分散固相萃取-超高效液相色谱-串联质谱法测定禽蛋中氟虫腈及其代谢产物

发布时间：2018-02-01 21:39

  本文关键词： 超高效液相色谱-串联质谱 分散固相萃取 氟虫腈 禽蛋　出处：《色谱》2017年12期 　论文类型：期刊论文

【摘要】：建立了分散固相萃取-超高效液相色谱-串联质谱检测禽蛋中氟虫腈及其代谢产物氟甲腈、氟虫腈硫醚和氟虫腈砜的方法。样品用含1%(体积分数)乙酸的乙腈提取后,加无水硫酸钠、十八烷基键合硅胶(C18-N)及氨基-丙基乙二胺(NH2-PSA)3种净化剂,旋涡振荡,对样品进行净化。以Shim-pack GIST C18色谱柱(50 mm×2.1 mm,2μm)进行分离,以甲醇和1 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,在电喷雾离子源负离子模式和多反应检测(MRM)模式下进行定性定量分析。考察了净化剂中无水硫酸钠、C18-N和NH2-PSA的用量对加标回收率的影响,优化了实验条件。结果表明:4种化合物在0.4~100μg/L范围内线性关系良好,相关系数r2≥0.998 9;回收率为95.09%~103.26%;定量限为0.2μg/kg。该方法前处理简单,回收率高,重复性好,可作为禽蛋中氟虫腈及其代谢产物的有效检测方法。
[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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