超高效液相色谱-电喷雾串联四极杆质谱法检测动物组织中20种β_2-兴奋剂残留

Simultaneous determination of 20 β_2-agonists residues in animal tissues by ultra performance liquid chromatography-electrospray tandem mass spectrometry

目的：应用超高效液相色谱-电喷雾串联四极杆质谱联用技术,建立动物组织中20种β2-兴奋剂残留的多组分检测方法。方法：样品经酶解、高氯酸沉淀蛋白,MCX柱净化和富集。选择沙丁醇胺-d3,克伦特罗-d9,莱卡多巴胺-d9为内标,通过Waters ACQUITY UPLCTMBEHShield RP C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相,梯度洗脱,MRM方式测定。结果：该方法的检出限为0.01-0.33μg/kg,最低定量限为0.04-1.11μg/kg。添加水平为0.5、1.0、2.0μg/kg时,20种β2-兴奋剂的加标回收率为75.5%-108.4%,相对标准偏差为2.9%-19.0%。结论：该方法灵敏度高、回收率好,能够快速准确地对动物组织中20种β2-兴奋剂进行检测。

Objective：A analytical method based on ultra performance liquid chromatography-electrospray tandem mass spectrometry（UPLC-MS/MS） has been developed for the simultaneous determination of 20 β2-agonists in animal tissues.Methods：Samples were deconjugated with β-glucuronidase/arylsulfatase enzyme in acetate buffer and deproteinized by perchloric acid,and then adjusted to pH 4.0.Sample concentration and purification were performed using Oasis MCX cartridge.The separation was performed on a Waters ACQUITY UPLCTM BEH Shield RP 18 column（100 mm×2.1 mm i.d.,1.7 μm） with gradient elution using acetontrile and water（containing 0.1% formic acid） at a flow rate of 0.3 ml/min.Results：The limits of detection（LOD）of the method were 0.01-0.23 μg/kg and the limits of quantification（LOQ） 0.04-1.11 μg/kg.Average recoveries for 20 β2-agonists at the spiking levels of 0.5,1.0 and 2.0 ranged from 75.5% to 108.4%,with relative standard deviations between 2.9% and 19.0%.Conclusion：The established method is sensitive and of good recoveries.It can be applied as a rapid and reliable method for determination of 20 β2-agonists in animal tissues.