色谱2017,Vol.35Issue(11):1160-1164,5.DOI:10.3724/SP.J.1123.2017.07005
固相萃取-超高效液相色谱联用测定水果及果酱中的展青霉素
Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography
摘要
Abstract
With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target com-pounds were separated on a C18 column (100 mm×2. 1 mm, 1. 8μm), using 0. 8% (v/v) tetra-hydrofuran solution as mobile phase with a flow rate of 0. 5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0. 1 to 10 mg/L with the correlation coefficient ( R2 ) of 1. The limit of detection for this method was 10. 22 μg/kg. The spiked recoveries of samples were 86. 58%-94. 84% with the relative standard deviations ( RSDs ) of 1. 45%-2. 28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.关键词
固相萃取/超高效液相色谱/展青霉素/水果制品Key words
solid phase extraction ( SPE)/ultra performance liquid chromatography ( UPLC)/patulin ( PAT)/fruit products分类
化学化工引用本文复制引用
吕伟超,申书昌,王超..固相萃取-超高效液相色谱联用测定水果及果酱中的展青霉素[J].色谱,2017,35(11):1160-1164,5.基金项目
黑龙江省教育厅基本业务专项(135209221,135109206). Special Research Project of Heilongjiang Province Education Office ( Nos. 135209221, 135109206) . (135209221,135109206)