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    气相色谱-串联质谱法快速测定电子电气产品用塑料中45种添加剂

    Rapid Determination of 45 Additives in Plastics for Electronic and Electrical Products by Gas Chromatography-Tardem Mass Spectrometry

    • 摘要: 建立了气相色谱-串联质谱法(GC-MS/MS)同时测定电子电气产品用塑料中45种添加剂的方法。将塑料样品剪碎成1 cm×1 cm的碎片后,取0.5 g,用体积比为1∶1的二氯甲烷-甲醇混合液(提取剂)于60 ℃超声提取30 min,提取2次,合并提取液并用提取剂定容至25 mL。选用DB-5HT色谱柱,在进样口温度350 ℃,离子源温度230 ℃,选择离子监测(SIM)扫描模式下对其进行分析。结果显示:45种添加剂的质量浓度在0.5~5.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)均为0.2 mg·L-1。对空白样品进行3个浓度水平的加标回收试验,回收率为82.0%~119%,测定值的相对标准偏差(RSD,n=6)为0.31%~8.5%。对样品进行6次重复性测定,测定值的RSD为0.22%~6.9%。方法用于测定实际样品中45种添加剂的含量,苯并(a)芘、邻苯二甲酸二正辛酯(DNOP)、邻苯二甲酸二辛酯(DEHP)、邻苯二甲酸二异丁酯(DIBP)均被不同程度地检出。

       

      Abstract: A method for simultaneous determination of 45 additives in plastics for electronic and electrical products by GC-MS/MS was established. The plastic samples were cut into 1 cm×1 cm fragments, then sample (0.5 g) was taken and extracted by ultrasonic twice with a mixture (extractant) of methylene chloride and methanol at volume ratio of 1:1 at 60℃ for 30 min. The obtained extracting solution was combined and made its volume up to 25 mL with extractant. DB-5HT column was used, and the sample solution were analyzed at inlet temperature of 350℃ and ion source temperature of 230℃ under SIM mode. As shown by the results, linear relationships between mass concentrations of 45 additives and their peak areas were kept in the range of 0.5-5.0 mg·L-1, with detection limit (3S/N) of 0.2 mg·L-1. Recovery test was made on the blank samples by standard addition method at 3 concentration levels, giving results in the range of 82.0%-119%, and RSDs (n=6) of the determined values were ranged from 0.31% to 8.5%. Repeatability test was made with RSDs (n=6) of the determined values ranged from 0.22% to 6.9%. The method was applied to the determination of 45 additives in actual samples, and benzo pyrene, DNOP, DEHP and DIBP were detected in different degrees.

       

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