【摘要】：建立了液相色譜-四極桿飛行時(shí)間質(zhì)譜(LC-QTOF MS)測(cè)定禽蛋及蛋制品中氟蟲(chóng)腈及其代謝物的快速篩查方法。樣品經(jīng)酸性乙腈提取,PRiME HLB SPE柱凈化,Poroshell 120 EC C18色譜柱(150 mm×3 mm,2.7μm)分離,以水-乙腈為流動(dòng)相,梯度洗脫,負(fù)離子模式下測(cè)定,以乙蟲(chóng)腈為內(nèi)標(biāo)定量。實(shí)驗(yàn)中建立了一級(jí)精確質(zhì)量和二級(jí)碎片離子質(zhì)譜數(shù)據(jù)庫(kù),并且對(duì)4種禽蛋及蛋制品的基質(zhì)效應(yīng)進(jìn)行了考察。結(jié)果表明,氟蟲(chóng)腈及其代謝物在0.1~5μg/L范圍內(nèi)線(xiàn)性關(guān)系良好,相關(guān)系數(shù)(r2)均大于0.99。方法的檢出限(LOD,S/N3)和定量限(LOQ,S/N10)分別為0.2μg/kg和1μg/kg。在不同基質(zhì)中,氟蟲(chóng)腈及其代謝物在1、2和5μg/kg的添加水平下平均加標(biāo)回收率為82.6%~98.1%,相對(duì)標(biāo)準(zhǔn)偏差為3.8%~9.9%(n=6)。該方法有效消除了液相色譜-四極桿飛行時(shí)間質(zhì)譜檢測(cè)過(guò)程中的離子化抑制效應(yīng),靈敏度和準(zhǔn)確度高,適用于雞蛋、雞蛋面、蛋糕和蛋黃醬中氟蟲(chóng)腈、氟蟲(chóng)腈砜、氟蟲(chóng)腈亞砜和氟甲腈的快速篩查。
[Abstract]:A rapid screening method for determination of fluronitrile and its metabolites in eggs and egg products by liquid chromatography-quadrupole time of flight mass spectrometry (LC-QTOF MS) was established. The samples were purified on, PRiME HLB SPE column with acid acetonitrile and separated by Poroshell 120 EC C18 column (150 mm 脳 3 mm,2.7 渭 m). The samples were separated by aqueous acetonitrile as mobile phase, gradient eluted, determined by negative ion mode, and determined with acetonitrile as internal standard. The first order accurate mass and second order fragment ion mass spectrometry databases were established and the matrix effects of four kinds of poultry eggs and egg products were investigated. The results showed that there was a good linear relationship between fluronitrile and its metabolites in the range of 0.1 渭 g / L, and the correlation coefficient (R2) was higher than 0.99. The detection limit (LOD,S/N3) and quantitative limit (LOQ,S/N10) of the method were 0.2 渭 g/kg and 1 渭 g / kg, respectively. The average recoveries of fluoronitrile and its metabolites in different substrates were 82.6% and 98.1 at the addition level of 1 渭 g/kg and 5 渭 g/kg respectively, and the relative standard deviation was 3.8% (n = 6). This method can effectively eliminate the inhibition effect of ionization in the detection process of liquid chromatography-quadrupole time-of-flight mass spectrometry, and has high sensitivity and accuracy. It is suitable for flufenonitrile and flunonitrile in eggs, egg noodles, cakes and mayonnaise. Rapid screening of fluronitrile sulfoxide and fluoronitrile.
【作者單位】： 上海出入境檢驗(yàn)檢疫局;江蘇出入境檢驗(yàn)檢疫局;
【基金】：上海市科委2015年度科學(xué)儀器領(lǐng)域項(xiàng)目(15142201700)~~
【分類(lèi)號(hào)】：O657.63;TS253.7

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