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| 氟吡菌胺及其代谢物在黄瓜中的残留研究 |
| Residue of fluopicolide and its metabolites in cucumber |
| 投稿时间：2019-11-06 修订日期：2020-02-06 |
| DOI： |
| 中文关键词: QuEChERS 高效液相色谱 氟吡菌胺 2,6-二氯苯甲酰胺 残留 |
| 英文关键词: QuEChERS high performance liquid chromatography fluopicolide 2,6-dichlorobenzamide residue |
| 基金项目:中国农业科学院科技创新工程协同创新任务（CAAS-XTCX2016015) |
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| 中文摘要: |
| 摘要：为评价氟吡菌胺及其代谢物在黄瓜上的安全性，建立了同时检测氟吡菌胺及其代谢物2,6-二氯苯甲酰胺的高效液相色谱-串联质谱法。前处理方法采用乙腈提取，无水硫酸镁、石墨化碳（GCB）和乙二胺-N-丙基硅烷（PSA）分散固相净化，应用高效液相色谱-串联质谱仪多反应离子监测（MRM）检测。研究结果表明，在0.05-5 mg?kg-1的加标范围内，氟吡菌胺和2,6-二氯苯甲酰胺的平均回收率分别为82%~98%和90%~100%。相对标准偏差（RSD，n=5）分别为1.6%~7.9%和3.2 %~9.4 %。定量检出限（LOQ）为0.05 mg?kg-1。最终残留试验表明：在氟吡菌胺推荐剂量（735 g?hm-2）下，施药3次，距最后一次施药间隔1、3和5 d时，氟吡菌胺及2,6-二氯苯甲酰胺在黄瓜上的最高残留量均小于0.05 mg?kg-1，低于我国规定的氟吡菌胺在黄瓜中的最大残留限量0.5 mg?kg-1。 |
| 英文摘要: |
| Abstract: In order to evaluate the safety of fluopicolide and its metabolites on cucumber, a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of fluopicolide and its metabolite 2,6-dichlorobenzamide. The pretreatment method was carried out by acetonitrile extraction, anhydrous magnesium,sulfate,graphitized carbon (GCB) and ethylenediamine-N-propylsilane (PSA) dispersed solid phase purification, and then detected by multi-reaction ion monitoring (MRM) with high performance liquid chromatography-tandem mass spectrometry. Three concentrations of fluopicolide and 2,6-dichlorobenzamide standard solutions were added to the cucumber samples. The results showed that the average recovery rates were 82%~98% and 90%~100%, respectively. The relative standard deviations (RSD, n=5) were 1.6%~7.9% and 3.2%~9.4%, respectively. The limit of detection (LOQ) is 0.05 mg?kg-1, which is simpler, faster and safer than existing assays. The final residue test indicated that the drug was applied 3 times at the recommended dose of fluopicolide (735 g?hm-2). The maximum residual amount ?of fluopicolide and 2,6-dichlorobenzamide on cucumber was less than 0.05 mg?kg-1from the last application interval of 1, 3 and 5 days. Both are lower than the maximum residue limit of 0.5 mg?kg-1 of fluopicolide in cucumber in China. |
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