超高效液相色譜-電噴霧電離-串聯(lián)質(zhì)譜法測定豬糞便中6種抗生素殘留的基質(zhì)效應(yīng)研究
發(fā)布時間:2018-06-05 15:15
本文選題:基質(zhì)效應(yīng) + 離子抑制率 ; 參考:《分析測試學(xué)報》2017年08期
【摘要】:基質(zhì)效應(yīng)普遍存在于液質(zhì)聯(lián)用分析中。該文通過評價"離子抑制率"指標(biāo),系統(tǒng)考察了應(yīng)用超高效液相色譜-電噴霧電離-串聯(lián)質(zhì)譜法(UPLC-ESI-MS/MS)測定豬糞便中二甲氧芐啶、磺胺對甲氧嘧啶、恩諾沙星、環(huán)丙沙星、金霉素、泰樂菌素6種抗生素殘留的基質(zhì)效應(yīng)。樣品經(jīng)McIlvaine-Na_2EDTA緩沖溶液提取后,采用HLB固相萃取柱凈化,濃縮富集后用0.1%甲酸-甲醇溶液(85∶15,體積比)溶解。經(jīng)SB C_(18)RRHD色譜柱分離,以甲醇-0.1%甲酸為流動相進(jìn)行梯度洗脫,在正離子電噴霧下采用多反應(yīng)監(jiān)測模式檢測。結(jié)果表明,豬糞便基質(zhì)對6種抗生素的測定存在基質(zhì)增強效應(yīng)。采用基質(zhì)匹配標(biāo)準(zhǔn)曲線校正法并優(yōu)化樣品處理條件可以對基質(zhì)效應(yīng)產(chǎn)生的影響進(jìn)行補償與消除。該研究為提高檢測結(jié)果的準(zhǔn)確度與精密度提供了借鑒。
[Abstract]:The matrix effect is widely used in liquid-mass spectrometry. The determination of dimethoprim, sulfamethoxine, enrofloxacin, ciprofloxacin, chlortetracycline in pig feces by UPLC-ESI-MS / MSM was systematically studied by evaluating the index of "ion inhibition rate" by ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS). Matrix effect of 6 antibiotic residues of tylosin. The samples were extracted by McIlvaine-Na_2EDTA buffer solution, purified by HLB solid-phase extraction column, concentrated and dissolved in 0.1% formic acid-methanol solution (85: 15, volume ratio). After separation by SB C_(18)RRHD column, gradient elution was carried out with methanol-0.1% formic acid as mobile phase, and detected by multi-reaction monitoring mode under positive ion electrospray. The results showed that porcine fecal matrix had matrix enhancement effect on the determination of 6 antibiotics. The matrix matching standard curve correction method and the optimization of sample treatment conditions can compensate and eliminate the effect of matrix effect. This study provides a reference for improving the accuracy and precision of the detection results.
【作者單位】: 上海市動物疫病預(yù)防控制中心;
【基金】:上海市科技興農(nóng)重點攻關(guān)項目[滬農(nóng)科攻字(2011)第4-9號]資助
【分類號】:O657.63;S859.8
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