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超高效液相色譜-串聯(lián)質(zhì)譜法快速測(cè)定豬尿液中30種不同種類“瘦肉精”藥物殘留

發(fā)布時(shí)間:2018-08-22 07:28
【摘要】:建立了超高效液相色譜-串聯(lián)質(zhì)譜快速簡(jiǎn)單地同時(shí)測(cè)定豬尿液中30種不同種類"瘦肉精"藥物(賽庚啶、可樂(lè)定及28種β-受體激動(dòng)劑類)殘留的方法。對(duì)液相色譜分離條件、MS/MS檢測(cè)參數(shù)及樣品前處理方式進(jìn)行了優(yōu)化。試樣經(jīng)5000 r/min離心5 min后直接經(jīng)MCX柱凈化,分別用3 m L水和3 m L甲醇淋洗,5%氨化甲醇進(jìn)行洗脫,N2吹干后以流動(dòng)相進(jìn)行復(fù)溶,UPLC-MS/MS進(jìn)行測(cè)定。結(jié)果表明,30種藥物可在5.0 min內(nèi)有效分離;各藥物在0.1~10μg/L范圍內(nèi)呈良好的線性關(guān)系,相關(guān)系數(shù)均大于0.992;方法的檢出限為0.1μg/L,定量限為0.3μg/L。在3個(gè)濃度水平下的平均回收率為67.6%~103.2%,日內(nèi)、日間相對(duì)標(biāo)準(zhǔn)偏差分別為2.8%~16.8%和2.6%~15.8%。
[Abstract]:A rapid and simple method for the simultaneous determination of 30 different kinds of "lean meatine" (cyproheptadine, clonidine and 28 尾 -agonists) in pig urine by ultra-high performance liquid chromatography-tandem mass spectrometry was established. The detection parameters and sample pretreatment methods of MS / MS were optimized. The samples were purified by MCX column after centrifugation for 5 min with 5000 r/min. The samples were eluted with 3 mL water and 3 mL methanol respectively. The samples were eluted by N _ 2 and dried by N _ 2. The mobile phase was determined by UPLC-MS / MS. The results showed that 30 drugs could be effectively separated within 5.0 min, the linear range of each drug was 0.1 渭 g / L and the correlation coefficient was greater than 0.992.The detection limit of the method was 0.1 渭 g / L and the quantitative limit was 0.3 渭 g / L. The average recoveries were 67.6 and 103.2, and the relative standard deviations during the day were 2.816.8% and 2.615.8%, respectively.
【作者單位】: 中國(guó)動(dòng)物衛(wèi)生與流行病學(xué)中心動(dòng)物產(chǎn)品安全監(jiān)測(cè)室;農(nóng)業(yè)部畜禽產(chǎn)品質(zhì)量安全風(fēng)險(xiǎn)評(píng)估實(shí)驗(yàn)室(青島);青島易邦生物工程有限公司;安徽農(nóng)業(yè)大學(xué)動(dòng)物科技學(xué)院;
【基金】:農(nóng)業(yè)部"農(nóng)產(chǎn)品質(zhì)量風(fēng)險(xiǎn)評(píng)估項(xiàng)目"(No.GJFP201600706) 中國(guó)動(dòng)物衛(wèi)生與流行病學(xué)中心創(chuàng)新基金項(xiàng)目(No.2014IF-0003FF)資助
【分類號(hào)】:S859.8;O657.63
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本文編號(hào):2196403

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