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Application of syringe to syringe dispersive micro-solid phase extraction using a magnetic layered double hydroxide for the determination of cadmium(ii) and lead(ii) ions in food and water samples†
Analytical Methods ( IF 2.7 ) Pub Date : 2018-01-29 00:00:00 , DOI: 10.1039/c7ay01857f Somayeh Arghavani-Beydokhti 1, 2, 3, 4 , Maryam Rajabi 1, 2, 3, 4 , Alireza Asghari 1, 2, 3, 4
Analytical Methods ( IF 2.7 ) Pub Date : 2018-01-29 00:00:00 , DOI: 10.1039/c7ay01857f Somayeh Arghavani-Beydokhti 1, 2, 3, 4 , Maryam Rajabi 1, 2, 3, 4 , Alireza Asghari 1, 2, 3, 4
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In this research work, for the first time, a new mode of dispersive solid-phase extraction named syringe to syringe magnetic dispersive micro-solid phase extraction is introduced as an efficient, simple, rapid, and eco-friendly sample extraction method. A nickel–aluminum layered double hydroxide coated on magnetic nanoparticles (Fe3O4@Ni–Al–CO3-LDH), as an efficient nanosorbent, was synthesized and successfully applied for the concurrent extraction of trace amounts of Cd2+ and Pb2+ ions in food and water samples prior to their determination using a microsampling-flame atomic absorption spectrometry technique. After extraction and magnetic separation, the elution step was easily performed through dissolving the magnetic layered double hydroxide (LDH) containing the target analytes in an acidic solution. Also the use of a magnetic LDH overcomes the difficulty of phase separation that decreases the extraction time. The optimum conditions efficiently evaluated via the response surface methodology (RSM) were pH 7.0, 13.7 mg of the nanosorbent, 16 extraction cycles, 125 μL of 3.8 mol L−1 trifluoroacetic acid, and an ultrasonic time of 75 s. According to the optimum conditions obtained in above, good linear ranges (0.75–35 ng mL−1 for Cd2+ ions and 4.0–370 ng mL−1 for Pb2+ ions) with coefficient of determination (R2) values higher than 0.995 were obtained. The limits of detection were found to be 0.25 and 1.0 ng mL−1 for Cd2+ and Pb2+, respectively. The preconcentration factor for the target analytes was 80 in a 10 mL sample solution. The obtained results indicated the high quality of the developed procedure for the much-needed quantification of the aforementioned metal ions in food and water samples.
中文翻译：
注射器中的应用使用磁性层状双氢氧化物为镉决心注射器分散微固相萃取（II）和铅（II）离子的食物和水样中†
在这项研究工作中，首次引入了一种称为注射器到注射器的磁性分散微固相萃取的新型分散固相萃取模式，作为一种高效，简单，快速且环保的样品萃取方法。合成了一种包覆在磁性纳米粒子上的镍铝层状双氢氧化物（Fe 3 O 4 @ Ni–Al–CO 3 -LDH），作为一种有效的纳米吸附剂，成功地用于同时萃取痕量的Cd 2+和Pb 2+使用微量进样火焰原子吸收光谱法测定食品和水样品中的离子之前，需先进行测定。萃取和磁分离后，通过将含有目标分析物的磁性层状双氢氧化物（LDH）溶解在酸性溶液中，可以轻松进行洗脱步骤。磁性LDH的使用也克服了相分离的困难，这减少了提取时间。通过响应表面方法（RSM）有效评估的最佳条件是pH 7.0、13.7 mg纳米吸附剂，16个萃取循环，125μL3.8 mol L -1三氟乙酸和75 s的超声时间。根据上面获得的最佳条件，良好的线性范围（Cd为0.75–35 ng mL -1获得了2+离子和Pb 2+离子为4.0–370 ng mL -1），测定系数（ R 2）值高于0.995。发现Cd 2+和Pb 2+的检出限分别为0.25和1.0 ng mL -1。在10 mL样品溶液中目标分析物的预浓缩系数为80。所获得的结果表明，所开发程序的质量很高，可用于食品和水样中上述金属离子的急需定量。
更新日期：2018-01-29
中文翻译：
注射器中的应用使用磁性层状双氢氧化物为镉决心注射器分散微固相萃取（II）和铅（II）离子的食物和水样中†
在这项研究工作中，首次引入了一种称为注射器到注射器的磁性分散微固相萃取的新型分散固相萃取模式，作为一种高效，简单，快速且环保的样品萃取方法。合成了一种包覆在磁性纳米粒子上的镍铝层状双氢氧化物（Fe 3 O 4 @ Ni–Al–CO 3 -LDH），作为一种有效的纳米吸附剂，成功地用于同时萃取痕量的Cd 2+和Pb 2+使用微量进样火焰原子吸收光谱法测定食品和水样品中的离子之前，需先进行测定。萃取和磁分离后，通过将含有目标分析物的磁性层状双氢氧化物（LDH）溶解在酸性溶液中，可以轻松进行洗脱步骤。磁性LDH的使用也克服了相分离的困难，这减少了提取时间。通过响应表面方法（RSM）有效评估的最佳条件是pH 7.0、13.7 mg纳米吸附剂，16个萃取循环，125μL3.8 mol L -1三氟乙酸和75 s的超声时间。根据上面获得的最佳条件，良好的线性范围（Cd为0.75–35 ng mL -1获得了2+离子和Pb 2+离子为4.0–370 ng mL -1），测定系数（ R 2）值高于0.995。发现Cd 2+和Pb 2+的检出限分别为0.25和1.0 ng mL -1。在10 mL样品溶液中目标分析物的预浓缩系数为80。所获得的结果表明，所开发程序的质量很高，可用于食品和水样中上述金属离子的急需定量。
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