相对标准偏差3．8％～4．3％。在1～30 mg／kg V6添加水平内的平均回收率为87．2％～95．7％，相对标准偏差4．8％～6．5％。 DBPP和V6的方法检出限（ S／N＞10）分别为0．01，1 mg／kg。该方法快速简捷，灵敏度高，定性准确，易于操作，适用于进出口儿童产品中的DBPP和V6日常检测工作。
An analytical method was developed for rapid determination of extraction of bis（4-tert-butylphe-nyl）phenyl phosphate（DBPP） and 2,2-bis（chloromethyl）trimethylene（bis（2-chloroethyl）phosphate）（V6） in child products by GC-MS.The separation and detection conditions were optimized for different extraction methods ,different extraction solvent and chromatography columns .Using acetone as solvent extraction ,DB-PP and V6 were extracted by ultrasonic .DBPP and V6 were separated by using the DB-5MS column and detected by mass spectrometry .The results showed that the linear correlation coefficient （ R2 ） of DBPP were higher than 0.999 1 with 0.01～10 mg/kg,the average recoveries were between 89.3%～94.2%,the line-ar correlation coefficient （ R2 ） of V6 were higher than 0.999 3 with 1～30 mg/kg,the average recoveries were between 87.2%～95.7%in the spiked range of 1～30 mg/kg,and the relative standard deyiations （RSDs）were between 4.8%～6.5%.The limit of detection of DBPP was 0.01 mg/kg,V6 was 1 mg/kg. This proposed method is rapid and convenient for the determination ,and easy for the operation .It is appro-priate for the determination of DBPP and V 6 in child products for import and export .
出处
《应用化工》
CAS
CSCD
北大核心
2015年第4期754-757,共4页
Applied Chemical Industry
基金
江苏省科技支撑计划(BE2013507)
关键词
气相色谱-质谱
超声萃取
有机磷阻燃剂
儿童产品
gas chromatography-mass spectrometry （ GC-MS ）
ultrasonic extraction
organophosphorousflame retardant
child products
