發(fā)布時(shí)間：2018-06-15 13:46

  本文選題：殺菌劑 + 固相萃取　； 參考：《分析化學(xué)》2017年08期

【摘要】：利用固相萃取-液相色譜-飛行時(shí)間質(zhì)譜(SPE-LC-Q-TOF/MS)技術(shù)建立了谷物、蔬菜和水果中25種殺菌劑農(nóng)藥殘留的快速篩查和確證檢測(cè)方法。樣品經(jīng)1%(V/V)乙酸-乙腈溶液提取,經(jīng)Crabon/NH_2柱凈化,乙腈-甲苯(3∶1,V/V)洗脫,C_(18)色譜柱分離,乙腈和0.1%甲酸溶液(含5 mmol/L乙酸銨)梯度洗脫,采用LC-Q-TOF/MS檢測(cè),外標(biāo)法定量。建立了25種殺菌劑的一級(jí)精確質(zhì)量數(shù)據(jù)庫(kù)和二級(jí)譜圖庫(kù),通過化合物的精確質(zhì)量數(shù)、保留時(shí)間、同位素峰分布、同位素比例等信息對(duì)檢測(cè)結(jié)果進(jìn)行自動(dòng)檢索,在無(wú)對(duì)照標(biāo)準(zhǔn)品的情況下實(shí)現(xiàn)了25種農(nóng)藥的定性鑒定。結(jié)果表明,25種殺菌劑在0.02~200μg/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)R2≥0.9950,加標(biāo)回收率在71.8%~114.0%之間,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為0.1%~21.3%(n=3)。25種殺菌劑檢出限為0.01~5.00μg/kg,定量限為0.02~20.00μg/kg。本方法簡(jiǎn)便、快速、可靠,可用于谷物、蔬菜、水果中25種殺菌劑的快速篩查。
[Abstract]:The SPE-LC-Q-TOF / MS technique of SPE-LC-Q-TOF / MS was used to establish a rapid screening and identification method for the pesticide residues of 25 fungicides in cereals, vegetables and fruits. The samples were extracted by acetonitrile solution of V / V, purified by Crabon / NH _ 2 column, eluted by acetonitrile-toluene 3: 1 V / V) column, separated by acetonitrile and 0.1% formic acid solution (containing 5 mmol / L ammonium acetate) by gradient elution, detected by LC-Q-TOF / MS and quantified by external standard method. The first order accurate mass database and the second order spectrum map database of 25 kinds of fungicides were established. The detection results were automatically retrieved by the information of accurate mass number, retention time, isotope peak distribution and isotope ratio of compounds. The qualitative identification of 25 pesticides was carried out without the control standard. The results showed that the linear range of 25 fungicides was within the range of 0.02 ~ 200 渭 g / L, the correlation coefficient R ~ 2 鈮，

本文編號(hào)：2022200