首页> 中文期刊> 《分析测试学报》 >固相萃取/高效液相色谱法同时测定水中4种直链烷基苯磺酸钠

固相萃取/高效液相色谱法同时测定水中4种直链烷基苯磺酸钠

     

摘要

A solid phase extraction coupled with high performance liquid chromatographic (SPE/HPLC) method was established for the determination of 4 kinds of sodium n-alkyl benzene sulfonates in water. The samples were refrigerated and centrifuged, then purified and enriched with MAX complex anion exchange column. Four sodium n-alkyl benzene sulfonates were successfully separated by HPLC using acetonitrile - 100 mmol/L ammonium acetate (73 : 27, by volume) as mobile phase with a flow rate of 1 mL/min, column temperature of 30 ℃, detection wavelength of 225 nm and injection volume of 10 μL. Under the optimal conditions, the calibration curves were linear in the range of 10 -50 mg/L for sodium undecylbenzene sulfonte and sodium N-tridecylbenzene sulfonate with detection limits of 10 mg/L, and 5 -25 mg/L for sodium dodecylbenzene sulphonate and sodium tetradecylbenzene sulfonate with detection limits of 5 mg/L. The spiked recoveries were in the range of 86% -98% with relative standard deviations(RSDs) of 2. 9% -7.4%.%建立了水中4种直链烷基苯磺酸钠的固相萃取/高效液相色谱的测定方法.样品经高速冷冻离心,用MAX复合阴离子交换小柱净化富集后直接进样.在以乙腈-100 mmol/L乙酸铵(体积比73:27)为流动相,流速1 mL/min,柱温30 ℃,检测波长225 nm,进样体积10 μL的条件下,4种直链烷基苯磺酸钠得到很好的分离.在优化实验条件下,十一烷基苯磺酸钠与十三烷基苯磺酸钠的线性范围为10~50 mg/L,检出限为10 mg/L,十二烷基苯磺酸钠与十四烷基苯磺酸钠的线性范围为5~25 mg/L,检出限为5 mg/L;加标回收率为86%~98%;相对标准偏差为2.9%~7.4%.

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