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%.
Determination of Trace of 3-Hydroxypropanal in Water by High Performance Liquid Chromatography Combined with Fluorescence Detector after Derivatization with Dansulfonyl Hydrazine
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%.
high performance liquid chromatographyfluorescence detectordansulfonyl hydrazine3-hydroxypropanalderivatization
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