分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2014年
9期
1026-1031
,共6页
高效液相色谱法%间接紫外检测%烷基磺酸盐%咪唑离子液体
高效液相色譜法%間接紫外檢測%烷基磺痠鹽%咪唑離子液體
고효액상색보법%간접자외검측%완기광산염%미서리자액체
high performance liquid chromatography%indirect ultraviolet detection%alkyl sulfonates%imidazolium ionic liquids
建立了以咪唑离子液体为背景紫外吸收试剂间接检测无紫外光吸收的烷基磺酸盐的高效液相色谱法。该方法采用反相C18色谱柱,以咪唑离子液体-有机溶剂为流动相,实现了2种烷基磺酸盐的分离和检测。研究了检测波长、有机溶剂和咪唑离子液体种类、浓度、pH值等因素对分离和测定的影响,探讨了保留规律,优化了色谱条件。结果表明,在柱温30℃,流速1.0 mL/min,检测波长210 nm,以0.7 mmol/L 1-乙基-3-甲基咪唑四氟硼酸盐水溶液(2 mmol/L磷酸二氢钠-磷酸调至pH 3.0)-甲醇(55:45)作为流动相,戊烷磺酸钠和庚烷磺酸钠可在10 min内完全分离,线性范围分别为0.8~200 mg/L和2.5~200 mg/L,线性系数均达到0.999以上,检出限分别为0.24,0.75 mg/L。将方法应用于环境水样的测定,加标回收率为98.3%~99.1%,相对标准偏差小于1.5%。该方法准确、可靠,可以满足定量分析的要求。
建立瞭以咪唑離子液體為揹景紫外吸收試劑間接檢測無紫外光吸收的烷基磺痠鹽的高效液相色譜法。該方法採用反相C18色譜柱,以咪唑離子液體-有機溶劑為流動相,實現瞭2種烷基磺痠鹽的分離和檢測。研究瞭檢測波長、有機溶劑和咪唑離子液體種類、濃度、pH值等因素對分離和測定的影響,探討瞭保留規律,優化瞭色譜條件。結果錶明,在柱溫30℃,流速1.0 mL/min,檢測波長210 nm,以0.7 mmol/L 1-乙基-3-甲基咪唑四氟硼痠鹽水溶液(2 mmol/L燐痠二氫鈉-燐痠調至pH 3.0)-甲醇(55:45)作為流動相,戊烷磺痠鈉和庚烷磺痠鈉可在10 min內完全分離,線性範圍分彆為0.8~200 mg/L和2.5~200 mg/L,線性繫數均達到0.999以上,檢齣限分彆為0.24,0.75 mg/L。將方法應用于環境水樣的測定,加標迴收率為98.3%~99.1%,相對標準偏差小于1.5%。該方法準確、可靠,可以滿足定量分析的要求。
건립료이미서리자액체위배경자외흡수시제간접검측무자외광흡수적완기광산염적고효액상색보법。해방법채용반상C18색보주,이미서리자액체-유궤용제위류동상,실현료2충완기광산염적분리화검측。연구료검측파장、유궤용제화미서리자액체충류、농도、pH치등인소대분리화측정적영향,탐토료보류규률,우화료색보조건。결과표명,재주온30℃,류속1.0 mL/min,검측파장210 nm,이0.7 mmol/L 1-을기-3-갑기미서사불붕산염수용액(2 mmol/L린산이경납-린산조지pH 3.0)-갑순(55:45)작위류동상,무완광산납화경완광산납가재10 min내완전분리,선성범위분별위0.8~200 mg/L화2.5~200 mg/L,선성계수균체도0.999이상,검출한분별위0.24,0.75 mg/L。장방법응용우배경수양적측정,가표회수솔위98.3%~99.1%,상대표준편차소우1.5%。해방법준학、가고,가이만족정량분석적요구。
A novel analytical method was developed for the determination of alkyl sulfonates by high performance liquid chromatography -indirect ultraviolet detection using imidazolium ionic liquid as the background ultraviolet absorption reagent without ultraviolet absorption. Chromatographic separa-tion was performed on a reversed-phase C18 column using imidazolium ionic liquid-organic solvent as mobile phase. Effects of detection wavelength,kinds and concentrations of organic solvents and imi-dazolium ionic liquids,and other parameters on the separation and determination of alkyl sulfonates were investigated. The retention rules of the alkyl sulfonates under different chromatographic condi-tions were discussed and the chromatographic conditions were optimized. The successful separation and detection of two alkyl sulfonates( sodium pentanesulfonate and sodium heptanesulfonate)were a-chieved using the optimized mobile phase of 0. 7 mmol/L 1-ethyl-3-methyl-imidazolium tetrafluorobo-rate( pH 3. 0 , adjusted with 2 mmol/L monosodium phosphate - phosphoric acid )- methanol (55 : 45)at a flow rate of 1. 0 mL/min,a detection wavelength of 210 nm and a column temperature of 30 ℃. Under the optimal conditions,two alkyl sulfonates could be successfully separated in 10 min. The calibration curves showed good linearities in the ranges of 0. 8-200 mg/L and 2. 5-200 mg/L for two alkyl sulfonates,respectively,with correlation coefficients above 0. 999. The detection limits of two alkyl sulfonates were 0. 24 mg/L and 0. 75 mg/L,respectively. The method was applied in the determination of environmental water samples,with spiked recoveries of 98. 3% -99. 1% and relative standard deviations less than 1. 5% . The method was simple,accurate and reliable,and could meet the requirements for quantitative analysis.