分散固相萃取-液相色谱-串联质谱法测定谷物、蔬菜、水果中27种新型杀菌剂

发布时间：2018-05-18 03:16

  本文选题：液相色谱-串联质谱 + 分散固相萃取　； 参考：《色谱》2017年05期

【摘要】：建立了同时检测谷物、蔬菜和水果中27种新型杀菌剂的分散固相萃取-液相色谱-串联质谱(DSPE-LC-MS/MS)分析方法。样品经1%(体积分数)乙酸丙酮溶液提取,以无水硫酸镁(MgSO_4)脱水,经N-丙基乙二胺(PSA)、C_(18)、无水MgSO_4、多壁碳纳米管(MWCNT)混合净化剂净化,经C_(18)色谱柱分离,用乙腈和体积分数为0.1%的甲酸水溶液(含5 mmol/L乙酸铵)梯度洗脱,多反应监测(MRM)正离子模式扫描,采用外标法定量。噻呋酰胺和氯啶菌酯在20.47~200μg/kg范围内线性关系良好,其他25种新型杀菌剂在0.02~100μg/kg范围内线性关系良好,相关系数R~2≥0.995 0,加标回收率为70.02%~117.6%,相对标准偏差(RSD)为0.01%~19.62%(n=3)。噻呋酰胺和氯啶菌酯的检出限为6.15~16.67μg/kg,定量限为20.47~55.5μg/kg。其他25种新型杀菌剂的检出限为0.006~4.44μg/kg,定量限为0.02~14.79μg/kg。该方法简便、快速、可靠,可用于谷物、蔬菜、水果中27种新型杀菌剂的快速测定。
[Abstract]:A method for simultaneous determination of 27 new fungicides in cereals, vegetables and fruits by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry (DSPE-LC-MS / MS) was developed. The sample was extracted from acetone acetate solution (volume fraction), dehydrated with anhydrous magnesium sulfate (MgSO4), purified by a mixture of N-propyl ethylenediamine (PSAA) Con 18, anhydrous MgSO4, multiwalled carbon nanotubes (MWCNT), and purified by Cist18 column. Acetonitrile and 0.1% aqueous solution of formic acid (containing 5 mmol/L ammonium acetate) were eluted by gradient, and positive ion mode scanning was used to monitor the reaction. The linear range of thiofuroxime amide and chlorzidime was 20.47 渭 g/kg, and the other 25 new fungicides were linear in the range of 0.02 ~ 100 渭 g/kg, the correlation coefficient was R _ (2) 鈮，

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