超声辅助-固相萃取-UFLC-MS/MS法测定猪肉中3种常用β-受体激动剂

Analysis of 3 β-agonists in pork by ultrasonic-solid phase extraction coupled with ultrafast liquid chromatography-tandem mass spectrometry

目的:建立猪肉中3种沙丁胺醇、莱克多巴胺和克伦特罗的超声辅助-固相萃取-超快速液相色谱-串联质谱(UFLC-MS/MS)测定方法。方法:样品采用乙酸-乙酸钠缓冲液(pH=5.2)为提取溶剂进行超声提取,WCX固相萃取小柱净化,在Xbridge C18反相液相色谱柱(2.1 mm×100 mm,5μm)上分离,采用电喷雾离子源(ESI)在多反应监测(MRM)模式下检测。结果:3种β-受体激动剂在0.1μg/kg～8.0μg/kg(相当于0.25μg/L～20.0μg/L)范围内具有良好的线性(r>0.999),检出限为0.01μg/kg～0.02μg/kg,最低定量限为0.04μg/kg～0.05μg/kg,RSDs为4.7%～7.5%;3种β-受体激动剂在猪肉样品中的加标回收率分别为97.4%～106.6%、93.1%～98.5%和94.2%～95.0%。结论:本方法可用于猪肉中沙丁胺醇、莱克多巴胺和克伦特罗残留的快速筛查和确证分析。

Objective ： To develop a method for the simultaneous determination of 3 β - agonists namely salbuta- tool, raetopamine and elenbuterol in pork by ultrasonic - solid phase extraction coupled with ultrafast liquid chroma- tography -tandem mass spectrometry （UFLC -MS/MS）. Methods： Pork samples were extracted ultrasonically with sodium acetate - acetic acid buffer solution （ pH = 5.2 ） and cleaned up by WCX solid - phase extraction （ SPE ） cartridges. Chromatographic separation was performed on a Xbridge C18 analytical colunm （ 100 mm × 2.1 mmi. d. , 5.0 μm）. The tandem mass spectrometer was operated by using electrospray ion source （ESI） in tile nmhiple reaction monitoring （MRM） mode. Results： Linearities were in the range of 0.1 μg/kg ～ 8.0 μg/kg （ equivalent to 0.25 μg/L - 20.0 μg/L） with determination coefficients （ r2 ） higher than 0. 999 for the 3 β - agonists. The limits of detection （LODs） in pork samples were in the range of 0.01 μg/kg -0.02 μg/kg and the limits of quantification （LOQs） were between 0.04 μg/kg- 0.05 μg/kg. The relative standard deviations （RSDs） were in the range of4.7% ～7.5%. Recoveries were between 97.4% - 106.6% at the spiked level of 0.2 p^g/kg, 93.1% -98.5% at 0.8 txg/kg and 94.2% ～95.0% at 4.0 trg/kg, respectively. Conclusion： The developed method can be applied to the routine analysis h^r the determination of the 3 β - agonists in pork samples.