摘要
建立了一种同时测定果蔬中啶酰菌胺、吡噻菌胺、吡唑萘菌胺、氟唑菌酰胺、联苯吡菌胺、氟唑环菌胺、氟唑菌 苯胺和氟吡菌酰胺8种新型琥珀酸脱氢酶抑制剂类杀菌剂残留量的液相色谱-串联质谱方法.通过比较乙二胺-N- 丙基硅烷（PSA）和十八烷基键合硅胶吸附剂（ C18 ） 两种分散固相萃取剂不同添加剂量下的吸附作用和净化效果, 优化QuEChERS方法净化过程,以乙腈-0. 1% （ 体积分数）甲酸水溶液为流动相进行梯度洗脱,使 8 种目标化合物 在 Poroshell 120 EC-C18色谱柱上分离,经电喷雾正/负双离子扫描、多反应监测模式质谱检测,外标法定量.8 种 目标化合物在0. 5～500. 0 μg/L范围内线性关系良好,相关系数均大于0. 998,方法检出限为0. 2～1. 7 μg/kg,定量限为0.5～5.0 μg/kg.各种目标化合物在8 种基质中3 个添加水平（ 5 .0、 25 .0和 125.0 μg / k g ）下的回收率为 71.4%～121.3%,相对标准偏差（RSD,n=6）为 0.8%～17.2%.该方法操作简单、净化效果好,适用于果蔬中新型琥珀酸脱氢酶抑制剂类杀菌剂的快速检测.
A method was developed for the simultaneous determination of eight novel succinate dehydrogenase inhibitor fungicides （boscalid, penflufen, bixafen,sedaxane,fluopyram, pen- thiopyrad, isopyrazam, fluxapyroxad） residues in vegetables and fruits by liquid chromatogra-phy-tandem mass spectrometry （LC-MS/MS） coupled with modified QuEChERS. The amount of the two solid phase extraction agents （octadecyl bonded silica （C18） and primary secondary amine （PSA）） in QuEChERS method was optimized according to their adsorption and purifica-tion capacities. The eight compounds were extracted from samples by acetonitrile and purified by solid phase extraction agents. The eight compounds were separated on a Poroshell 120 EC-C18 column by the gradient elution using acetonitrile- 0. 1% （v/v） formic acid aqueous solu-tion as mobile phases, detected by MS/MS with positive/negative electrospray ionization （ESI＋/ESI-） in multiple reaction monitoring （MRM） mode,and finally quantified by external standard method. The correlation coeffcients （r ） of the eight compounds were all above 0. 998 in the mass concentration ranging from 0. 5 to 500. 0 μg/L. The limits of detection and the limits of quantification of the method were 0. 2-1. 7 μg/kg and 0. 5-5. 0 μg/kg, respectively. The recoveries of the eight analytes spiked at three levels （5. 0, 25. 0 and 125. 0 μg/kg） in eight matrices ranged from 71. 4% to 121.3% with the relative standard deviations （RSDs, n = 6 ） from 0. 8% to 17. 2%. The method is easy to operate and with good purification effect. It can be applied to the rapid determination of the novel succinate dehydrogenase inhibitor fungicides in vegetables and fruits.
出处
《色谱》
CAS
CSCD
北大核心
2016年第11期1070-1076,共7页
Chinese Journal of Chromatography
基金
国家农产品质量安全风险评估项目(GJFP2016001001)
中央级公益性科研院所基本科研业务费专项资金项目(2014RG006)~~
关键词
液相色谱-串联质谱
QUECHERS
新型琥珀酸脱氢酶抑制剂类杀菌剂
蔬菜
水果
liquid chromatography-tandem mass spectrometry （LC-MS/MS）
QuEChERS
novel succinate dehydrogenase inhibitor （SDHI） fungicides
vegetables
fruits
