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

作者：Chen Da Wei; Yin Yi Qun; Miao Hong; Zhao Yun Feng^*

来源：Chinese Journal of Analytical Chemistry, 2015, 43(4): 542-547.

DOI：10.11895/j.issn.0253-3820.140784

• Dispersive micro solid phase extraction
• Morpholine
• High resolution mass spectrometry
• Beverage

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 mu m) using a gradient elution program. The accurate mass measurements (precursor ion and fragment ion) of morpholine were obtained using tMSMS 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 mu g/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 mu g/L and 2 mu g/L respectively. The method was simple, sensitive and accurate, and suitable for the rapid screening and confirmation of morpholine residue in fruit juice beverages.

• 出版日期2015-4
• 单位大连市疾病预防控制中心; 国家食品安全风险评估中心