摘要
提出了搅拌棒吸附萃取(SRAE)-气相色谱-质谱法测定化妆水中7种多氯联苯含量的方法。采用正交试验方法研究了萃取时间、分散剂种类及体积、热脱附时间及冷阱收集温度对萃取效率的影响。分析中采用DB-5MS毛细管色谱柱作为分离柱,质谱条件为电子轰击电离源全扫描监测模式。7种多氯联苯的峰面积与其质量分数在一定范围内呈线性关系,测定下限(10S/N)在5~60ng.kg-1之间。分别在3个浓度水平对方法的回收率和精密度进行了试验,测得回收率在74%~107%之间,测定值的相对标准偏差(n=6)在1.1%~16.9%之间。
A method of GC-MS with stirring rod adsorptive extraction for the determination of 7 polychloro biphenyls (PCB' s) in cosmetic lotion was proposed. Influential factors of the extraction process, including extraction time, extraction solvent and its amount, thermodesorption time and cold injection temperature were studied by orthogonal testing. DPrSMS capillary chromatographic column was used in C-C, and the full scanning monitoring with electron impact ionization source was adopted in MS. Linear relationship between values of peak area and mass fraction of PCB's was obtained in definite ranges, with lower limits (10S/N) of determination in the range of 5-60 ng·kg^-1 Tests for recovery and precision were made at 3 concentration levels, giving results of recove ry in the range of 74%-107% with values of RSD's (n=6) in the range of 1.1%-16.9%
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2012年第6期705-708,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
浙江省科技计划资助项目(2010C33074和2011C37020)