【作者】 贾晓飞；

【导师】 曲建强；

【作者基本信息】 天津大学 ， 有机化学， 2007， 硕士

【摘要】 随着经济的快速发展,动物源性食品在人们生活中所占比例越来越大,而各种动物源性食品中的兽药残留污染已成为危及人类身体健康的公共卫生热点问题,本文建立了尿液中9种β₂-受体激动剂残留的超高效液相色谱-电喷雾串联四极杆、多反应监测（MRM）模式的质谱（正离子模式）分析方法。样品加入缓冲溶液,经酶解高氯酸超声提取、HLB柱富集、MCX柱净化,通过Waters ACQUITY UPLCTM BEH C18 （100 mm×2.1 mm, 1.7μm）色谱柱分离,以甲醇和0.1 %甲酸水溶液为流动相（流速为0.3 mL/min）进行梯度洗脱,超高效液相色谱-质谱/质谱分析。以保留时间和离子对（定量离子、确证离子）信息比较进行定性,以母离子和响应值高的碎片离子进行定量。最低方法检出限介于0.002⁰.02μg/L,最低定量限介于0.007⁰.06μg/L,添加水平为0.1μg/L、0.5μg/L、2μg/L,加标回收率为75.3¹16.0 %,批内相对标准偏差介于3.4²7.4 %,批间相对标准偏差介于5.2²4.5 %。更多还原

【Abstract】 As the fast development of economy, food derived from animal is becoming more and more important in our life, but drug residues derived from food in every kind of animal have become a hot topic of public health. In this paper, an analytical method based on ultra performance liquid chromatography-tandem mass spectrometry with positive mode has been developed for the simultaneous determination ofβ₂-agonists in urines. Samples were deconjugated withβ-glucuronidase/sulfatase enzyme in acetate buffer, deproteinized by perchloric acid and the pH was adjusted to 4.0. The concentration and purification was performed using Oasis HLB, Oasis MCX. The separation was performed on a Waters ACQUITY UPLC^TM BEH C18 column （100 mm×2.1 mm, 1.7μm） with gradient elution using methanol and 0.1 % formic acid at a flow rate of 0.3 mL/min. The limits of detection （LOD） of the method ranged from 0.002 to 0.02μg/L and the limits of quantification （LOQ） ranged from 0.007⁰.06μg/L. Average recoveries at the spiking levels of 0.1, 0.5 and 2μg/L ranged from 75.3 % to 116.0 %, with relative standard deviations of within-run between 3.4 % and 27.4 % and relative standard deviations of between-run between 5.2 % and 24.5 %.更多还原