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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 establish a method for the determination of three salbutamol, ractopamine and clenbuterol in pork by ultrasonography-solid phase extraction-ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS / MS). METHODS: Samples were extracted with acetic acid-sodium acetate buffer (pH = 5.2) and extracted by WCX SPE cartridge. The samples were separated on a Xbridge C18 reverse-phase liquid chromatography column (2.1 mm × 100 mm, 5 μm) , Using electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. Results: The three β-agonists showed good linearity (r> 0.999) in the range of 0.1μg / kg to 8.0μg / kg (equivalent to 0.25μg / L to 20.0μg / L) μg / kg ~ 0.02μg / kg, the lowest limit of quantification was 0.04μg / kg ~ 0.05μg / kg and RSDs was 4.7% ~ 7.5%. The recoveries of three β-agonists in pork samples were 97.4% -106.6%, 93.1% -98.5% and 94.2% -95.0%. Conclusion: This method can be used for the rapid screening and confirmatory analysis of salbutamol, ractopamine and clenbuterol residues in pork.