高效液相色谱法测定含氮类肥料中缩二脲假阳性结果分析及解决方法  

Analysis and Solution of False Positive Results in the Determination of Biuret in Nitrogen-containing Fertilizers by High Performance Liquid Chromatography

作　　者：李美玲 钟亚 韩晓培 刘文枚 胡宏鲲 陈江 LI Mei-Ling;ZHONG Ya;HAN Xiao-Pei;LIU Wen-Mei;HU Hong-Kun;CHEN Jiang(Chongqing Customs Technical Center,Chongqing 400020;Yongchuan Customs,Yongchuan 402160)

机构地区：[1]重庆海关技术中心,重庆400020 [2]永川海关,永川402160

出　　处：《中国口岸科学技术》2023年第8期82-89,共8页China Port Science and Technology

摘　　要：基于亲水作用色谱(Hydrophilic interaction chromatography,HILIC)技术分离双氰胺与缩二脲,建立复混肥料(复合肥料)中缩二脲和双氰胺的高效液相色谱检测方法。该方法解决了GB/T 22924—2008《复混肥料(复合肥料)中缩二脲含量的测定》实施过程中,双氰胺对缩二脲测定结果的干扰。优化方法中的样品经95%乙腈提取后,采用Venusil HILIC色谱柱分离,乙腈与水(95∶5)作流动相,使用二极管阵列检测器(Diode array detector,DAD)进行检测。在该体系下,缩二脲在10~100 mg/L范围内线性相关系数(r)为0.9994,双氰胺在10~100 mg/L范围内线性相关系数(r)为0.9996;以三元复混肥、硝酸铵为基底,缩二脲加标回收率为95.7%~100.1%,双氰胺加标回收率为95.8%~106.1%。该方法能有效分离肥料中的缩二脲和双氰胺。Based on the separation of dicyandiamide and biuret by hydrophilic interaction chromatography(HILIC),a high performance liquid chromatography(HPLC)method for the determination of biuret and dicyandiamide in compound fertilizers was established.This method solved the interference of dicyandiamide on the determination of biuret in compound fertilizers during the implementation of GB/T 229242008.The samples in the optimization method were extracted by 95%acetonitrile and separated by a Venusil HILIC chromatographic column.Acetonitrile and water(95:5)were used as the mobile phase,and were detected by diode array detector(DAD).In this system,the linear correlation coeficient(r)of biuret was 0.9994 in the range of 10-100 mg/L,and the linear correlation coefficient (r) of dicyandiamide line was 0.9996 in the range of 10-100 mg/L. Based on ternary compound fertilizerand ammonium nitrate, the recovery rates of biuret and dicyandiamide were 95.7%-100.1% and 95.8%-106.1%, respectively. Themethod can effectively separate biuret and dicyandiamide from fertilizer.

关 键 词：含氮类肥料 缩二脲 假阳性 高效液相色谱法 

分 类 号：O657.72[理学—分析化学] TQ441[理学—化学]