固相萃取-液相色譜-四極桿飛行時間質譜法快速篩查禽蛋及蛋制品中氟蟲腈及其代謝物
發(fā)布時間：2018-10-14 11:03
【摘要】：建立了液相色譜-四極桿飛行時間質譜(LC-QTOF MS)測定禽蛋及蛋制品中氟蟲腈及其代謝物的快速篩查方法。樣品經(jīng)酸性乙腈提取,PRiME HLB SPE柱凈化,Poroshell 120 EC C18色譜柱(150 mm×3 mm,2.7μm)分離,以水-乙腈為流動相,梯度洗脫,負離子模式下測定,以乙蟲腈為內標定量。實驗中建立了一級精確質量和二級碎片離子質譜數(shù)據(jù)庫,并且對4種禽蛋及蛋制品的基質效應進行了考察。結果表明,氟蟲腈及其代謝物在0.1~5μg/L范圍內線性關系良好,相關系數(shù)(r2)均大于0.99。方法的檢出限(LOD,S/N3)和定量限(LOQ,S/N10)分別為0.2μg/kg和1μg/kg。在不同基質中,氟蟲腈及其代謝物在1、2和5μg/kg的添加水平下平均加標回收率為82.6%~98.1%,相對標準偏差為3.8%~9.9%(n=6)。該方法有效消除了液相色譜-四極桿飛行時間質譜檢測過程中的離子化抑制效應,靈敏度和準確度高,適用于雞蛋、雞蛋面、蛋糕和蛋黃醬中氟蟲腈、氟蟲腈砜、氟蟲腈亞砜和氟甲腈的快速篩查。
[Abstract]:A rapid screening method for determination of fluronitrile and its metabolites in eggs and egg products by liquid chromatography-quadrupole time of flight mass spectrometry (LC-QTOF MS) was established. The samples were purified on, PRiME HLB SPE column with acid acetonitrile and separated by Poroshell 120 EC C18 column (150 mm 脳 3 mm,2.7 渭 m). The samples were separated by aqueous acetonitrile as mobile phase, gradient eluted, determined by negative ion mode, and determined with acetonitrile as internal standard. The first order accurate mass and second order fragment ion mass spectrometry databases were established and the matrix effects of four kinds of poultry eggs and egg products were investigated. The results showed that there was a good linear relationship between fluronitrile and its metabolites in the range of 0.1 渭 g / L, and the correlation coefficient (R2) was higher than 0.99. The detection limit (LOD,S/N3) and quantitative limit (LOQ,S/N10) of the method were 0.2 渭 g/kg and 1 渭 g / kg, respectively. The average recoveries of fluoronitrile and its metabolites in different substrates were 82.6% and 98.1 at the addition level of 1 渭 g/kg and 5 渭 g/kg respectively, and the relative standard deviation was 3.8% (n = 6). This method can effectively eliminate the inhibition effect of ionization in the detection process of liquid chromatography-quadrupole time-of-flight mass spectrometry, and has high sensitivity and accuracy. It is suitable for flufenonitrile and flunonitrile in eggs, egg noodles, cakes and mayonnaise. Rapid screening of fluronitrile sulfoxide and fluoronitrile.
【作者單位】： 上海出入境檢驗檢疫局;江蘇出入境檢驗檢疫局;
【基金】：上海市科委2015年度科學儀器領域項目(15142201700)~~
【分類號】：O657.63;TS253.7
本文編號：2270261
[Abstract]:A rapid screening method for determination of fluronitrile and its metabolites in eggs and egg products by liquid chromatography-quadrupole time of flight mass spectrometry (LC-QTOF MS) was established. The samples were purified on, PRiME HLB SPE column with acid acetonitrile and separated by Poroshell 120 EC C18 column (150 mm 脳 3 mm,2.7 渭 m). The samples were separated by aqueous acetonitrile as mobile phase, gradient eluted, determined by negative ion mode, and determined with acetonitrile as internal standard. The first order accurate mass and second order fragment ion mass spectrometry databases were established and the matrix effects of four kinds of poultry eggs and egg products were investigated. The results showed that there was a good linear relationship between fluronitrile and its metabolites in the range of 0.1 渭 g / L, and the correlation coefficient (R2) was higher than 0.99. The detection limit (LOD,S/N3) and quantitative limit (LOQ,S/N10) of the method were 0.2 渭 g/kg and 1 渭 g / kg, respectively. The average recoveries of fluoronitrile and its metabolites in different substrates were 82.6% and 98.1 at the addition level of 1 渭 g/kg and 5 渭 g/kg respectively, and the relative standard deviation was 3.8% (n = 6). This method can effectively eliminate the inhibition effect of ionization in the detection process of liquid chromatography-quadrupole time-of-flight mass spectrometry, and has high sensitivity and accuracy. It is suitable for flufenonitrile and flunonitrile in eggs, egg noodles, cakes and mayonnaise. Rapid screening of fluronitrile sulfoxide and fluoronitrile.
【作者單位】： 上海出入境檢驗檢疫局;江蘇出入境檢驗檢疫局;
【基金】：上海市科委2015年度科學儀器領域項目(15142201700)~~
【分類號】：O657.63;TS253.7
【相似文獻】
相關期刊論文 前9條
1 丁立平;劉微;方光偉;郭菁;鄭鈴;張睿;陳志濤;;改進QuChERS-氣質聯(lián)用法測定蔬菜中氟蟲腈和丁烯氟蟲腈殘留量[J];分析試驗室;2013年08期
2 許行義;潘荷芳;劉勁松;鄒巧莉;楊寅森;鐘光劍;;氣相色譜法測定水中吡蟲啉和氟蟲腈[J];環(huán)境監(jiān)測管理與技術;2011年04期
3 唐晗簫;唐光傳;;160g/L氟蟲脲+100g/L氟蟲腈懸浮劑的高效液相色譜檢測[J];世界農(nóng)藥;2014年01期
4 周昱;徐敦明;陳達捷;張志剛;鄭向華;方恩華;;固相微萃取-氣相色譜法和氣相色譜-質譜法測定茶葉中氟蟲腈及其代謝物殘留[J];色譜;2011年07期
5 丁立平;;氣相色譜-質譜聯(lián)用儀測定茶葉中氟蟲腈的不確定度評定[J];分析測試技術與儀器;2011年03期
6 涂立生,黃偉東;氟蟲腈的氣相色譜分析[J];現(xiàn)代農(nóng)藥;2002年06期
7 付如剛;曹成;王永生;任雪峰;劉青;;氟蟲腈在B-Z化學振蕩體系中的分析檢測[J];化學世界;2013年06期
8 馬超;徐妍;郭鑫宇;羅湘仁;吳學民;;聚羧酸型梳狀共聚物超分散劑在氟蟲腈顆粒界面的吸附性能[J];高等學�；瘜W學報;2013年06期
9 吳培慧;孫有娥;郝媛媛;邢海燕;李一辰;;ICP-OES法同時測定蛋制品中鉛、鋅、銅含量[J];廣州化工;2014年11期
，本文編號：2270261
本文鏈接：http://sikaile.net/kejilunwen/huaxue/2270261.html
教材專著
