离子交换色谱-紫外检测器法测定马铃薯中马来酰肼的残留量
Determination of Residue of Maleic Hydrazide in Potato by Ion Exchange Chromatography Combined with Ultraviolet Detector
王晓威 1孟玲玲 1蔡丹旎 1于世强 1刘鹏宇 1栾绍嵘1
作者信息
- 1. 华东理工大学 化学与分子工程学院,上海 200237
- 折叠
摘要
提出了离子交换色谱-紫外检测器法测定马铃薯中马来酰肼残留量的方法.称取1 g洗净、去皮、搅碎的马铃薯样品,加入10 mL甲醇,超声提取30 min,于60℃水浴加热5 min,离心20 min,取上清液过0.22 μm滤膜和反相前处理柱.采用Dionex IonPac AS16分析柱和Dionex IonPac AG16保护柱分离,KOH溶液梯度洗脱,在205 nm波长下进行检测.结果表明:马来酰肼的质量浓度在0.182 5～10.14 mg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)为0.06 mg·L-1;按照标准加入法进行回收试验,马来酰肼回收率为97.9%～108%;柱温、流量和紫外检测波长的微小改变,对MH的检测均没有影响;方法用于实际马铃薯样品分析,均未检出马来酰肼.
Abstract
A method for the determination of residue of maleic hydrazide in potato by ion exchange chromatography combined with ultraviolet detector was proposed.The washed,peeled and mashed potato sample(1 g)was taken,and 10 mL of methanol was added.The mixture was extracted by ultrasonic for 30 min,heated in water bath at 60℃for 5 min,and centrifuged for 20 min.The supernatant was passed through 0.22 μm filter membrane and reverse-phase pretreatment column.Separation was performed on Dionex IonPac AS16 analytical column and Dionex IonPac AG16 guard column,with KOH solution for gradient elution,and detection at wavelength of 205 nm.It was shown that linear relationship between the mass concentration and its peak area of maleic hydrazide was kept in the range of 0.182 5-10.14 mg·L-1,with detection limit(3S/N)of 0.06 mg·L-1.Test for recovery was made by the standard addition method,giving results in the range of 97.9%-108%.Slight changes in column temperature,flow rate and UV detection wavelength had no effect on the detection of maleic hydrazide.The method was used to analyze the actual potato samples,in which maleic hydrazide was not detected.
关键词
马铃薯/马来酰肼/离子交换色谱/紫外检测器Key words
potato/maleic hydrazide/ion exchange chromatography/ultraviolet detector引用本文复制引用
出版年
2024
NETL
NSTL
万方数据