Sánchez-Ponce Lorena, Casanueva-Marenco María José, Díaz-de-Alba Margarita, Galindo-Riaño María Dolores, Granado-Castro María Dolores
Department of Analytical Chemistry, Institute of Biomolecules (INBIO), Faculty of Sciences, International Campus of Excellence of the Sea (CEI-MAR), University of Cadiz, Campus Rio San Pedro, Puerto Real, 11510 Cadiz, Spain.
Polymers (Basel). 2023 Oct 14;15(20):4082. doi: 10.3390/polym15204082.
The design, characterization, and analytical application of a green optical sensor for the selective determination of Fe(II) ions is proposed. The sensor is based on the immobilization of the chromogenic reagent picolinaldehyde salicyloylhydrazone (SHPA) within a polymer inclusion membrane. To reduce solvent usage, the reagent was synthesized using a green mechanochemical procedure. The components for sensor preparation were optimized with a sequential simplex method and the optimal composition was found to be 0.59 g cellulose triacetate (base polymer), 0.04 g SHPA (chemosensor reagent), 4.9 mL dibutyl phthalate (plasticizer), and 38 mL dichloromethane (solvent). The conditions of iron analysis were also optimized resulting in pH 6 for aqueous solution, 90 min exposure time and 10 min short-term stability. The optical sensor showed a linear range from the limit of detection (0.48 µmol L) to 54 µmol L Fe(II). The precision of the method was found to be 1.44% and 1.19% for 17.9 and 45 µmol L Fe(II), respectively. The characteristics of the sensor allowed the design of a Fe(II)/Fe(III) speciation scheme. The methodology was successfully applied to the determination of iron in food preservatives, food additives, and dietary supplement. Additionally, the Fe speciation scheme was successfully applied to an agricultural fertilizer.
本文提出了一种用于选择性测定Fe(II)离子的绿色光学传感器的设计、表征及分析应用。该传感器基于将显色试剂吡啶甲醛水杨酰腙(SHPA)固定在聚合物包容膜内。为减少溶剂使用,采用绿色机械化学方法合成了该试剂。用序贯单纯形法对传感器制备的组分进行了优化,发现最佳组成为0.59 g三醋酸纤维素(基础聚合物)、0.04 g SHPA(化学传感器试剂)、4.9 mL邻苯二甲酸二丁酯(增塑剂)和38 mL二氯甲烷(溶剂)。还对铁分析条件进行了优化,得到水溶液pH为6、暴露时间90 min和短期稳定性为10 min。该光学传感器对Fe(II)的线性范围为检测限(0.48 µmol/L)至54 µmol/L。该方法对17.9和45 µmol/L Fe(II)的精密度分别为1.44%和1.19%。该传感器的特性有助于设计Fe(II)/Fe(III)形态分析方案。该方法成功应用于食品防腐剂、食品添加剂和膳食补充剂中铁的测定。此外,Fe形态分析方案成功应用于一种农用肥料。