第 46 卷第 3 期Vol. 46 No. 3
2016 年 6 月Jun 2016

所属栏目:分析与测试

气相色谱法测定样品中丁二醛的含量
方 燕1,韩海平1,张芝平1,董建生1,毕 强1,徐晓勇2,李 忠2,叶振君1,2* (1. 上海生农生化制品有限公司,上海 201619;2. 华东理工大学,上海 200237)
摘 要:建立了以2,5-二甲氧基四氢呋喃为原料水解合成的丁二醛样品的气相色谱测定法。选用HP-FFAP毛细管柱,柱温80℃,流速 20 mL/min,以二氧六环为内标物,采用内标标准曲线法定量分析丁二醛含量。结果表明,方法在8.0~40.0 g/L的浓度范围内呈良好线性关系(r=0.999 94),相对标准偏差RSD为0.52%,加标回收率在96.23%~102.87%之间。该法简便、快速,具有良好的精密度和准确度,可用于合成样品中丁二醛含量的测定。
关键词:气相色谱法;丁二醛;2,5-二甲氧基四氢呋喃
中图分类号:O657.7+1  文献标识码:A  文章编号:1009-9212(2016)03-0073-04
Determination of Succinaldehyde Using Gas Chromatography
FANG Yan1, HAN Hai-ping1, ZHANG Zhi-ping1, DONG Jian-sheng1, BI Qiang1, XU Xiao-yong2, LI Zhong2, YE Zhen-jun1,2* (1. Shanghai Shengnong Pesticide Co., Ltd., Shanghai 200619, China; 2. East China University of Science and Technology, Shanghai 200237, China)
Abstract:A GC method was established for monitoring the succinaldehyde in the samples taking from the preparation reaction using 2,5-dimethoxy-dihydrofuran as the starting material. The content of succinaldehyde was quantitatively analyzed using internal standard curve method with a HP-FFAP capillary column and dioxane as internal standard substance. In this method, the flow rate was 20 mL/min and the column temperature was 80℃. The results indicated that this method had a good linear relation(r=0.999 94) in a concentration range from 8.0 g/L to 40.0 g/L with an average RSD of 0.52% and a recovery rate range from 96.2% to 102.8%. This method has been proved to be simple, rapid with good accuracy and reliability, which could be applicable in the monitoring of succinaldehyde in the samples taking from the preparation reaction using 2,5-dimethoxy-dihydrofuran as the starting material.
Key words:gas chromatography; succinaldehyde; 2,5-dimethoxy-dihydrofuran
基金项目: 中国博士后面上项目资助(2016M590329),上海市优秀技术带头人计划资助(16XD1422300)。
作者简介: 方 燕(1987-),女,安徽黄山人,工程师,硕士,主要从事农药检测与质量控制(E-mail:fy@shengnong-pesticide.com.cn)。
联 系 人:叶振君,高级工程师,主要从事新农药创制与产品开发(E-mail:zjyee@163.com)。
收稿日期: 2016-05-1