离子交换固相萃取结合超高效液相色谱-北京交通大学学报.PDF

166 2014, Vol.35, No.10 食品科学 ※分析检测 离子交换固相萃取结合超高效液相色谱-串联 质谱法测定豆制品中乌洛托品残留量 马雪涛，牛之瑞，冯 雷，谭健林 （云南省产品质量监督检验研究院，云南昆明 650223 ） 摘  要： - 建立了离子交换固相萃取结合超高效液相色谱 串联质谱测定豆制品中乌洛托品残留量的分析方法。通过 0.4%高氯酸提取，固相萃取净化，超高效液相色谱- 串联质谱在正离子模式下，通过多反应监测方式进行检测。比 较了Strata-SCX、SepPak C18和Cleanert PCX三种不同的固相萃取小柱对豆制品中乌洛托品残留量的净化和富集， Cleanert PCX 5.0 μg/kg 50.0 μg/kg 其中 净化效果最好。在添加水平为 和 时，3 种豆制品中乌洛托品的回收率范围在 76.0%～83.6%，相对标准偏差低于6% 。方法具有快速、灵敏、准确、重复性较好的特点，适合于日常大批量样品 的测定。 关键词：乌洛托品；超高效液相色谱- 串联质谱；豆制品 Determination of Urotropine Residue in Processed Soybean Products by Ion Exchange Solid-Phase Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry MA Xue-tao, NIU Zhi-rui, FENG Lei, TAN Jian-lin (Yunnan Institute of Product Quality Supervision and Inspection, Kumming 650223, China) Abstract: An analytical method for the determination of urotropine residue in processed soybean products was developed using ion exchange solid-phase extraction coupled with ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-MS-MS). Samples were extracted with 0.4% perchloric acid followed by clean-up using solid-phase extraction. The analysis was carried out under negative electrospray ionization mode using multiple reaction monitoring. Cleanert PCX cartridge showed better clean-up and enrichment than Strata-SCX and SepPak C18 cartridges for urotropine residue. The average recoveries of urotropine in three kinds of processed soybean products at spiked levels of 5.0 and 50.0 μg/kg ranged from 76.0% to 83.6% with relative standard deviations (R