涡旋辅助衍生化-气相色谱法测定水果中2,4-滴残留
Rapid determination of 2,4-Dichlorophenoxyacetic acid residues in fruits by vortex-assisted derivatization and gas chromatography
李霞 1王艳丽 1鞠香 1李海霞 1李洁 1申中兰 1徐大玮 1刘艳明1
作者信息
- 1. 山东省食品药品检验研究院,国家市场监督重点实验室(肉及肉制品监管技术),产业技术基础公共服务平台,济南 250101
- 折叠
摘要
水果在生长和运输过程中使用2,4-滴而造成的残留药害,严重影响水果的质量.为提高水果中2,4-滴检测效率及节能降耗的需要,本文建立了涡旋辅助衍生化结合气相色谱-电子捕获检测器(GC-ECD)测定水果中2.4滴的快速检测方法.样品经乙腈提取,氮气吹干后加入140μL甲醇和40μL浓硫酸涡旋衍生化1 min,采用正己烷提取衍生化产物,饱和氯化钠水溶液净化,经DB-17色谱柱分离和GC-ECD检测分析,外标法定量.结果显示2,4-滴在1.0～1000μg/L时保持良好的线性关系(r=0.99993),方法检出限为0.001 mg/kg,定量限为0.003 mg/kg.加标回收实验的回收率为89.2％～103.8％,相对标准偏差(RSD)为2.2％～6.2％.本方法操作简单,检测效率高,与现行国标测定方法相比,衍生化时间缩短44倍,试剂消耗少,前处理时间缩短4～5倍;可用于水果中2,4-滴残留的快速测定.
Abstract
Residues of 2,4-Dichlorophenoxyacetic acid (2,4-D) from agricultural use during the growth and transportation of fruits significantly affect their quality. To improve the detection efficiency of 2,4-D in fruits and while conserving energy and resources,a rapid detection method was developed using vortex-assisted derivatization combined with gas chromatography-electron capture detector (GC-ECD). Fruit samples were extracted with acetonitrile and dried under nitrogen. Subsequently,140 μL of methanol and 40 μL of concentrated sulfuric acid were added,and the mixture was vortexed for 1 minute to achieve rapid derivatization. Derivatives were extracted using n-hexane and purified with a saturated sodium chloride solution. Separation was performed on a DB-17 capillary column,and detection was achieved using GC-ECD. Quantification was conducted using both matrix-matched calibration curves and external standard method. The results demonstrated that 2,4-D exhibited good linearity in the range of 1.0～1000 μg/L with a correlation coefficient of 0.99993. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.001 and 0.003 mg/kg,respectively. Recover rates from spiking experiments ranged from 89.2％ to 103.8％,with relative standard deviations (RSDs) between 2.2％ and 6.2％. This method was simple to operate,had high detection efficiency,and compared to the current national standard method,reduced derivatization time by 44-fold,minimized reagent consumption,and shortened pretreatment time by 4～5 times. It is suitable for the rapid determination of 2,4-D residues in fruits.
关键词
水果/2,4-滴/衍生化/气相色谱-电子捕获检测器Key words
fruit/2,4-dichlorophenoxyacetic acid (2,4-D)/derivatization/gas chromatography-electron capture detector引用本文复制引用
出版年
2025
国家科技期刊平台
NSTL
万方数据