高效液相色谱荧光检测器法快速测定水果中乙氧基喹啉残留量研究
Rapid Determination of Ethoxyquin Residues in Fruits by High Performance Liquid Chromatography with Fluorescence Detector
周志杰 1程雪 1韩东明1
作者信息
- 1. 济南市食品药品检验检测中心,山东济南 250000
- 折叠
摘要
建立了高效液相色谱仪串联荧光检测器测定苹果、梨样品中乙氧基喹啉残留量的方法.水果样品加入抗坏血酸后进行混合匀浆制样,向样品中加入0.1 mol·L-1 氢氧化钠溶液,在碱性条件下经正己烷进行3 次提取,合并提取液氮吹至干,用含有抗坏血酸的乙腈复溶,采用液相色谱荧光检测器法上机测定,外标法定量.荧光检测器激发波长365 nm,发射波长 435 nm,流动相采用乙腈∶水=65∶35.结果表明,本方法在 2.00～200.00 ng·mL-1 浓度范围内呈现良好线性关系,线性方程为Y=1.06×104X-1.74×103,相关系数(r)为 0.999 97.在 0.02 mg·kg-1、0.20 mg·kg-1、1.00 mg·kg-1 3 个浓度水平进行加标,并进行 6 次平行实验,回收率在81.09%～86.43%,相对标准偏差为1.18%～3.09%.本方法简单快速,提取效率高,仪器灵敏度高,准确度和重复性良好,可用于水果中乙氧基喹啉残留量的测定.
Abstract
To establish a method for the determination of residual ethoxyquin in apple and pear samples by high performance liquid chromatograph tandem fluorescence detector.The fruit samples were mixed with ascorbic acid and homogenized for sample preparation.0.1 mol·L-1 sodium hydroxide solution was added to the samples.The samples were extracted by n-hexane for three times under alkaline conditions,and the liquid nitrogen was extracted and blown to dry.Dissolve with acetonitrile containing ascorbic acid,use liquid chromatography fluorescence detector method for machine measurement,and use external standard method for quantification.The excitation wavelength of fluorescence detector is 365 nm,the emission wavelength is 435 nm,and the mobile phase is acetonitrile : water = 65 : 35.The results showed that the method presented a good linear relationship in the concentration range of 2.00～200.00 ng·mL-1,the linear equation was Y=1.06×104X-1.74×103,and the correlation coefficient(r)was 0.999 97.Three concentration levels of 0.02 mg·kg-1,0.20 mg·kg-1 and 1.00 mg·kg-1 were added,and six parallel experiments were carried out.The recoveries were 81.09％～86.43％,and the relative standard deviations(RSD)were 1.18％～3.09％.The method is simple and rapid,has high extraction efficiency,high instrument sensitivity,good accuracy and repeatability,and can be used for the determination of ethoxyquin residues in fruits.
关键词
乙氧基喹啉/荧光检测器/水果Key words
ethoxyquin/fluorescence detector/fruit引用本文复制引用
出版年
2024
NETL
NSTL
万方数据