优化的QuEChERS-超高效液相色谱-串联质谱法检测黄瓜中29种杀菌剂残留
投稿时间:2017-05-31      点此下载全文 HTML
引用本文:蒋建功,杨松,林琎,周秀玲,孙丰收,慕卫,等.优化的QuEChERS-超高效液相色谱-串联质谱法检测黄瓜中29种杀菌剂残留[J].农药学学报,2017,19(6):735-743.
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蒋建功 山东农业大学 植物保护学院 农药毒理与应用技术省级重点实验室, 山东 泰安 271018;山东农业大学 农药环境毒理研究中心, 山东 泰安 271018  
杨松 山东农业大学 农药环境毒理研究中心, 山东 泰安 271018  
林琎 山东农业大学 植物保护学院 农药毒理与应用技术省级重点实验室, 山东 泰安 271018;山东农业大学 农药环境毒理研究中心, 山东 泰安 271018  
周秀玲 山东农业大学 农药环境毒理研究中心, 山东 泰安 271018  
孙丰收 山东农业大学 农药环境毒理研究中心, 山东 泰安 271018  
慕卫 山东农业大学 植物保护学院 农药毒理与应用技术省级重点实验室, 山东 泰安 271018;山东农业大学 农药环境毒理研究中心, 山东 泰安 271018 muwei@sdau.edu.cn 
基金项目:国家重点研发计划(2016YFD0200500);国家自然科学基金(31572040)
中文摘要:建立了采用QuEChERS-超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测黄瓜中29种杀菌剂残留的分析方法。黄瓜样品经乙腈提取和前处理方法优化,以乙二胺-N-丙基硅烷(PSA)和石墨化碳黑(GCB)为分散固相萃取(dSPE)吸附剂,涡旋提取后过滤膜,采用UPLC-MS/MS检测。结果表明:在0.000 1~0.05 mg/kg范围内,29种杀菌剂的质量浓度与相应的峰面积间呈良好的线性关系,相关系数均大于0.996,定量限(LOQ)在0.000 1~0.01 mg/kg之间;在0.01、0.05和0.5 mg/kg添加水平下,29种杀菌剂的平均回收率均在74%~112%之间,相对标准偏差(RSD)在1.1%~17%之间(n=5)。经实际样品检测验证,该方法快速、简便、可靠、高效,且成本低廉,适用于同时检测黄瓜中29种杀菌剂的残留量。
中文关键词:QuEChERS  超高效液相色谱-串联质谱  黄瓜  杀菌剂  残留
 
Determination of 29 fungicide residues in cucumber by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry
Abstract:A multiresidue method was developed for the simultaneous determination of 29 fungicides in cucumber by using modified QuEChERS-ultra performance liquid chromatography-tandem mass spetrometry (UPLC-MS/MS). The cucumber samples were first extracted by acetonitrile and the preprocessing method was optimized. The N-(n-propyl) ethylenediamine (PSA) and graphitized carbon blacks (GCB) were used as adsorbent materials in the dispersive solid phase extraction (dSPE) process. The extraction was carried out, and the samples were detected by UPLC-MS/MS. The results demonstrate the concentrations of 29 fungicides have a good linear relationship with the corresponding peak area in the range of 0.000 1-0.05 mg/kg at 0.01, 0.05 and 0.5 mg/kg spiked levels. The correlation coefficients of all fungicides are above 0.996.The average recoveries of these pesticides rang from 74% to 112%, with RSDs rang from 1.1%-17% (n=5). The LOQs (limit of quantification) are 0.000 1-0.01 mg/kg. This method has been successfully applied in real samples. This method is simple, rapid, robust, efficient and inexpensive. It is suitable for the simultaneous determination of 29 fungicides in cucumber.
Key words:QuEChERS  ultra performance liquid chromatography-tandem mass spetrometry (UPLC-MS/MS)  cucumber  fungicide  residue
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