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    高效液相色谱-串联质谱法同时测定玩具中5种PBT物质的含量

    Simultaneous Determination of 5 PBT Substances in Toys by High Performance Liquid Chromatography-Tandem Mass Spectrometry

    • 摘要: 提出了高效液相色谱-串联质谱法同时测定玩具中5种持久性、生物累积性和毒性(PBT)物质含量的方法。按照ISO 8124-3:2020对玩具中的涂层、塑料及纺织物进行取样和处理,分取1 g,加入10 mL甲苯。密封,于常温超声萃取30 min。取上层清液过0.45 μm滤膜,滤液用高效液相色谱-串联质谱仪分析。在色谱分析中,以Agilent Poroshell HPH-C18色谱柱为固定相,以不同体积比的甲醇-0.1%(体积分数)乙酸溶液的混合溶液为流动相进行梯度洗脱分离。在质谱分析中,采用电喷雾离子源正离子(ESI+)模式和多反应监测(MRM)模式扫描,外标法定量。结果显示,5种PBT物质的质量浓度在0.005~0.2 mg·L-1内和峰面积呈线性关系,检出限(3S/N)为0.010~0.078 mg·kg-1。按照标准加入法进行回收试验,回收率为85.7%~105%,测定值的相对标准偏差(n=6)均不大于7.0%。

       

      Abstract: A method of high performance liquid chromatography-tandem mass spectrometry was proposed for the simultaneous determination of 5 persistent, bioaccumulative and toxic (PBT) substances in toys. The coatings, plastics, and textiles of toys were collected and treated in accordance with ISO 8124-3:2020, and an aliquot (1 g) was taken, and mixed with 10 mL of toluene. After sealing, ultrasonic extraction was performed at room temperature for 30 min. The supernatant was taken and passed through a 0.45 μm filter membrane, and the filtrate was analyzed by high performance liquid chromatograph-tandem mass spectrometer. In the chromatography analysis, Agilent Poroshell HPH-C18 column was used as the stationary phase, and mixed solutions composed of methanol and 0.1% (volume fraction) acetic acid solution at different volume ratios were used as the mobile phase for gradient elution separation. In the mass spectrometry analysis, ESI+ and MRM modes were used for scanning, and external standard method was used for quantification. It was shown that linear relationships between values of the mass concentration of 5 PBT substances and the peak area were kept in the range of 0.005-0.2 mg·L-1, with detection limits (3S/N) in the range of 0.010-0.078 mg·kg-1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 85.7%-105%, and RSDs (n=6) of the determined values were not greater than 7.0%.

       

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