【摘要】：建立了固相萃取-液相色譜串聯(lián)質(zhì)譜法(SPE-LC-MS/MS)同時(shí)檢測(cè)養(yǎng)殖海水中17種喹諾酮類藥物殘留的分析方法。海水經(jīng)酸化處理后,采用HLB固相萃取柱富集、凈化目標(biāo)化合物,通過(guò)對(duì)比水樣在不同上樣p H、淋洗液與洗脫液等條件下的回收率,以此對(duì)前處理方法進(jìn)行優(yōu)化。收集到的洗脫液經(jīng)氮?dú)獯蹈珊笥昧鲃?dòng)相定容至1 ml,待測(cè)。色譜流動(dòng)相A相為0.1%甲酸水溶液,B相為乙腈,所有藥物經(jīng)梯度洗脫進(jìn)行分離,在LC-MS/MS正離子模式的多反應(yīng)監(jiān)測(cè)模式下進(jìn)行定性定量分析。17種化合物可以在10 min中內(nèi)得到較好的分離,線性范圍為1 200 ng/ml,線性相關(guān)系數(shù)均大于0.999,檢出限均在2 10 ng/L范圍內(nèi),定量限均在5 20 ng/L范圍內(nèi)。以空白海水為基質(zhì),在20、100、200 ng/L三個(gè)不同添加水平下采用內(nèi)標(biāo)法定量的加標(biāo)回收率均在71.3% 125.0%范圍內(nèi),相對(duì)標(biāo)準(zhǔn)偏差(RSD)為2.44% 12.27%(n=5)。采用該方法對(duì)黃海靈山灣近岸4個(gè)養(yǎng)殖場(chǎng)進(jìn)行海水采集并檢測(cè),共檢測(cè)出4種喹諾酮類藥物,分別是恩諾沙星、氧氟沙星、諾氟沙星和環(huán)丙沙星,其中,恩諾沙星濃度最高。研究表明,該方法快速、可靠,適用于養(yǎng)殖海水中喹諾酮類藥物的檢測(cè)。
[Abstract]:A method for the simultaneous determination of 17 quinolones residues in cultured seawater by solid phase extraction-liquid chromatography tandem mass spectrometry (SPE-LC-MS/MS) was established. After acidizing, the seawater was enriched by HLB solid phase extraction column to purify the target compounds. The recovery rates of water samples under different conditions, such as pH, eluent and eluent, were compared to optimize the pretreatment method. The collected eluent was dried by nitrogen and then the volume was fixed to 1 ml,. The chromatographic mobile phase A is 0.1% formic acid aqueous solution and B phase is acetonitrile. All the drugs are separated by gradient elution. the 17 compounds can be separated qualitatively and quantitatively in the multi-reaction monitoring mode of LC-MS/MS positive ion mode. 17 compounds can be separated in 10 min, the linear correlation coefficient is 1 鈮，

本文編號(hào)：2526131