Department of Marine Chemistry, Faculty of Marine Science, Khorramshahr University of Marine Science and Technology, Khorramshahr, Iran.
Anal Chim Acta. 2013 Jan 31;762:61-7. doi: 10.1016/j.aca.2012.11.054. Epub 2012 Dec 5.
A novel and efficient digestion method based on choline chloride-oxalic acid (ChCl-Ox) deep eutectic solvent (DES) was developed for flame atomic absorption spectrometry (FAAS) determination of Cu, Zn, and Fe in biological fish samples. Key parameters that influence analyte recovery were investigated and optimized, using the fish protein certified reference material (CRM, DORM-3) throughout the procedure. In this method, 100 mg of the sample was dissolved in ChCl-Ox (1:2, molar ratio) at 100°C for 45 min. Then, 5.0 mL HNO(3) (1.0 M) was added. After centrifugation, the supernatant solution was filtered, diluted to a known volume, and analyzed by FAAS. Under optimized conditions, an excellent agreement between the obtained results and the certified values was observed, using Student's t-test (P=0.05); the extraction recovery of the all elements was greater than 95.3%. The proposed method was successfully applied to the determination of analytes in different tissues (muscle, liver, and gills) having a broad concentration range in a marine fish sample. The reproducibility of the method was validated by analyzing all samples by our method in a different laboratory, using inductively coupled plasma optical emission spectrometry (ICP-OES). For comparison, a conventional acid digestion (CAD) method was also used for the determination of analytes in all studied samples. The simplicity of the proposed experimental procedure, high extraction efficiency, short analysis time, lack of concentrated acids and oxidizing agents, and the use of safe and inexpensive components demonstrate the high potential of ChCl-Ox (1:2) for routine trace metal analysis in biological samples.
一种新颖高效的基于氯化胆碱-草酸(ChCl-Ox)深共晶溶剂(DES)的消解方法,用于火焰原子吸收光谱法(FAAS)测定生物鱼样中的 Cu、Zn 和 Fe。在整个过程中,使用鱼蛋白标准参考物质(CRM,DORM-3)研究和优化了影响分析物回收率的关键参数。在该方法中,将 100mg 样品溶解在 ChCl-Ox(1:2,摩尔比)中,在 100°C 下加热 45min。然后加入 5.0mL HNO(3)(1.0M)。离心后,将上清液过滤,稀释至已知体积,并用 FAAS 分析。在优化条件下,用学生 t 检验(P=0.05)观察到获得的结果与认证值之间非常吻合;所有元素的提取回收率均大于 95.3%。该方法成功应用于海洋鱼类样品中不同组织(肌肉、肝脏和鳃)中具有较宽浓度范围的分析物的测定。通过在不同实验室用我们的方法分析所有样品,验证了该方法的重现性,使用电感耦合等离子体发射光谱法(ICP-OES)。为了比较,还使用了常规酸消解(CAD)方法测定所有研究样品中的分析物。该实验方法简单、提取效率高、分析时间短、不使用浓酸和氧化剂,以及使用安全廉价的成分,证明了 ChCl-Ox(1:2)在生物样品中常规痕量金属分析中的高潜力。