Department of Chemistry, Federal University of Santa Maria, Av. Roraima, 1000, 97.105-900 Santa Maria, RS, Brazil.
Department of Chemistry, Federal University of Santa Maria, Av. Roraima, 1000, 97.105-900 Santa Maria, RS, Brazil.
Talanta. 2017 Aug 1;170:488-495. doi: 10.1016/j.talanta.2017.04.048. Epub 2017 Apr 22.
A calibration strategy using porous nylon disks and reference solutions is proposed for the first time for matrix matching and determination of As, Ba, Cd, Cr, Pb, Sr and Zn in polymers by laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS). Polymer samples commonly used in contact with food were analyzed. The procedure consists on the use of porous nylon disks as support for a dried droplet reference solution. Calibration in the range of 0.50-190μgg for Ba, Cd, Cr, Pb, Sr and Zn and from 0.30-9.0μgg for As was used. Laser and ICP-MS instrument conditions were evaluated in order to achieve the best signal-to-background ratio. The radiofrequency power and carrier gas flow rate were fixed at 1300W and 1.25Lmin, respectively. Spot size, repetition rate, scan line speed and laser fluency were set to 100µm, 20Hz, 100µms and 17.9Jcm, respectively, as the established conditions for analysis of standards and samples. By using these conditions, limits of detection, estimated considering B+3s (where B is the value of the blank and s is the standard deviation of 10 measurements of the blank), ranged from 0.09μgg (Pb) to 1.09 (Cr) and 0.05μgg (Pb) to 2.10 (Cr) for calibration with and without C as internal standard (IS). In spite to the use of nylon for matrix matching of different polymeric matrices, the normalization with C as IS was also evaluated. The precision of the method is relatively good (RSD<20%), and the accuracy of the method, evaluated by analysis of certified reference materials (CRM) and by comparison with results obtained from solution analysis by ICP-MS after sample decomposition by microwave induced combustion (MIC) is relatively good. The suitability of the proposed method resulted in direct and reliable analyses of polymer samples with a simplified or unnecessary sample preparation step. In addition, the calibration with dried droplet reference solutions may be considered a promising procedure in view of its advantages to other forms of calibration, as the use of CRM or the preparation of synthetic standards. The use of porous nylon disks spiked with reference solutions for calibration is the main advantage of the present work.
本文首次提出了一种使用多孔尼龙圆盘和参考溶液的校准策略,用于通过激光烧蚀-电感耦合等离子体质谱法(LA-ICP-MS)对聚合物中的 As、Ba、Cd、Cr、Pb、Sr 和 Zn 进行基体匹配和测定。分析了常用于接触食品的聚合物样品。该方法包括使用多孔尼龙圆盘作为支撑,用于干燥液滴参考溶液。在 0.50-190μg/g 范围内对 Ba、Cd、Cr、Pb、Sr 和 Zn 以及 0.30-9.0μg/g 范围内对 As 进行了校准。为了获得最佳的信噪比,评估了激光和 ICP-MS 仪器条件。射频功率和载气流量分别固定在 1300W 和 1.25L/min。光斑尺寸、重复率、扫描线速度和激光能量密度分别设置为 100μm、20Hz、100μms 和 17.9J/cm,作为分析标准和样品的既定条件。使用这些条件,考虑到 B+3s(其中 B 是空白值,s 是空白值的 10 次测量的标准偏差),检测限范围为 0.09μg/g(Pb)至 1.09(Cr)和 0.05μg/g(Pb)至 2.10(Cr),用于有和没有 C 作为内标(IS)的校准。尽管使用尼龙对不同聚合物基质进行基体匹配,但也评估了用 C 作为 IS 的归一化。该方法的精密度相对较好(RSD<20%),并且通过分析认证参考物质(CRM)和通过与微波诱导燃烧(MIC)后溶液分析得到的结果进行比较,该方法的准确性相对较好。该方法的适用性导致了聚合物样品的直接和可靠分析,简化或无需进行样品制备步骤。此外,与使用 CRM 或合成标准品的其他形式的校准相比,使用干燥液滴参考溶液进行校准可能是一种很有前途的方法。使用多孔尼龙圆盘加参考溶液进行校准是本工作的主要优点。