多壁碳纳米管固相萃取-高效液相色谱法测定水中三唑酮
HPLC Determination of Triadimefon in Water with Solid Phase Extraction Using Multiwall Carbon Nano-tubes as Adsorbent
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摘要: 提出了用多壁碳纳米管(MWCNT′s)作吸附剂的固相萃取法(SPE)富集水样中残留的三唑酮,并用高效液相色谱法测定其含量。取一定体积的水样以4 mL·min-1流量通过用MWCNT′s填充的SPE柱,用二氯甲烷作洗脱剂洗脱吸附在柱上的三唑酮。洗脱液用氮吹蒸干后溶于1.0 mL甲醇-水(70+30)混合液中,用C18色谱柱作固定相,用甲醇-水(70+30)混合液作流动相进行分离,在波长225 nm处进行紫外检测。三唑酮的质量浓度在1.0~50.0 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为0.3 μg·L-1。在2个浓度水平上对方法做回收试验,测得回收率在95.0%~104%之间。Abstract: Multiwall carbon nano-bubes (MWCNT′s) was used as adsorbent in the solid phase extraction (SPE) for enrichment of residual triadimefon in water sample, and the enriched analyte was determined by HPLC. A definite volume of water sample was taken and passed through SPE column packed with MWCNT′s at a flow-rate of 4 mL·min-1. Dichloromethane was used as eluant to desorb triadimefon from the column, and the eluate obtained was evaporate to dryness by N2-blowing. The residue was dissolved and made up to 1.0 mL with the mobile phase. Chromatographic separation was made by using C18-column as stationary phase and mixture of CH3OH-H2O (70+30) as mobile phase. Linear relationship between values of peak area and mass concentration of triadimefon was obtained in the range of 1.0~50.0 μg·L-1, with detection limit (3S/N) of 0.3 μg·L-1. Recovery was tested at 2 concentration levels, giving results of recovery ranged from 95.0% to 104%.