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

作　　者：王芳[1,2] 罗敏 黄杰军[3] 徐林[3] WANG Fang;LUO Min;HUANG Jiejun;XU Lin(Yangzhou Polytechnic Institute,Yangzhou 225127,China;College of Chemistry and Chemical Engineering,Yangzhou University,Yangzhou 225002,China;Jiangsu Yangnong Chemical Group Co.,Ltd.,Yangzhou 225009,China)

机构地区：[1]扬州工业职业技术学院,扬州225127 [2]扬州大学化学化工学院,扬州225002 [3]江苏扬农化工集团有限公司,扬州225009

出　　处：《理化检验（化学分册）》2024年第1期79-82,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：扬州科技计划项目(YZ2022189)。

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 C_(18)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7.6~380.0μg·L^(-1)内与衍生物的峰面积呈线性关系,检出限(3S/N)为1.1μg·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%。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 C_(18)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 7.6-380.0μg·L^(-1),with detection limit(3S/N)of 1.1μg·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%.

关 键 词：高效液相色谱法 荧光检测器 丹磺酰肼 3-羟基丙醛 衍生 

分 类 号：O657.7[理学—分析化学]