罗丹明类柱前衍生剂HPLC-MS法检测果蔬中的单氰胺

Determination of Cyanamide in Fruits and Vegetables by HPLC-MS with Rhodamine Precolumn Derivatization Agent

合成了新型化学衍生试剂罗丹明B-N-羟基琥珀酰亚胺酯(RBS),基于RBS柱前衍生和高效液相色谱-质谱联用法建立了果蔬中单氰胺的检测方法。样品经乙酸乙酯萃取,用RBS衍生化后,采用高效液相色谱-质谱联用法测定。结果显示:衍生化试剂RBS具有很好的质谱检测灵敏度,对单氰胺的衍生化反应高效、专一。单氰胺浓度在0.005~5 mmol/L时呈现良好的线性关系,相关系数为0.9969,该方法的检出限为0.001 mmol/L,定量限为0.0025 mmol/L,样品加标回收率为77.56%~105.21%,相对标准偏差为1.88%~4.04%。该方法选择性好、灵敏度高、检测限低,可满足果蔬中的单氰胺残留量的测定。

In this work,the detection method of cyanamide in fruits and vegetables was established,using a synthesized rhodamine B-N-hydroxy succinimide(RBS)as the new pre-column derivatizing reagent.After extracted with ethyl acetate and derivatized with RBS,the samples were determined by high performance liquid chromatography-mass spectrometry.The results showed that the reagent RBS had advantages of detection sensitivity for mass spectrometry and was highly efficient and specific in the derivatization reaction of cyanamide.In addition,a better linear relationship was shown when the concentration of cyanamide was 0.005-5 mmol/L,with the correlation coefficient was 0.9969.It was found that the detection limits and quantification limits of this method were 0.001 mmol/L and 0.0025 mmol/L,respectively.The standard recovery rate of samples was in the range of 77.56%-105.21%and the relative standard deviation was among 1.88%-4.04%.This method meets the requirements of analysis,with good selectivity,high sensitivity and low detectable limit,and is suitable for the determination of cyanamide residues in fruits and vegetables.