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  

Determination of 27 new fungicides in cereals,vegetables and fruits by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry

作　　者：崔春艳[1,2] 张红医[1] 吴兴强[1,2] 范春林[2] 李帅[2,3] 陈辉[2] 常巧英[2] 庞国芳[2] 

机构地区：[1]河北大学化学与环境科学学院,河北保定071002 [2]中国检验检疫科学研究院,北京100176 [3]山东农业大学食品科学与工程学院,山东泰安271018

出　　处：《色谱》2017年第5期487-494,共8页Chinese Journal of Chromatography

基　　金：国家科技基础性工作专项(2015FY111200)~~

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。A method for simultaneous determination of 27 new fungicides in cereals, vegetables and fruits using dispersive solid phase extraction and liquid chromatography-tandem mass spec-trometry （DSPE- LC-MS/MS） was developed. Samples were extracted with acetone containing 1% （v/v ） acetic acid,purified by a mixed sorbent of ethylenediamine善 propylsilane （PSA）, C18,anhydrous magnesium sulfate （MgSO#） and multi-walled carbon nanotubes （MWCNT）, separated by a reversed phase C18 column,and gradiently eluted with acetonitrile and 0. 1% （v/v ） formic acid solution （containing 5 mmol/L ammonium acetate）. Anhydrous magnesium sulfate was used as a dewatering agent. The positive ion mode and multiple reaction monitoring （MRM） mode were used in the analysis,and the analytes were quantified by external standard method. Thif^uzamide and triclopyricarbe showed good linearities in the range of 20.47-200 pg/kg,and the limits of detection （LODs） and the limits of quantification （LOQs） were 6. 15-16. 67 and 20. 47-55. 5 μg/ kg , respectively. The other 25 new fungicides showed good lineari-ties in the range of 0. 02-100 μg/ kg , and the LODs and LOQs were 0. 006-4. 44 and 0. 02-14. 79 pg/kg, respectively. The linear relative coefficients were not less than 0. 995 0. The recoveries were in the range of 70. 02%-117. 6 % and the relative standard deviations （RSDs） ranged from 0.01% to 19.62% （ n = 3）. The method has the advantages of simplicity, rapidity, high sensitivity and better purification effect. It is suitable for the rapid determination of the 27 new fungicides in cereals,vegetables and fruits.

关 键 词：液相色谱-串联质谱 分散固相萃取 新型杀菌剂 谷物 蔬菜 水果 

分 类 号：O658[理学—分析化学]