Chemistry Department, Hacettepe University, 06800, Beytepe, Ankara, Turkey.
Environmental Engineering Department, Hacettepe University, 06800, Beytepe, Ankara, Turkey.
Anal Methods. 2021 Feb 28;13(8):1058-1068. doi: 10.1039/d0ay02235g. Epub 2021 Feb 11.
In this study ultrasound assisted-deep eutectic solvent-based liquid phase microextraction followed by microsampling-flame atomic absorption spectrometry was developed to determine prohibited lead and cadmium traces in hair dye and henna samples. For this purpose, deep eutectic solvent, prepared from choline chloride and phenol, was used as an extraction solvent, dithizone was used as a complexing agent, and THF was used as an aprotic solvent. All parameters that affect extraction efficiency, such as pH, the DES volume and composition, the extraction time, the amount of dithizone, were optimized. Under the optimal conditions, for Pb(ii) and Cd(ii), enhancement factors of 92 and 57, LODs of 2.5 μg L and 0.75 μg L, LOQs of 7.8 μg L and 2.5 μg L, linear working ranges of 10-250 μg L and 2.5-50 μg L, were obtained, respectively. Relative standard deviation (n = 10) was calculated to be 2.7 for 100 μg L of Pb(ii) and 2.1 for 25 μg L of Cd(ii). The matrix effect was investigated by comparing the solvent-based calibration curve with the matrix-matched calibration curve. The determination of lead and cadmium in hair dye and henna samples without being affected by the sample matrix was successfully performed. The lead content was between 1.3 and 6.5 μg g, and the cadmium content was between 0.028 and 0.54 μg g for the selected hair dye and henna samples.
本研究建立了一种超声辅助-深共晶溶剂液相微萃取结合微采样-火焰原子吸收光谱法,用于测定染发剂和指甲花样品中禁用的铅和镉痕迹。为此,我们使用了由氯化胆碱和苯酚制备的深共晶溶剂作为萃取溶剂,二硫腙作为络合剂,THF 作为非质子溶剂。优化了影响萃取效率的所有参数,如 pH 值、DES 体积和组成、萃取时间、二硫腙用量等。在最佳条件下,对于 Pb(ii)和 Cd(ii),分别获得了 92 和 57 的增强因子、2.5 μg/L 和 0.75 μg/L 的检出限、7.8 μg/L 和 2.5 μg/L 的定量限、10-250 μg/L 和 2.5-50 μg/L 的线性工作范围。对于 100 μg/L 的 Pb(ii),相对标准偏差(n=10)为 2.7%,对于 25 μg/L 的 Cd(ii),相对标准偏差(n=10)为 2.1%。通过比较基于溶剂的校准曲线和基质匹配的校准曲线,研究了基质效应。成功地在不受样品基质影响的情况下,对染发剂和指甲花样品中的铅和镉进行了测定。所选染发剂和指甲花样品的铅含量在 1.3 至 6.5 μg/g 之间,镉含量在 0.028 至 0.54 μg/g 之间。