节点文献
液相色谱-串联质谱法测定牛肉中咪唑烟酸
Determination of imidazolnicotinic acid in beef by liquid chromatography-tandem mass spectrometry
【摘要】 基于液液萃取技术,本文采用乙腈饱和的正己烷对提取液进行除酯、净化,进而建立了牛肉组织中咪唑烟酸残留的高效液相色谱-三重四级杆串联质谱(LC-MS/MS)仪测定方法。通过对建立的分析方法进行性能考察,结果表明,咪唑烟酸在其线性范围内相关系数均大于0.999;以S/N≥3确定方法的检出限(LOD)为0.01μg·kg-1;以S/N≥10确定方法的定量限(LOQ)为0.1μg·kg-1。在3个加标水平(定量限0.1、0.5、1μg·kg-1)下,咪唑烟酸的回收率在75%~116.6%,相对标准偏差为3.5%~10.3%。总的来说,该方法具有简单快捷,灵敏度高,准确度好,通用性强的特点,能满足相关临时限量要求并有效用于牛肉中咪唑烟酸的检测。
【Abstract】 Based on liquid-liquid extraction technology, acetonitrile-saturated n-hexane was used to deester and purify the extract, and then a high performance liquid chromatography coupled with triple four-stage tandem mass spectrometry(LC-MS/MS)instrument was established to determine imidazolnicotinic acid residue in beef tissue.The performance of the established analytical method was investigated.The results showed that the correlation coefficients of imidazolium nicotinic acid were all greater than 0.999 in the linear range.The limit of detection(LOD)of S/N≥3 was 0.01μg·kg-1.The limit of quantification(LOQ)of the method with S/N≥10 was 0.1μg·kg-1.At three spiked levels(limits of quantification 0.1,0.5,1μg·kg-1),the recoveries of imidazolnicotinic acid ranged from 75%to 116.6%,and the relative standard deviations ranged from 3.5%to 10.3%.In general, this method has the characteristics of simple, rapid, high sensitivity, good accuracy and strong universality, which can meet the relevant temporary limit requirements and can be effectively used for the detection of imidazolnicotinic acid in beef.
【Key words】 imazapyr; pesticide residues; beef; liquid chromatography-tandem mass spectrometry;
- 【文献出处】 化学研究与应用 ,Chemical Research and Application , 编辑部邮箱 ,2023年04期
- 【分类号】O657.63;TS251.52
- 【下载频次】17