土壤中双氰胺残留量的检测方法  

A Determination Method of Dicyandiamide Residues in Soil

作　　者：盛立彦 李美华[1] 吕靖[1] 孙雯[1] 潘洁[1] 

机构地区：[1]上海化工研究院,上海200062

出　　处：《核农学报》2017年第1期163-168,共6页Journal of Nuclear Agricultural Sciences

基　　金：国家科技支撑计划项目(2015BAK45B01)

摘　　要：为检测双氰胺的残留量,在土壤样品加入自制的双氰胺-15N4内标,经超声萃取及冷冻离心处理,采用电喷雾(ESI+)正离子扫描模式,在选择离子监控模式(SRM)下,建立高效液相色谱-串联质谱法定量分析双氰胺的方法。结果表明,该方法在10~50μg·L-1的浓度范围内线性良好,标准曲线回归方程为y=0.9698 x+0.0039,r2=0.9994。方法的检出限与定量限分别为5μg·L-1和16μg·L-1,回收率为97%~104%,RSD<1.2%(n=6)。采用该方法检测3类不同的土壤样品,其结果均与理论预期相符。综上,该方法简便、灵敏、准确,为科学施用含双氰胺氮肥的研究提供了一种表征手段。A high performance liquid chromatography- mass spectrometry（ HPLC- MS / MS） method was established for the determination of dicyandiamide in soils with self- prepared dicyandiamide-15N4 as internal standard. Soil samples were prepared by ultrasonic solvent extraction and refrigerated centrifugation. The mass spectrometer was operated in the positive mode using SRM. The linear range of the dicyandiamide concentration was obtained from 10 to 50μg· L- 1with correlation coefficients（ r2） more than 0. 999. The limit of detection（ LOD） and the limit of quantitation（ LOQ） were5 μg·L- 1and 16μg·L- 1,respectively. The recoveries were between 97% to 104%,and RSD value less than 1. 2%（ n = 6）. The testing results of three kinds of soil samples by this method agreed to their expectation. The method was simple,sensitive and accurate,filling in the gaps in the analytical technics of soil research.

关 键 词：高效液相色谱-串联质谱法 双氰胺 同位素内标 土壤 

分 类 号：X833[环境科学与工程—环境工程]