固相萃取-液相色谱-四极杆飞行时间质谱法快速筛查禽蛋及蛋制品中氟虫腈及其代谢物

发布时间：2018-10-14 11:03

【摘要】：建立了液相色谱-四极杆飞行时间质谱(LC-QTOF MS)测定禽蛋及蛋制品中氟虫腈及其代谢物的快速筛查方法。样品经酸性乙腈提取,PRiME HLB SPE柱净化,Poroshell 120 EC C18色谱柱(150 mm×3 mm,2.7μm)分离,以水-乙腈为流动相,梯度洗脱,负离子模式下测定,以乙虫腈为内标定量。实验中建立了一级精确质量和二级碎片离子质谱数据库,并且对4种禽蛋及蛋制品的基质效应进行了考察。结果表明,氟虫腈及其代谢物在0.1~5μg/L范围内线性关系良好,相关系数(r2)均大于0.99。方法的检出限(LOD,S/N3)和定量限(LOQ,S/N10)分别为0.2μg/kg和1μg/kg。在不同基质中,氟虫腈及其代谢物在1、2和5μg/kg的添加水平下平均加标回收率为82.6%~98.1%,相对标准偏差为3.8%~9.9%(n=6)。该方法有效消除了液相色谱-四极杆飞行时间质谱检测过程中的离子化抑制效应,灵敏度和准确度高,适用于鸡蛋、鸡蛋面、蛋糕和蛋黄酱中氟虫腈、氟虫腈砜、氟虫腈亚砜和氟甲腈的快速筛查。
[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.
【作者单位】：上海出入境检验检疫局;江苏出入境检验检疫局;
【基金】：上海市科委2015年度科学仪器领域项目(15142201700)~~
【分类号】：O657.63;TS253.7

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