Department of Civil & Mineral Engineering, University of Toronto, 35 St. George Street, Toronto, Ontario, M5S 1A4, Canada.
Department of Civil & Mineral Engineering, University of Toronto, 35 St. George Street, Toronto, Ontario, M5S 1A4, Canada.
Talanta. 2022 Apr 1;240:123170. doi: 10.1016/j.talanta.2021.123170. Epub 2021 Dec 29.
Frequent use of persulfates as oxidants, for in situ chemical oxidation and advanced oxidation processes, warrants the need for developing a fast and efficient method for measuring persulfate concentrations in aqueous samples in the lab and on site. Here, we propose a modified method, based on Liang et al.'s (2008) spectrophotometric method, for measuring both peroxydisulfate (PDS) and peroxymonosulfate (PMS) in the aqueous samples. Our method involves a deep 96-well plate, multi-channel pipettes, a small orbital shaker, and a microplate reader; allowing the preparation and analysis of up to 96 samples in one run. Our proposed method shortens the time by 10 folds, consumes only ∼2% of the original reagents, and generates only ∼2% of the liquid waste compared to the Liang et al.'s method, thus, making our method high-throughput, time-efficient, and cost-effective with reduced environmental impact. The presented microplate reader method is validated in terms of linearity, LOD, LOQ, accuracy, precision, robustness, and selectivity. All the parameters satisfied the acceptance criteria, according to ICH guidelines. The linearity of calibration curves was evaluated by performing the F-test. In general, our method has linear ranges from 20 to 42,000 and 5 to 40,960 μM for PDS and PMS, respectively. Accuracy (% recovery) results suggested that the LOD and LOQ based on the standard deviation of y-intercepts of the regression lines were the most reliable. The LOD/LOQ values for PDS and PMS were 14.7/44.1 and 4.6/14.4 μM, respectively. The proposed method was also modified to work with a standard cuvette spectrophotometer and was validated. A comparison with the UHPLC analysis of PDS showed that our microplate reader method performed equivalently or even outperformed the UHPLC method, in the presence of common groundwater constituents and organic contaminants.
过硫酸盐作为氧化剂在原位化学氧化和高级氧化过程中被频繁使用，这就需要开发一种快速、高效的方法来测量实验室和现场水样中的过硫酸盐浓度。在这里，我们在 Liang 等人（2008 年）分光光度法的基础上提出了一种改进的方法，用于测量水样中的过一硫酸盐（PDS）和过氧单硫酸盐（PMS）。我们的方法涉及深 96 孔板、多通道移液器、小型轨道振荡器和微孔板读数器；允许在一次运行中制备和分析多达 96 个样品。与 Liang 等人的方法相比，我们提出的方法缩短了 10 倍的时间，仅消耗约 2%的原始试剂，产生的废液量仅为 2%，因此，我们的方法具有高通量、高效、节省成本和减少环境影响的特点。提出的微孔板读取器方法在线性度、LOD、LOQ、准确度、精密度、稳健性和选择性方面进行了验证。根据 ICH 指南，所有参数均满足验收标准。通过进行 F 检验评估校准曲线的线性度。一般来说，我们的方法对 PDS 和 PMS 的线性范围分别为 20 至 42000 和 5 至 40960μM。准确度（%回收率）结果表明，基于回归线 y 截距标准偏差的 LOD 和 LOQ 是最可靠的。PDS 和 PMS 的 LOD/LOQ 值分别为 14.7/44.1 和 4.6/14.4μM。该方法还经过修改，可与标准比色皿分光光度计一起使用并进行验证。与 PDS 的 UHPLC 分析进行比较表明，在常见地下水成分和有机污染物存在的情况下，我们的微孔板读取器方法的性能与 UHPLC 方法相当，甚至优于 UHPLC 方法。
