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选择性加速溶剂萃取法结合超高效液相色谱-串联质谱测定杭白菊中19种三唑类杀菌剂
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作者单位
吴慧珍,李晓丹,汪建妹,王向军,杨华,徐杰,吉小凤,钱鸣蓉 1.浙江树人大学生物与环境工程学院2.浙江农林大学林业与生物技术学院 3.浙江省农业科学院农产品质量标准研究所 
基金项目:国家青年科学基金资助项目(LY15B070002)
中文摘要:建立了选择性加速溶剂萃取法结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定杭白菊中19种三唑类杀菌剂的分析方法。样品经乙腈提取,N-丙基乙二胺(PSA)、石墨化碳(GCB)和C18组合净化,萃取液浓缩后以2 mmol/L甲酸铵(含0.1%甲酸)和甲醇为流动相,采用BEH C18色谱柱分离,在电喷雾正离子模式下以多反应监测模式进行检测,基质匹配外标法定量。19种三唑类杀菌剂在1.0~100.0 μg/L范围内线性关系良好,相关系数(r2)≥0.99,方法检出限及定量下限分别为0.6~3.0 μg/kg和2.1~10.0 μg/kg。在10、50、100 μg/kg加标水平下,目标物的回收率为70.3%~95.3%,相对标准偏差为0.60%~12%。该方法操作简单,样品提取和净化可同步完成,自动化程度高,重复性好,灵敏度能够满足日常检测要求。
中文关键词:选择性加速溶剂萃取  超高效液相色谱-串联质谱(UPLC-MS/MS)  三唑类杀菌剂  杭白菊
 
Determination of 19 Triazole Fungicides in Chrysanthemum morifolium by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Combined with Selective Accelerated Solvent Extraction
Abstract:A selective accelerated solvent extraction method combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of 19 triazole fungicides in Chrysanthemum morifolium.The sample was extracted with acetonitrile,and the mixed dispersive sorbents(PSA,GCB and C18) were dispersed in the extract to reduce the effects of interfering components during the extraction procedure.After concentration,the extract was separated on a BEH C18 column using 2 mmol/L ammonium formate containing 0.1% formic acid and methanol as mobile phases,and detected under multi-reaction monitoring mode in electrospray positive ion mode.Matrix matched method was used for quantitative analysis.There were good linear relationships for 19 triazole fungicides in the range of 1.0-100.0 μg/L with their correlation coefficients(r2) not less than 0.99.The limits of detection and quantitation were 0.6-3.0 μg/kg and 2.1-10.0 μg/kg,respectively.Under the optimal conditions,the average recoveries for those compounds at three spiked levels of 10,50 and 100 μg/kg ranged from 70.3% to 95.3%,with relative standard deviations(RSD) of 0.60%-12%.This method is simple,reproducible and sensitive,and is applicable for the simultaneous determination of triazole fungicides in Chrysanthemum morifolium samples.
Key Words:selective accelerated solvent extraction  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  triazole fungicide  Chrysanthemum morifolium
引用本文:吴慧珍,李晓丹,汪建妹,王向军,杨华,徐杰,吉小凤,钱鸣蓉.选择性加速溶剂萃取法结合超高效液相色谱-串联质谱测定杭白菊中19种三唑类杀菌剂[J].分析测试学报,2019,(6):661-667.
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