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    丹磺酰肼衍生-高效液相色谱-荧光检测器法测定水中痕量3-羟基丙醛

    Determination of Trace of 3-Hydroxypropanal in Water by High Performance Liquid Chromatography Combined with Fluorescence Detector after Derivatization with Dansulfonyl Hydrazine

    • 摘要: 提出了丹磺酰肼衍生-高效液相色谱-荧光检测器法测定水中痕量3-羟基丙醛(3-HPA)的方法。将1.0 g水样、2.0 mL含200 mg·L-1丹磺酰肼的乙腈溶液、1.0 mL 3.0%(体积分数)乙酸溶液混合,再用乙腈定容至50 mL,于40 ℃衍生反应30 min。以Agilent Eclipse Plus C18色谱柱为固定相,以不同体积比的乙腈-0.10%(质量分数)七氟丁酸溶液的混合溶液为流动相进行梯度洗脱,采用荧光检测器测定。结果表明:衍生试剂丹磺酰肼与3-HPA衍生物在20 min内可实现基线分离;3-HPA的质量浓度在7.6~380.0 μg·L-1内与衍生物的峰面积呈线性关系,检出限(3S/N)为1.1 μg·L-1;方法用于实际水样分析,测定值的相对标准偏差(n=6)为0.71%,3-HPA的加标回收率为98.0%~102%。

       

      Abstract: A method for the determination of trace of 3-hydroxypropanal (3-HPA) in water by high performance liquid chromatography combined with fluorescence detector after derivatization with dansulfonyl hydrazine was proposed. The water sample (1.0 g) was mixed with 2.0 mL of acetonitrile solution containing 200 mg·L-1 dansulfonyl hydrazine and 1.0 mL 3.0% (volume fraction) acetic acid solution, and its volume was made up to 50 mL with acetonitrile. Then the mixed solution was derived at 40 ℃ for 30 min. Agilent Eclipse Plus C18 column was used as the stationary phase, and gradient elution was performed with the mixtures of acetonitrile and 0.10% (mass fraction) perfluorobutanoic acid solution at different volume ratios as the mobile phase, with fluorescence detector for determination. It was shown that derivatization reagent dansulfonyl hydrazine and 3-HPA derivative could be separated at baseline within 20 min, and linear relationship between the mass concentration of 3-HPA and the peak area of derivative was kept in the range of 7.6-380.0 μg·L-1, with detection limit (3S/N) of 1.1 μg·L-1. The method was applied to analysis of actual samples, with RSD (n=6) of the determined values was 0.71%, and the spiked recoveries of 3-HPA were in the range of 98.0%-102%.

       

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