| 第 49 卷第 5 期 |  | Vol. 49 No. 5 | | 2019 年 10 月 | Oct 2019 |
|
所屬欄目：分析與測試
超高效液相色譜-串聯(lián)質(zhì)譜法同時(shí)檢測葡萄中吡唑醚菌酯、氟吡菌胺及其代謝物（BAM）殘留 |
| 羅 傲1，陳恒輝1，熊 勝1，張宸宇1，鄧小嵐1，龔道新1，2*
（1. 湖南農業(yè)大學(xué) 資源環(huán)境學(xué)院，湖南 長(cháng)沙 410128；2. 湖南農業(yè)大學(xué) 農業(yè)環(huán)境保護研究所，湖南 長(cháng)沙 410128） |
| 摘 要：建立了超高效液相色譜-串聯(lián)質(zhì)譜（UPLC-MS／MS）快速檢測葡萄中吡唑醚菌酯、氟吡菌胺及其代謝物2，6-二氯苯甲酰胺（BAM）殘留量的方法。葡萄樣品用乙腈提取，過(guò)0.22 μm有機系濾膜后，在電噴霧正離子模式下以多反應監測（MRM）模式測定，基質(zhì)校正標準溶液外標法定量。結果表明：方法的線(xiàn)性范圍為0.05～2.00 mg·kg-1，決定系數（r）＞0.99；在0.05 mg·kg-1、0.50 mg·kg-1和2.00 mg·kg-1，3個(gè)添加水平下，吡唑醚菌酯、氟吡菌胺和2，6-二氯苯甲酰胺（BAM）的平均回收率為91%~97%、91%~93%和94%~100%，相對標準偏差為 4%~7%、1%~3%和2%~3%，定量限為0.05 mg·kg-1。該處理方法準確、簡(jiǎn)單、快速，是葡萄中吡唑醚菌酯、氟吡菌胺和BAM殘留檢測理想的辦法。 |
| 關(guān)鍵詞：超高效液相色譜-串聯(lián)質(zhì)譜（UPLC-MS／MS）；葡萄；吡唑醚菌酯；氟吡菌胺；2，6-二氯苯甲酰胺（BAM） |
| 中圖分類(lèi)號：O657.7 文獻標識碼：A 文章編號：1009-9212（2019）05-0068-05 |
|
| Determination of Pyraclostrobin, Fluopyram and Its Metabolites in Grape by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry |
| LUO Ao1, CHEN Heng-hui1, XIONG Sheng1, ZHANG Chen-yu1, DENG Xiao-lan1, GONG Dao-xin1,2*
(1. College of resources and environment, Hunan Agricultural University, Changsha 410128, China; 2. Institute of agricultural environmental protection, Hunan Agricultural University, Changsha 410128, China) |
| Abstract：A rapid method for the determination of pyraclostrobin ether ester, fluopicolide and its 2,6-dichlorobenzamide(BAM) residues in grapes by ultra-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS) was established. The grape samples were extracted with acetonitrile, and then passed through a 0.22 μm organic membrane. After being monitored by multiple reaction monitoring (MRM) mode under the electrospray ionization mode, the standard solution was corrected by external standard method. The results showed that the linear range of the method was 0.05~2.00 mg·kg-1, and the determination coefficient (r) was > 0.99. At the three levels of 0.05, 0.50 and 2.00 mg·kg-1, the average recovery of pyraclostrobin ether ester, fluopicolide and its 2,6-dichlorobenzamide (BAM) was 91%~97%, 91%~93% and 94%~100%, the relative standard deviation was 4%~7%, 1%~3% and 2%~3%, and the quantitative limit was 0.05 mg·kg-1. The method is stable, accurate and sensitive. It is very suitable for practical operation. This method is accurate, simple and fast, and is an ideal method for the determination of pyrazolyl ester, flupirimide and bam residues in grape. |
| Key words：ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS); grape; pyraclostrobin ether ester; fluopicolide; 2,6-dichlorobenzamide(BAM) |
|
作者簡(jiǎn)介：羅 傲（1994-），男，湖南邵陽(yáng)人，碩士研究生，研究方向：有機污染物檢測（E-mail：452729285@qq.com）。
|
聯(lián) 系 人：龔道新，教授，主要從事有機污染物檢測及治理（E-mail：gdx4910@163.com；E-mail：Author of correspondence）。
|
收稿日期：2019-10-10
|
|