本文選題：四極桿軌道阱串聯(lián)質(zhì)譜(Q-Orbitrap + MS)��； 參考：《質(zhì)譜學(xué)報(bào)》2017年05期

【摘要】：建立了頭孢噻呋及其主要代謝物去呋喃甲�；^孢噻呋殘留的超高效液相色譜-四極桿軌道阱串聯(lián)質(zhì)譜(UHPLC-Q-Orbitrap MS)分析方法。選用Kinetex F5 100A色譜柱(50mm×3.0mm×2.6μm)分離,在Q-Exactive高分辨質(zhì)譜Full MS/dd-MS2掃描模式下采集數(shù)據(jù)進(jìn)行定性定量分析。兩種目標(biāo)物在3種基質(zhì)中相應(yīng)濃度范圍內(nèi)的線性關(guān)系良好,相關(guān)系數(shù)r2均大于0.990,回收率為83.2%~129.7%,RSD均小于15%。通過(guò)對(duì)雞體內(nèi)頭孢噻呋及其代謝物殘留規(guī)律的分析表明,給藥后,雞胸肉中頭孢噻呋和去呋喃甲�；^孢噻呋均可檢出,且消除時(shí)間均為12~24h;雞肝、雞腎中頭孢噻呋可在0.5h內(nèi)迅速代謝為去呋喃甲�；^孢噻呋,雞肝和雞腎中去呋喃甲�；^孢噻呋的消除時(shí)間分別為48~72h和72~120h。本研究可為保障動(dòng)物源性食品安全以及雞體內(nèi)頭孢噻呋最大殘留限量標(biāo)準(zhǔn)和休藥期的制訂提供理論和實(shí)踐依據(jù)。
[Abstract]:A high performance liquid chromatography-quadrupole orbital trap tandem mass spectrometry (UHPLC-Q-Orbitrap) method was developed for the determination of cefotioxime and its main metabolite, defurfuryl cefotaxime. A 50 mm 脳 3.0mm 脳 2.6 渭 m Kinetex F5100A column was used for qualitative and quantitative analysis of the data collected by Q-Exactive high resolution mass spectrometry Full MS/dd-MS2 scanning mode. The linear relationship between the two targets in the corresponding concentration range of the three substrates is good, the correlation coefficient R2 is greater than 0.990, the recovery rate is 83.2 and 129.7% RSD is less than 15%. The results of analysis of cefotaxime and its metabolites in chicken body showed that both cefotioxime and defuranyl cefotioxime could be detected in chicken breast meat after administration, and the elimination time was 124h. Ceftiofuroxime in chicken kidney was rapidly metabolized as defurfuryl cefotioxime within 0.5 h, and the elimination time of defuryl cefotiofuroxime in chicken liver and kidney was 48 ~ 72 h and 72 ~ 120 h, respectively. This study can provide theoretical and practical basis for the protection of animal food safety, maximum residue limit of cefotaxime in chicken and the period of withdrawal of cefotaxime.
【作者單位】： 陜西師范大學(xué);中國(guó)檢驗(yàn)檢疫科學(xué)研究院;北京市理化分析測(cè)試中心北京市食品安全分析測(cè)試工程技術(shù)研究中心;北京出入境檢驗(yàn)檢疫局檢驗(yàn)檢疫技術(shù)中心;廈門市出入境檢驗(yàn)檢疫局檢驗(yàn)檢疫技術(shù)中心;
【基金】：國(guó)家重大儀器開(kāi)發(fā)專項(xiàng)(2012YQ14000806) 北京市科技計(jì)劃項(xiàng)目(Z141100002614020)資助
【分類號(hào)】：O657.63;TS251.7

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