QuEChERS-高效液相色谱-串联质谱法测定植物源食品中环磺酮残留

发布时间：2018-03-29 16:08

  本文选题：环磺酮　切入点：植物源食品　出处：《分析化学》2017年01期

【摘要】：建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定植物源食品中环磺酮残留量的分析方法。样品经改进的Qu ECh ERS方法一步完成萃取净化,经酸化乙腈(含0.1%(V/V)甲酸的乙腈)提取,经石墨化碳黑(GCB)净化,提取液经离心后直接过膜上机检测。HPLC-MS/MS方法以0.1%(V/V)甲酸-乙腈为流动相,在0.25 m L/min流速下梯度洗脱,采用C18色谱柱进行液相色谱分离,电喷雾正离子电离(ESI+),多重反应监测模式(MRM)检测,基质匹配外标法进行定量分析。结果表明,在10种基质(玉米、大米、小麦、葡萄、苹果、葡萄干、枸杞、西红柿、黄瓜、白菜)中,环磺酮在0.5~100.0 ng/m L范围内线性关系良好,相关系数均大于0.996;方法定量限(S/N≥10)为1.0μg/kg;在1.0,2.0和10.0μg/kg添加水平下,环磺酮的平均回收率为82.0%~111.8%,相对标准偏差为3.0%~14.9%。本方法高效快捷,灵敏度、准确度和精密度均符合农药残留检测要求。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was established for the determination of the residues of cyclosulfonone in vegetable foods. The samples were extracted and purified by an improved qu ECh ERS method. The samples were extracted by acidified acetonitrile (acetonitrile containing 0.1 V / V) formic acid. After purification by graphitized carbon black (L/min), the extract was separated by liquid chromatography on C18 column after centrifugation. The mobile phase was 0.1 V / V form-acetonitrile, the mobile phase was 0.1 V / V formic acid-acetonitrile, and the separation was carried out on a C18 chromatographic column with a gradient elution at a flow rate of 0.25 m L/min. Electrospray positive ion ionization (ESI), multiple reaction monitoring model (MRM), matrix matching external standard method were used for quantitative analysis. The results showed that, in 10 substrates (corn, rice, wheat, grape, apple, raisin, medlar, tomato, cucumber), In Chinese cabbage, the linear range of cyclosulfonone was 0.5 ~ 100.0 ng/m / L, the correlation coefficients were all greater than 0.996; the quantification limit S / N 鈮，

本文编号：1681864