| 魏 进, 张 盈, 曾 雪, 高 迪, 龙家寰, 龚庆东, 段婷婷*.超高效液相色谱-串联质谱法快速检测核桃中戊唑醇､肟菌酯及肟菌酸残留[J].植物保护,2021,47(4):134-140. |
| 超高效液相色谱-串联质谱法快速检测核桃中戊唑醇､肟菌酯及肟菌酸残留 |
| Simultaneous determination of residue of tebuconazole, trifloxystrobin and its metabolite trifloxystrobin acid in walnut by UHPLC-MS/MS |
| 投稿时间：2020-05-08 修订日期：2020-06-28 |
| DOI：10.16688/j.zwbh.2020236 |
| 中文关键词: 戊唑醇 肟菌酯 肟菌酸 核桃 超高效液相色谱-串联质谱 残留检测 |
| 英文关键词:tebuconazole trifloxystrobin trifloxystrobin acid walnut UHPLC-MS/MS pesticide residue |
| 基金项目:黔农科院基础性公益性专项([2020]15号) |
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| 中文摘要: |
| 建立了超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定戊唑醇?肟菌酯及其代谢物肟菌酸在核桃中的残留检测方法?样品中待测农药组分采用2%乙酸乙腈溶剂振荡提取, 弗罗里硅土(florisil)净化, 利用乙腈和0.2%甲酸水作为流动相梯度洗脱, C18色谱柱分离, 在多反应监测模式下定量分析, 基质外标法定量?结果表明:戊唑醇添加水平为5~500 μg/kg时, 戊唑醇在核桃中添加回收率为80.3%~100.8%, 相对标准偏差(RSD)为2.5%~11.7%; 肟菌酯和肟菌酸添加水平为2~200 μg/kg时, 肟菌酯在核桃中添加回收率为91.1%~102.9%, 相对标准偏差(RSD)为1.7%~12.5%; 肟菌酸在核桃中添加回收率为91.7%~101.9%, 相对标准偏差(RSD)为3.7%~9.2%?戊唑醇?肟菌酯和肟菌酸溶剂标准曲线和基质标准曲线在1~1 000 μg/L范围内线性关系良好, 相关系数均大于0.99?戊唑醇定量限为5 μg/kg, 肟菌酯和肟菌酸定量限均为2 μg/kg?实际样品检测中, 戊唑醇残留结果为6~99 μg/kg, 肟菌酯残留结果为<2~103 μg/kg, 肟菌酸均小于检测限?该方法操作简便?快捷和准确, 满足在核桃实际样品中戊唑醇?肟菌酯及其代谢物肟菌酸的残留检测要求? |
| 英文摘要: |
| An ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was established for simultaneous determination of residue of tebuconazole, trifloxystrobin and its metabolite trifloxystrobin acid in walnut. Pesticide components under test in the sample were extracted by 2% acetic acid acetonitrile solvent oscillation extraction, purified by silica in florisil, eluted using acetonitrile and 0.2% formic acid water as mobile phase gradient elution, and separated by C18 chromatographic column. The pesticide components were quantitatively analyzed in multiple reaction monitoring mode by quantitative matrix external standard method. The results showed that when the spiked level of tebuconazole was 5-500 μg/kg, the recovery of tebuconazole in walnut was 80.3%-100.8%, and the relative standard deviation (RSD) was 2.5%-11.7%.When the spiked level of trifloxystrobin and trifloxystrobin acid were 2-200 μg/kg, the recovery of trifloxystrobin in walnut was 91.1%-102.9%, and the RSD was 1.7%-12.5%, the recovery of trifloxystrobin acid in walnut was 91.7%-101.9%, and the RSD was 3.7%-9.2%. The linear relationship between the solvent standard curve and the matrix standard curve was good in the range of 1-1 000 μg/L, and the correlation coefficient was all higher than 0.99. The quantitative limit of tebuconazole was 5 μg/kg, while that of trifloxystrobin and trifloxystrobin acid was 2 μg/kg. In the actual sample detection, the residue of tebuconazole was 6-99 μg/kg, the residue of trifloxystrobin were < 2-103 μg/kg, while the residue of its metabolite trifloxystrobin acid was less than the detection limit. The method is simple, fast and accurate, which can meet the requirement of residue detection of tebuconazole, trifloxystrobin and its metabolite trifloxystrobin acid in walnut samples. |
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