分散固相萃取-液相色譜-串聯(lián)質(zhì)譜法測(cè)定谷物、蔬菜、水果中27種新型殺菌劑
發(fā)布時(shí)間:2018-05-18 03:16
本文選題:液相色譜-串聯(lián)質(zhì)譜 + 分散固相萃取��; 參考:《色譜》2017年05期
【摘要】:建立了同時(shí)檢測(cè)谷物、蔬菜和水果中27種新型殺菌劑的分散固相萃取-液相色譜-串聯(lián)質(zhì)譜(DSPE-LC-MS/MS)分析方法。樣品經(jīng)1%(體積分?jǐn)?shù))乙酸丙酮溶液提取,以無(wú)水硫酸鎂(MgSO_4)脫水,經(jīng)N-丙基乙二胺(PSA)、C_(18)、無(wú)水MgSO_4、多壁碳納米管(MWCNT)混合凈化劑凈化,經(jīng)C_(18)色譜柱分離,用乙腈和體積分?jǐn)?shù)為0.1%的甲酸水溶液(含5 mmol/L乙酸銨)梯度洗脫,多反應(yīng)監(jiān)測(cè)(MRM)正離子模式掃描,采用外標(biāo)法定量。噻呋酰胺和氯啶菌酯在20.47~200μg/kg范圍內(nèi)線性關(guān)系良好,其他25種新型殺菌劑在0.02~100μg/kg范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)R~2≥0.995 0,加標(biāo)回收率為70.02%~117.6%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為0.01%~19.62%(n=3)。噻呋酰胺和氯啶菌酯的檢出限為6.15~16.67μg/kg,定量限為20.47~55.5μg/kg。其他25種新型殺菌劑的檢出限為0.006~4.44μg/kg,定量限為0.02~14.79μg/kg。該方法簡(jiǎn)便、快速、可靠,可用于谷物、蔬菜、水果中27種新型殺菌劑的快速測(cè)定。
[Abstract]:A method for simultaneous determination of 27 new fungicides in cereals, vegetables and fruits by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry (DSPE-LC-MS / MS) was developed. The sample was extracted from acetone acetate solution (volume fraction), dehydrated with anhydrous magnesium sulfate (MgSO4), purified by a mixture of N-propyl ethylenediamine (PSAA) Con 18, anhydrous MgSO4, multiwalled carbon nanotubes (MWCNT), and purified by Cist18 column. Acetonitrile and 0.1% aqueous solution of formic acid (containing 5 mmol/L ammonium acetate) were eluted by gradient, and positive ion mode scanning was used to monitor the reaction. The linear range of thiofuroxime amide and chlorzidime was 20.47 渭 g/kg, and the other 25 new fungicides were linear in the range of 0.02 ~ 100 渭 g/kg, the correlation coefficient was R _ (2) 鈮,
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