分散微固相萃取-超高效液相色谱-高分辨质谱法测定果汁饮料中的吗啉残留

Dispersive Micro Solid Phase Extraction Combined with Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry for Determination of Morpholine Residue in Fruit Juices Beverages

基于强阳离子交换填料（PCX）,采用分散微固相萃取（DMSPE）前处理技术,结合超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用技术（UPLC/Q Orbitrap）,建立了果汁饮料中吗啉残留的快速检测分析方法。通过对DMSPE技术中PCX用量、吸附时间、洗脱溶剂氨水浓度和洗脱体积的优化,实现样品中吗啉的最优提取。以BEH HILIC色谱柱（100 mm×2.1 mm,1.7μm）进行色谱分离,通过静电场轨道阱质谱t MSMS采集模式获得吗啉的精确母离子及碎片离子质量数,进行定性定量分析。结果显示,吗啉在1-100μg/L浓度范围内存在良好的线性关系（R^2〉0.999）,方法检出限和定量限分别为1和2μg/L;平均加标回收率为85.9%-103.8%,日内和日间精密度分别为3.7%-5.2%和3.5%-9.4%。本方法简单精确,灵敏度高,样品处理快捷简便,适用于果汁饮料中吗啉残留的快速分析测定。

A rapid analytical method was established for the determination of morpholine residue in fruit juice beverages by using dispersive micro solid phase extraction（ DMSPE） based on a strong cation exchange adsorbent（ PCX） by UPLC / Q Orbitrap. For DMSPE pretreatment method,the parameters that affected the extraction efficiency of morpholine,such as the amount of PCX,the adsorption time,the concentration of ammonium hydroxide and the volume of eluent were studied. The analyte was separated on a BEH HILIC column（ 100 mm × 2. 1 mm,1. 7 μm） using a gradient elution program. The accurate mass measurements（ precursor ion and fragment ion） of morpholine were obtained using t MSMS scan mode by Q Exactive. In the fruit juices beverages samples, morpholine was screened qualitatively and subjected to the quantitative analysis. The method showed a good linearity（ R^2 〉0. 999） in the ranges of 1- 100 μg / L for morpholine with average recoveries of 85. 9%- 103. 8%,and intra- and inter-day precision of 3. 7%- 5. 2% and 3. 5%-9. 4%,respectively. The limits of detection（ LOD） and quantification（ LOQ） for the method were 1 μg / L and 2 μg / L respectively. The method was simple,sensitive and accurate,and suitable for the rapid screening and confirmation of morpholine residue in fruit juice beverages.