Heilongjiang Province Key Laboratory of Photochemical Biomaterials and Energy Storage Materials, College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin, P. R. China.
J Sep Sci. 2019 May;42(9):1733-1739. doi: 10.1002/jssc.201801277. Epub 2019 Mar 20.
An analytical method was developed for the simultaneous determination of thiocyanate and iodide by reversed-phase liquid chromatography with UV detection using imidazolium ionic liquids as mobile phase additives. The chromatographic behaviors of the two anions on a C column were studied and compared with four types of reagents including imidazolium ionic liquids, pyridinium ionic liquids, 4-aminophenol hydrochloride and tetrabutylammonium as mobile phase additives. The effects of the concentrations of imidazolium ionic liquids, organic solvents and detection wavelength on separation and detection of the anions were investigated. The role of ionic liquids, retention rules and mechanisms were discussed. The separation of the anions was performed on the C reserved-phase column using acetonitrile-0.3 mmol/L 1-amyl-3-methylimidazolium tetrafluoroborate (10:90, v/v) as mobile phase, with column temperature of 35°C, flow rate of 1 mL/min and detection wavelength of 210 nm. Under these conditions, the two anions can be completely separated within 6 min. The limits of detection were 0.05 mg/L. The method was applied for the determination of thiocyanate and iodide in ionic liquid samples and iodide drugs, and the spiked recoveries ranged from 97 to 101%. The method is simple, accurate and meets the requirements of quantitative analysis for thiocyanate and iodide.
建立了一种用反相液相色谱-紫外检测法同时测定硫氰酸盐和碘化物的分析方法,使用咪唑鎓离子液体作为流动相添加剂。研究了两种阴离子在 C 柱上的色谱行为,并与四种试剂(包括咪唑鎓离子液体、吡啶鎓离子液体、4-氨基酚盐酸盐和四丁基铵)进行了比较,作为流动相添加剂。考察了离子液体浓度、有机溶剂和检测波长对阴离子分离和检测的影响。讨论了离子液体的作用、保留规律和机制。在 35°C 柱温、1 mL/min 流速和 210nm 检测波长下,用乙腈-0.3mmol/L 1-戊基-3-甲基咪唑四氟硼酸盐(10:90,v/v)作为流动相,在 C 保留相柱上分离两种阴离子,6min 内可完全分离。两种阴离子的检出限均为 0.05mg/L。该方法用于离子液体样品和碘化物药物中硫氰酸盐和碘化物的测定,加标回收率在 97%~101%之间。该方法简单、准确,满足硫氰酸盐和碘化物定量分析的要求。