气相色谱-质谱法测定书写笔用橡塑材料中18种多环芳烃的含量  

GC-MS Determination of 18Polycyclic Aromatic Hydrocarbons in Rubber-Plastic Materials of Writing Pens

作　　者：郝晓红 史福霞[1] 肖湾 马红青[1] HAO Xiaohong;SHI Fuxia;XIAO Wan;MA Hongqing(Institute of Quality Inspection of Light Industry&Chemical Products,Shanghai Institute of quality Inspection and Technical Research,Shanghai 201114,China)

机构地区：[1]上海市质量监督检验技术研究院轻工与化工产品质量检验所,上海201114

出　　处：《理化检验（化学分册）》2022年第1期7-12,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：上海市科学技术委员会研发公共服务平台建设项目(14DZ2293000)。

摘　　要：建立了气相色谱-质谱法测定书写笔用橡塑材料中18种多环芳烃(PAHs)含量的方法。在1g样品中加入40mL甲苯,于60℃水浴中超声提取80min,取2mL样品溶液,采用硅胶固相萃取柱(6mL/2g)净化,经5mL甲苯洗脱,收集洗脱液于试管中,氮吹至近干;再加入2mL 0.1mg·L^(-1)的内标溶液,在离子源温度为280℃,选择离子监测(SIM)模式下进行测定,内标法定量。结果显示:18种PAHs标准曲线的线性范围均为0.005~1.000mg·L^(-1),检出限(3S/N)为0.05~0.10mg·kg^(-1);对实际样品进行3个浓度水平的加标回收试验,18种PAHs的回收率为90.0%~104%,测定值的相对标准偏差(RSD,n=7)为1.0%~7.5%。A method for determination of 18kinds of polycyclic aromatic hydrocarbons(PAHs)in rubberplastic materials of writing pens by gas chromatography-mass spectrometry(GC-MS)was established.Toluene of 40mL was added into the sample of 1g,and ultrasonic extraction was carried out in 60℃water bath for 80min.The sample solution of 2mL was purified by silica gel solid phase extraction column(6mg/2g),and eluted by toluene of 5mL.The eluent was collected in the test tube and blowed to nearly dry with nitrogen,and 0.1mg·L^(-1)internal standard solution of 2mL was added.The ion source temperature was 280℃,and SIM mode and internal standard method were used for quantitative analysis.It was showed that the linear ranges of 18PAHs standard curves were in the same range of 0.005-1.000mg·L^(-1),with detection limits(3S/N)in the range of 0.05-0.10mg·kg^(-1).Recovery test was made on substantial samples at 3concentration levels by standard addition method,giving results in the range of 90.0%-104%,and RSDs(n=7)of the determined values were ranged from 1.0%to 7.5%.

关 键 词：气相色谱-质谱法 多环芳烃 书写笔 橡塑材料 

分 类 号：O657.63[理学—分析化学]