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Development of Method Based on Dispersive Liquid-Liquid Microextraction Air-Assisted for Multi-Element Determination of Cadmium and Manganese in Sugarcane Spirit (Brazilian cachaça ) by FAAS
Food Analytical Methods ( IF 2.9 ) Pub Date : 2019-07-23 , DOI: 10.1007/s12161-019-01600-w Adrielle S. Fontes , Julia C. Romero , Leonardo B. Guimarães , Erik G. P. da Silva , Daniel de C. Lima , Fábio Alan C. Amorim
Food Analytical Methods ( IF 2.9 ) Pub Date : 2019-07-23 , DOI: 10.1007/s12161-019-01600-w Adrielle S. Fontes , Julia C. Romero , Leonardo B. Guimarães , Erik G. P. da Silva , Daniel de C. Lima , Fábio Alan C. Amorim
In this work, a new method was developed for multi-element determination of Cd and Mn in samples of sugarcane spirit (cachaça) by FAAS using the air-assisted dispersive liquid-liquid microextraction (AA-DLLME). After univariate and multivariate optimizations (mixture design), the experimental conditions were as follows: 5.2 mL of sample at pH 8.5, 0.7 mL 10% (w/v) NaCl solution, 120 μL of trichlorethylene (extraction solvent) containing 1-(2-pyridylazo)-2-naphthol (PAN) at 0.05% (w/v) as chelating agent, six cycles of stirring the mixture with a glass syringe, and 3 min of centrifugation. In these conditions, the calibration curve obtained for Cd was Abs = 0.0158CCd + 0.0333, with R2 0.9951 and for Mn was Abs = 0.0011CMn + 0.0142 and R2 0.9911. The limits of detection, enrichment factor, and consumption index were, respectively, 0.51 μg L−1, 79 and 0.07 mL for Cd, and 1.64 μg L−1, 18, and 0.28 mL for Mn. Precision was evaluated at concentrations of 5 and 10 μg L−1, and RSD% (N = 10) was 0.97% and 6.6% for Cd and 2.8% and 4.5% for Mn, respectively. Addition and recovery tests in samples of Brazilian cachaça were performed to evaluate the accuracy, and recoveries were 87% to 120%, with concentrations found between 1.20 and 3.05 μg L−1 for Cd and between 6.98 and 14.4 μg L−1 for Mn. The developed method proved to be sensitive, efficient, simple, fast, and having low reagent consumption, and of applicability not previously reported in the literature.
中文翻译:
FAAS基于分散液微萃取空气辅助测定甘蔗精神中巴西镉和锰的方法的开发
在这项工作中,开发了一种新的方法,采用空气辅助分散液-液微萃取(AA-DLLME),通过火焰原子吸收光谱法(FAAS)对甘蔗精油(cachaça)样品中的镉和锰进行多元素测定。经过单变量和多变量优化(混合物设计)后,实验条件如下:5.2 mL pH 8.5的样品,0.7 mL 10%(w / v)NaCl溶液,120μL含1-(2)的三氯乙烯(萃取溶剂) -吡啶偶氮)-2-萘酚(PAN)(0.05%(w / v))作为螯合剂,用玻璃注射器搅拌混合物六个周期,并离心3分钟。在这些条件下,Cd的校准曲线为Abs = 0.0158C Cd + 0.0333,R 2为0.9951,Mn为Abs = 0.0011C Mn + 0.0142和R 2为0.9911。检测,富集因子,和消耗指数的范围分别为0.51微克大号-1,79和0.07 mL的Cd和1.64微克大号-1,18和0.28 mL的锰。在5和10μgL -1的浓度下评估精密度 ,镉的RSD%(N = 10)为0.97%,镉的RSD%为6.6%,锰的RSD %为2.8%,4.5%。在巴西干酪样品中进行了添加和回收测试以评估准确性,回收率在87%至120%之间,镉的浓度在1.20至3.05μgL -1之间,而Cd在6.98至14.4μgL之间。Mn为-1。事实证明,所开发的方法灵敏,高效,简单,快速,试剂消耗低,并且以前没有文献报道其适用性。
更新日期:2020-01-17
中文翻译:
FAAS基于分散液微萃取空气辅助测定甘蔗精神中巴西镉和锰的方法的开发
在这项工作中,开发了一种新的方法,采用空气辅助分散液-液微萃取(AA-DLLME),通过火焰原子吸收光谱法(FAAS)对甘蔗精油(cachaça)样品中的镉和锰进行多元素测定。经过单变量和多变量优化(混合物设计)后,实验条件如下:5.2 mL pH 8.5的样品,0.7 mL 10%(w / v)NaCl溶液,120μL含1-(2)的三氯乙烯(萃取溶剂) -吡啶偶氮)-2-萘酚(PAN)(0.05%(w / v))作为螯合剂,用玻璃注射器搅拌混合物六个周期,并离心3分钟。在这些条件下,Cd的校准曲线为Abs = 0.0158C Cd + 0.0333,R 2为0.9951,Mn为Abs = 0.0011C Mn + 0.0142和R 2为0.9911。检测,富集因子,和消耗指数的范围分别为0.51微克大号-1,79和0.07 mL的Cd和1.64微克大号-1,18和0.28 mL的锰。在5和10μgL -1的浓度下评估精密度 ,镉的RSD%(N = 10)为0.97%,镉的RSD%为6.6%,锰的RSD %为2.8%,4.5%。在巴西干酪样品中进行了添加和回收测试以评估准确性,回收率在87%至120%之间,镉的浓度在1.20至3.05μgL -1之间,而Cd在6.98至14.4μgL之间。Mn为-1。事实证明,所开发的方法灵敏,高效,简单,快速,试剂消耗低,并且以前没有文献报道其适用性。