气相色谱-质谱法测定韭菜中2,4-D丁酯  

Determination of 2,4-D-butyl Ester in Chinese Leek by Gas Chromatography-Mass Spectrometry

作　　者：曹艳平[1] 解力[1] 杨剑影[1] 

机构地区：[1]山东省疾病预防控制中心,山东济南250014

出　　处：《质谱学报》2006年第1期33-35,共3页Journal of Chinese Mass Spectrometry Society

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.

关 键 词：2 4-D丁酯 气相色谱-质谱 净化 

分 类 号：O657.63[理学—分析化学] S482.3[理学—化学]