Istanbul University, TEBİP Programme, Chemistry Department, 34220, İstanbul, Turkey.
Yıldız Technical University, Chemistry Department, 34220, İstanbul, Turkey.
J Trace Elem Med Biol. 2021 Dec;68:126859. doi: 10.1016/j.jtemb.2021.126859. Epub 2021 Sep 14.
An effective, green and rapid analytical strategy namely the simultaneous spray assisted droplet formation-liquid phase microextraction (S-SADF-LPME) method was developed for the determination of trace quantity of cadmium in saliva samples by using the slotted quartz tube-flame atomic absorption spectrophotometry (SQT-FAAS). By the developed method, external dispersive solvent usage for droplet formation was reduced to obtain a more environmental-friendly method.
Method consists of a simultaneous complexing and extraction step, which was based on spraying an extraction solvent containing a solid ligand into the aqueous sample solution, forming fine droplets without the use of dispersive solvent. The procedure was implemented using a customized, cost effective and portable spray apparatus to minimize the consumption of reagent, analysis time and operation steps. Thus, this methodology ensures better repeatability and accuracy while minimizing the relative errors caused by the experimental steps. Parameters including the buffer amount, extractant/ligand concentration, extraction solvent type, extraction/ligand solution volume, spraying number and vortex period were systemically optimized to lower the detection limit.
Under the optimal extraction conditions, 96.9-folds enhancement in the detection power of the traditional FAAS was achieved. The limit of detection and limit of quantification values of presented method were calculated to be 0.65 and 2.17 ng mL, respectively. Accuracy and applicability of the optimized method was investigated by collecting saliva samples from smokers. Satisfactory percent recovery values wereachieved for cadmium with a low standard deviation in the acceptable range of 84.9-109.6 %.
The developed dispersive solvent-free S-SADF-LPME technique presents a fast, simple, cost-effective and eco-friendly microextraction method based on the use of an easily accessible and functional spray apparatus.
开发了一种有效、绿色、快速的分析策略，即同时喷射辅助液滴形成-液相微萃取（S-SADF-LPME）方法，并用开槽石英管-火焰原子吸收光谱法（SQT-FAAS）测定唾液样品中痕量镉。通过该方法，减少了用于液滴形成的外部分散溶剂的使用，以获得更环保的方法。
该方法包括同时络合和萃取步骤，该步骤基于将含有固体配体的萃取溶剂喷射到水溶液样品溶液中，形成无需使用分散溶剂的细液滴。该程序使用定制的、经济高效的便携式喷雾装置来实施，以最大程度地减少试剂消耗、分析时间和操作步骤。因此，这种方法在最小化实验步骤引起的相对误差的同时，确保了更好的重复性和准确性。系统优化了包括缓冲液量、萃取剂/配体浓度、萃取溶剂类型、萃取/配体溶液体积、喷雾次数和涡旋周期等参数，以降低检测限。
在最佳萃取条件下，传统 FAAS 的检测能力提高了 96.9 倍。该方法的检出限和定量限分别计算为 0.65 和 2.17ng/mL。通过收集吸烟者的唾液样本，研究了优化方法的准确性和适用性。镉的回收率在 84.9-109.6%的可接受范围内，取得了令人满意的百分回收率值，且标准偏差较低。
所开发的无分散溶剂 S-SADF-LPME 技术是一种快速、简单、经济高效且环保的微萃取方法，基于使用易于获得和功能强大的喷雾装置。
