超高效液相色譜-串聯(lián)質(zhì)譜測(cè)定動(dòng)物肌肉組織中32種β-激動(dòng)劑、β-阻滯劑和糖肽類抗生素藥物殘留
發(fā)布時(shí)間:2018-07-03 20:57
本文選題:β-激動(dòng)劑 + β-阻滯劑; 參考:《分析化學(xué)》2016年02期
【摘要】:建立了同時(shí)測(cè)定動(dòng)物肌肉組織中27種β-激動(dòng)劑、3種β-阻滯劑和2種糖肽類抗生素的超高效液相色譜-串聯(lián)質(zhì)譜(UPLC-MS/MS)方法。樣品經(jīng)酶解、蛋白沉淀后,以乙酸乙酯-異丙醇(6∶4,V/V)提取,StarataX-C固相萃取凈化,BEH C18色譜柱分離,乙腈-0.1%甲酸梯度洗脫,串聯(lián)質(zhì)譜ESI+電離,多反應(yīng)監(jiān)測(cè)模式檢測(cè),外標(biāo)法定量。結(jié)果表明,32種目標(biāo)物在線性范圍內(nèi)相關(guān)性良好(R20.995),多巴胺、瑞普特羅、萬(wàn)古霉素和去甲萬(wàn)古霉素的方法檢出限為5μg/kg,其它目標(biāo)物的檢出限為3μg/kg;平均加標(biāo)回收率為83.6%~103%,相對(duì)標(biāo)準(zhǔn)偏差(n=6)為3.9%~10.4%,日間精密度為4.5%~9.8%。結(jié)果表明,本方法準(zhǔn)確、靈敏,適用于動(dòng)物肌肉組織中β-激動(dòng)劑、β-阻滯劑,以及糖肽類抗生素的高通量測(cè)定。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) method was developed for simultaneous determination of 27 尾 -agonists, 3 尾 -blockers and 2 glycopeptide antibiotics in animal muscle tissue. After enzymatic hydrolysis and protein precipitation, Starata X-C solid phase extraction (SPE) was used to purify the samples on the chromatographic column, acetonitrile-0.1% formic acid gradient elution, tandem mass spectrometry ESI ionization, multi-reaction monitoring mode detection and external standard method. The results showed that the linear range of 32 target compounds was good (R20.995), dopamine, rapterol, The detection limit of vancomycin and norvancomycin is 5 渭 g / kg, the detection limit of other target compounds is 3 渭 g / kg, the average recovery is 83.6% and 103%, the relative standard deviation (nn ~ (6) is 3.9g / kg and the precision during day is 4.59.8%. The results showed that the method was accurate and sensitive and was suitable for the high-throughput determination of 尾 -agonists, 尾 -blockers and glycopeptide antibiotics in animal muscle tissues.
【作者單位】: 廣州質(zhì)量監(jiān)督檢測(cè)研究院國(guó)家加工食品質(zhì)量監(jiān)督檢驗(yàn)中心(廣州)廣州市食品安全檢測(cè)技術(shù)重點(diǎn)實(shí)驗(yàn)室廣州市食品安全風(fēng)險(xiǎn)動(dòng)態(tài)監(jiān)測(cè)與預(yù)警研究中心;
【基金】:國(guó)家科技部港澳臺(tái)科技合作專項(xiàng)基金資助(No.2013DFH30070)~~
【分類號(hào)】:TS255.7;O657.63
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1 左文堅(jiān);高效液相色譜法手性色譜柱分離β-阻滯劑對(duì)映體[J];天津藥學(xué);2001年06期
,本文編號(hào):2094983
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