Abstract
For the determination of salicylaldoxime in environmental water samples, a stable and rapid method with low detection was proposed and established, based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector. Parameters including extraction solvent, ionic strength, solution pH, and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water. When the described method was applied to four spiked water samples, the obtained average extraction recovery rate was found between 87%–107% and relative standard deviation was below 6%. At the same time, good linear relationships were observed for spiked water samples from 0.01 to 10 μg/mL (R2=0.9993). In addition, the detection limit of salicylaldoxime was revealed between 0.003–0.008 μg/mL, which is two orders of magnitude lower than previously reported results. Thus, the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.
摘要
水杨醛肟是一种高效、高选择性的萃取剂,广泛应用于氧化铜矿冶炼过程、生物制药工业与有 机分析方面。为评估其对环境的影响,需对环境水体中水杨醛肟进行定量检测。本文基于液-液萃取–高效液相色谱(LLE-HPLC-UV)进行水样中水杨醛肟的定量分析,分别对萃取剂种类和体积、离子 强度、pH 值及萃取混合方式(涡旋、水浴与超声辅助萃取)进行了优化。最终在5 mL 甲苯作为萃取 剂,NaCl 含量30%(w/v),pH 稳定在7 的条件下涡旋萃取2 min,得到较高萃取率。水杨醛肟加标 水样在0.01~10 μg/mL 浓度范围内,呈现良好线性(R2=0.9993)。该方法检出限为0.003~0.008 μg /mL, 比已有文献报导的降低两个数量级。对4 种不同基质的水体进行加标回收实验,回收率为87%~107%, 相对标准偏差均低于6%。说明该方法可实现水环境中对于水杨醛肟快速、稳定且高效的检测。
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Foundation item: Project(201309052) supported by the National Special Fund for Scientific Research in the Public Interest; Project(2013FJ2003) supported by the Science and Technology Planning Project of Hunan Province of China
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Kong, Q., Bai, Xz., Lin, Hj. et al. Improved determination of salicylaldoxime in water samples by liquid-liquid extraction followed by high performance liquid chromatographic analysis. J. Cent. South Univ. 25, 701–708 (2018). https://doi.org/10.1007/s11771-018-3774-z
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DOI: https://doi.org/10.1007/s11771-018-3774-z