摘要
建立了高效液相色谱-串联质谱检测土壤中11种离子液体（ILs）阳离子的分析方法。样品经乙腈＋0．2mol／LNH4Cl提取，Strata-X-CW萃取小柱净化，AgilentSB—C18（1．88μm，2．1mm×50mm）色谱柱分离，以乙腈＋体积分数0．1％的甲酸水溶液为流动相进行梯度洗脱，以电喷雾正离子模式电离，多反应监测模式检测，外标法定量。11种ILs阳离子的质量浓度在2～500ng／mL范围内呈良好线性（r2〉0．995），方法检出限为0．72～1．95ng／g，定量限为2．38～6．44ng／g。以土壤为基质，加标回收率为78．0％-107．6％，相对标准偏差为0．3％～8．6％，11种ILs阳离子在12min内实现基线分离。方法满足土壤样品中ILs阳离子的检测要求。
A high performance liquid chromatography-tandem mass spectrometric method was developed for the determination of eleven ionic liquid cations in soil environmental samples. The samples were extracted with ace- tronitrile ＋ 0. 2 mol/L ammonium chloride （8：2, V/V; pH 3 ） and cleaned up on a Strata-X-CW solid-phase ex- traction column. The target compounds were separated on an AgilentSB-C18 （1.8 μm, 2. 1 mm ×50 mm） chro- matographic column by gradient elution using acetronitrile-water （containing 0. 1% formic acid ） as mobile phase. The ionic liquid cations were determined under the electrospray positive ionization （ ESI ~ ） and multiple reaction monitoring （MRM） mode, and quantified by the matrix-matched external standard method. The calibra- tion curves for eleven ionic liquid cations showed good linearities in the range of 2 -500 ng/mL with correlation coefficients （ r2 ） better than 0. 995. Detection limits （ S/N ≥ 3 ） and quantitation limits （ S/N ≥ 10） were in the range of 0. 72 - 1.95 ng/g and 2. 38 - 6. 44 ng/g, respectively. The recoveries of the eleven ionic liquid cations for soil samples were in the range of 78.0% - 107.6%, with relative standard deviations of 0. 31% - 8.6%. The method was sensitive and accurate, and could meet the requirements for the determination of ionic liquid cat- ions in soil.
出处
《分析试验室》
CAS
CSCD
北大核心
2014年第1期104-108,共5页
Chinese Journal of Analysis Laboratory
