本文關(guān)鍵詞： 超高效液相色譜-串聯(lián)質(zhì)譜 分散固相萃取 氟蟲腈 禽蛋　出處：《色譜》2017年12期 　論文類型：期刊論文

【摘要】：建立了分散固相萃取-超高效液相色譜-串聯(lián)質(zhì)譜檢測(cè)禽蛋中氟蟲腈及其代謝產(chǎn)物氟甲腈、氟蟲腈硫醚和氟蟲腈砜的方法。樣品用含1%(體積分?jǐn)?shù))乙酸的乙腈提取后,加無(wú)水硫酸鈉、十八烷基鍵合硅膠(C18-N)及氨基-丙基乙二胺(NH2-PSA)3種凈化劑,旋渦振蕩,對(duì)樣品進(jìn)行凈化。以Shim-pack GIST C18色譜柱(50 mm×2.1 mm,2μm)進(jìn)行分離,以甲醇和1 mmol/L乙酸銨水溶液為流動(dòng)相進(jìn)行梯度洗脫,在電噴霧離子源負(fù)離子模式和多反應(yīng)檢測(cè)(MRM)模式下進(jìn)行定性定量分析。考察了凈化劑中無(wú)水硫酸鈉、C18-N和NH2-PSA的用量對(duì)加標(biāo)回收率的影響,優(yōu)化了實(shí)驗(yàn)條件。結(jié)果表明:4種化合物在0.4~100μg/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)r2≥0.998 9;回收率為95.09%~103.26%;定量限為0.2μg/kg。該方法前處理簡(jiǎn)單,回收率高,重復(fù)性好,可作為禽蛋中氟蟲腈及其代謝產(chǎn)物的有效檢測(cè)方法。
[Abstract]:A dispersive solid phase extraction-ultrahigh performance liquid chromatography-tandem mass spectrometry was established for the determination of fluronitrile and its metabolite in poultry eggs. A method for extracting fluronitrile sulfides and flutamonitrile sulfone. The sample is extracted with acetonitrile containing 1 (volume fraction) of acetic acid and added with anhydrous sodium sulfate. 18 alkyl bonded silica gel (C18-N) and amino-propyl ethylenediamine (NH2-PSAN) were used as purifiers for vortex oscillation. The samples were purified and separated by Shim-pack GIST C18 column (50mm 脳 2.1mm ~ 2 渭 m). Methanol and 1 mmol/L ammonium acetate aqueous solution were used as mobile phase for gradient elution. Qualitative and quantitative analysis was carried out under the anion mode of electrospray ion source and MRM mode. The anhydrous sodium sulfate in the purifier was investigated. The effects of the amount of C18-N and NH2-PSA on the recoveries were optimized and the experimental conditions were optimized. The results showed that there was a good linear relationship between the four compounds in the range of 0.4 渭 g / L and 100 渭 g / L. Correlation coefficient R2 鈮，

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