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Determination of ionic liquid cations in soil samples by ultrasound-assisted solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry

机译:超声辅助固相萃取-液相色谱-串联质谱法测定土壤样品中的离子液体阳离子

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Liquid chromatography-tandem mass spectrometry coupled with an ultrasonic-assisted extraction and solid phase extraction procedure has been investigated for the separation and detection of imidazolium, pyridinium, pyrrolidinium, ammonium and phosphonium-based ionic liquid (IL) cations in soil samples. First, the samples were extracted with acetonitrilea€“0.2 mol La?’1 ammonium chloride solution (8:2, v/v; pH 3) using an ultrasonic assisted extraction procedure and then eluted on a Strata-X-CW solid-phase extraction column. The target compounds were effectively separated with an Agilent SB-C18 (1.88 ??m, 3.0 mm ?— 100 mm) chromatographic column by gradient elution, in which acetonitrilea€“water (containing 0.1% formic acid) acted as the mobile phase. The IL cations were determined by electrospray positive ionization (ESI+) combined with multiple reaction monitoring (MRM) mode, and quantified by the matrix-matched external standard method. The limits of detection (LODs) ranged from 0.15 to 2.88 ng ga?’1 and the limits of quantification (LOQs) from 0.50 to 9.50 ng ga?’1. The average recoveries of the twenty-three IL cations in soil samples were in the range of 69.3a€“106.8%, with relative standard deviations of 2.17a€“12.1%. This assay showed greater sensitivity and accuracy, to meet the requirements of the determination of IL cations in soil.
机译:液相色谱-串联质谱结合超声辅助萃取和固相萃取方法已被研究用于分离和检测土壤样品中的咪唑鎓,吡啶鎓,吡咯烷鎓,铵和磷基离子液体(IL)阳离子。首先,使用超声辅助萃取程序,用乙腈“ 0.2 mol La?1”氯化铵溶液(8:2,v / v; pH 3)萃取样品,然后在Strata-X-CW固相上洗脱萃取柱。用Agilent SB-C18(1.88?m,3.0 mm?-100 mm)色谱柱通过梯度洗脱有效分离目标化合物,其中乙腈水(含0.1%甲酸)作为流动相。通过电喷雾正电离(ESI +)结合多反应监测(MRM)模式确定IL阳离子,并通过基质匹配外标方法进行定量。检出限(LOD)为0.15至2.88 ng ga?1,定量限(LOQ)为0.50至9.50 ng ga?1。土壤样品中23种IL阳离子的平均回收率在69.3a€106.8%范围内,相对标准偏差为2.17a€12.1%。该测定法显示出更高的灵敏度和准确性,可以满足测定土壤中IL阳离子的要求。

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