摘要
以乙腈超声提取韭菜中2,4-D丁酯,80℃水浴中氮气吹至近干,以丙酮溶解,以活性炭、弗罗里硅土、氧化铝柱净化,以气相色谱-质谱选择m/z162、175、185、276四个碎片离子进行定性定量分析。2,4-D丁酯在0.002~1.0μg/mL成线性(r=0.9999),2种不同加标浓度0.01和1.0μg/mL下2,4-D丁酯平均回收率分别为88.2%、94.3%,相对标准偏差分别为6.93%、6.89%.样品中最低检出浓度(S/N=3)为0.02μg/kg。本方法适用于韭菜等蔬菜和水果中2,4-D丁酯的测定。
A method of determination of 2,4-D-butyl ester in Chinese Leek by GC/MS is established. 2,4-D-butyl ester in Chinese Leek was extracted with acetonitrile by ultrasonic wave. The extract was warmed with water at 80℃ and blowed with nitrogen gas until it got near to dryness. Then it was dissolved in acetone and cleaned-up by florisil-charcoal alumina glass column. Retention time and specific ions were used to identify 2,4-D-butyl ester. The selective fragments were m/z 162, 175,185, 276, respectively. The calibration curve of 2,4-D-butyl ester was linear (correlatiom coefficient: 0. 999 9) within the range of 0. 002- 1.0μg/mL. The recoveries (spiking at 0. 01μg/mL and 1. 0μg/mL ) were 88. 2%, 94.3%, respectively. The relative standard deviations (RSD) of the method was 〈10% for each case, and the limit of detection (LOD), defined in termes of 3 times baseline noise was 0. 02μg/kg. The method is suitable for determining 2,4-D-butyl ester in Chinese Leek and other vegetables and fruits.
出处
《质谱学报》
EI
CAS
CSCD
2006年第1期33-35,共3页
Journal of Chinese Mass Spectrometry Society
关键词
2
4-D丁酯
气相色谱-质谱
净化
2,4-D-butyl ester, gas chromatography-mass spectrometry(GC/MS)
cleanedup
作者简介
曹艳平(1963-),女(汉族)。山东临沂人。副主任技师.从事食品理化分析。E-mail:cap0124@sina.com