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

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,其中Cleanert PCX净化效果最好。在添加水平为5.0 μg/kg和50.0 μg/kg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。

Determination of Urotropine Residue in Processed Soybean Products by Ion Exchange Solid-Phase Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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 (RSDs) smaller than 6%. This method is rapid,
sensitive, accurate, repeatable and suitable for routine analysis of large-scale samples.