【摘要】：建立了固相萃取-超高效液相色譜-串聯(lián)質(zhì)譜(UPLC-MS/MS)同時(shí)檢測(cè)畜禽糞便中四環(huán)素類、磺胺類、氟喹諾酮類和大環(huán)內(nèi)酯類16種抗生素的分析方法。針對(duì)目標(biāo)物化學(xué)性質(zhì)和樣品雜質(zhì)情況,對(duì)質(zhì)譜條件、提取液種類、超聲功率等參數(shù)進(jìn)行了優(yōu)化。最終以50%乙腈(V/V)的磷酸鹽緩沖溶液(p H=4)提取3次,經(jīng)過(guò)超聲、離心、旋蒸、稀釋后,SAX-HLB串聯(lián)小柱凈化富集,用10 m L甲醇-丙酮混合液(80∶20,V/V)洗脫,35℃氮吹近干后,用含0.1%甲酸-甲醇(1∶1,V/V)定容,在UPLC-MS/MS多反應(yīng)檢測(cè)模式下進(jìn)行定性及定量分析。結(jié)果表明,糞便中四環(huán)素類、磺胺類、氟喹諾酮類和大環(huán)內(nèi)酯類抗生素的平均加標(biāo)回收率為56.4%~94.6%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)在2.6%~19.8%之間,方法檢出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分別為0.01~2.50μg/kg和0.05~7.90μg/kg。本方法簡(jiǎn)便、穩(wěn)定性好、靈敏度高、重現(xiàn)性好,適用于畜禽糞便中多種抗生素的同時(shí)檢測(cè)。
[Abstract]:A method for the simultaneous determination of 16 antibiotics such as tetracycline, sulfonamides, fluoroquinolones and macrolides in livestock and poultry feces by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. According to the chemical properties of the target and the impurity situation of the sample, the parameters such as mass spectrometry conditions, type of extract, ultrasonic power and so on were optimized. Finally, 50% acetonitrile (V 鈮，

本文編號(hào)：2481957