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

    • 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1 g样品中加入40 mL甲苯,于60℃水浴中超声提取80 min,取2 mL样品溶液,采用硅胶固相萃取柱(6 mL/2 g)净化,经5 mL甲苯洗脱,收集洗脱液于试管中,氮吹至近干;再加入2 mL 0.1 mg·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0.005~1.000 mg·L-1,检出限(3S/N)为0.05~0.10 mg·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%。

       

      Abstract: A method for determination of 18 kinds of polycyclic aromatic hydrocarbons (PAHs) in rubber-plastic materials of writing pens by gas chromatography-mass spectrometry (GC-MS) was established. Toluene of 40 mL was added into the sample of 1 g, and ultrasonic extraction was carried out in 60℃ water bath for 80 min. The sample solution of 2 mL was purified by silica gel solid phase extraction column (6 mg/2 g), and eluted by toluene of 5 mL. The eluent was collected in the test tube and blowed to nearly dry with nitrogen, and 0.1 mg·L-1 internal standard solution of 2 mL 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 18 PAHs standard curves were in the same range of 0.005-1.000 mg·L-1, with detection limits (3S/N) in the range of 0.05-0.10 mg·kg-1. Recovery test was made on substantial samples at 3 concentration 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%.

       

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