Abstract This study presents a new in-syringe solvent-assisted dispersive solid phase extraction (ISSADSPE) method for determination of nickel ions in water and food. The method involved dispersion of a few milligrams of sorbent in the sample solution inside the barrel of a syringe through application of a disperser solvent. In less than 1 min, the extraction equilibrium was achieved due to dispersion of the sorbent and high mass transfer rate. Afterwards, syringe membrane was employed to separate the dispersed sorbent from the solution. Then the ethanol was withdrawn by syringe membrane to dissolve the analyte-enriched sorbent. Flame atomic absorption spectroscopy was applied to assess the obtained extract. Effective factors such as the sorbent nature and amount, sample volume, pH, ligand concentration, type and volume of disperser solvent and eluent, ionic strength and extraction time were evaluated and optimized to improve the extraction efficiency. Under optimized conditions (pH = 8.0, ligand concentration = 2.0 × 10−4, sorbent = 10 mg of benzophenone, disperser solvent 500 μL of ethanol), the limit of detection and quantification were found to be 0.7 μg L−1 and 2.0 μg L−1, respectively. The calibration curve kept its linearity from 2 to150 μg L−1, with the square correlation coefficient of 0.997. The relative standard deviation was measured as 2.5% while the enrichment factor was assessed as 50. The proposed method was successfully applied for determination of nickel in environmental water, spinach and celery samples, with recovery range of 97–101%.

中文翻译：

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注射器内溶剂辅助分散固相萃取和火焰原子吸收光谱法测定水和食品样品中的镍

摘要 本研究提出了一种新的注射器内溶剂辅助分散固相萃取 (ISSADSPE) 方法，用于测定水和食品中的镍离子。该方法涉及通过应用分散溶剂将几毫克吸附剂分散到注射器筒内的样品溶液中。由于吸附剂的分散和高传质速率，在不到 1 分钟的时间内就达到了萃取平衡。然后，使用注射器膜从溶液中分离分散的吸附剂。然后通过注射器膜抽出乙醇以溶解富含分析物的吸附剂。应用火焰原子吸收光谱来评估获得的提取物。吸附剂的性质和数量、样品体积、pH 值、配体浓度、评估和优化分散溶剂和洗脱液的类型和体积、离子强度和提取时间，以提高提取效率。在优化条件下（pH = 8.0，配体浓度 = 2.0 × 10−4，吸附剂 = 10 mg 二苯甲酮，分散溶剂 500 μL 乙醇），发现检测限和定量限分别为 0.7 μg L-1 和 2.0 μg分别为 L−1。校准曲线在 2 到 150 μg L−1 范围内保持线性，相关系数为 0.997 的平方。相对标准偏差为2.5%，富集因子为50。该方法成功应用于环境水、菠菜和芹菜样品中镍的测定，回收率范围为97-101%。评估和优化离子强度和提取时间以提高提取效率。在优化条件下（pH = 8.0，配体浓度 = 2.0 × 10−4，吸附剂 = 10 mg 二苯甲酮，分散溶剂 500 μL 乙醇），发现检测限和定量限分别为 0.7 μg L-1 和 2.0 μg分别为 L−1。校准曲线在 2 到 150 μg L−1 范围内保持线性，相关系数为 0.997 的平方。相对标准偏差为2.5%，富集因子为50。该方法成功应用于环境水、菠菜和芹菜样品中镍的测定，回收率范围为97-101%。评估和优化离子强度和提取时间以提高提取效率。在优化条件下（pH = 8.0，配体浓度 = 2.0 × 10−4，吸附剂 = 10 mg 二苯甲酮，分散溶剂 500 μL 乙醇），发现检测限和定量限分别为 0.7 μg L-1 和 2.0 μg分别为 L−1。校准曲线在 2 到 150 μg L−1 范围内保持线性，相关系数为 0.997 的平方。相对标准偏差为2.5%，富集因子为50。该方法成功应用于环境水、菠菜和芹菜样品中镍的测定，回收率范围为97-101%。分散溶剂（500 μL 乙醇），检测限和定量限分别为 0.7 μg L-1 和 2.0 μg L-1。校准曲线在 2 到 150 μg L−1 范围内保持线性，相关系数为 0.997 的平方。相对标准偏差为2.5%，富集因子为50。该方法成功应用于环境水、菠菜和芹菜样品中镍的测定，回收率范围为97-101%。分散溶剂（500 μL 乙醇），检测限和定量限分别为 0.7 μg L-1 和 2.0 μg L-1。校准曲线在 2 到 150 μg L-1 范围内保持线性，相关系数为 0.997 的平方。相对标准偏差为2.5%，富集因子为50。该方法成功应用于环境水、菠菜和芹菜样品中镍的测定，回收率范围为97-101%。