亲水相互作用液相色谱-串联质谱法快速测定乳粉中异噻唑啉酮类药物残留量

doi:10.12441/spyswjs.20250126001

首页 > 过刊浏览>2025年第卷第3期 >142-152. DOI:10.12441/spyswjs.20250126001

亲水相互作用液相色谱-串联质谱法快速测定乳粉中异噻唑啉酮类药物残留量
DOI:
                        10.12441/spyswjs.20250126001
                    
CSTR:
                        
                    
作者:
                        
                        
                    
作者单位:上海动物疫病预防控制中心，上海 200124
作者简介:
通讯作者:黄士新（1969—），男，硕士，农业技术推广研究员，主要从事畜牧投入品质量安全监管。E-mail：yans08@163.com
中图分类号:
基金项目:上海市科技兴农项目（2022-02-08-00-12-F01100）。

Rapid Determination of Isothiazolinone Residues in Milk Powder by Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry

Author:

Affiliation:

Shanghai Animal Disease Control Center, Shanghai 200124, China

Fund Project:

摘要

图/表

访问统计

参考文献

相似文献

引证文献

资源附件

文章评论

摘要:

【目的】建立乳粉中3种异噻唑啉酮类药物残留量的液相色谱-串联质谱快速检测方法。【方法】试样经乙腈提取2次，合并提取液后经Waters Prime HLB小柱富集净化，洗脱液采用Waters BEH HILIC （2.1 mm×100 mm×1.7 μm）亲水相互作用色谱柱分离后，以串联四极杆质谱检测器分析，同位素内标法定量。【结果】 3种异噻唑啉酮药物在2.5~250.0 μg/kg范围内线性良好（r≥0.995），检测限（LOD）均为4 μg/kg，定量限（LOQ）均为10 μg/kg。在试样中进行三水平添加回收试验，3种药物的添加回收率为80.5%~94.3%，批内变异系数为3.52%~10.95%，批间变异系数为6.64%~9.67%。【结论】该方法操作简便，仪器分析时间短，方法灵敏度高，且具有较高的准确度与精密度，适用于乳粉中3种异噻唑啉酮类药物的检测。

Abstract:

[Objective] A liquid chromatography-tandem mass spectrometry method was developed for rapid determination of 3 isothiazolinone residues in milk powder. [Method]Each sample was extracted twice with acetonitrile, and the extract was purified and enriched by Waters Prime HLB. The eluate was separated on a Waters BEH HILIC column (2.1 mm×100 mm×1.7 μm) and determined by quadrupole-MS/MS, and an isotopic internal standard method was employed for quantitation. [Result] The 3 isothiazolinones showed with good linearity (r≥0.995) within the range from 2.5 μg/kg to 250.0 μg/kg. The limits of detection (LOD) and the limits of qualification (LOQ) for the 3 isothiazolinones were 4 μg/kg and 10 μg/kg, respectively. The spiked recovery tests at three levels were conducted for the samples, and the spiked recoveries of the 3 isothiazolinones varied between 80.5% and 94.3%. The intra-batch and inter-batch coefficients of variation were 3.52%~10.95% and 6.64%~9.67%, respectively. [Conclusion]This method, with simple operation, short analysis time, high sensitivity, high accuracy, and high precision, is suitable for the determination of 3 isothiazolinone residues in milk powder.

参考文献

相似文献

引证文献

引用本文

吴剑平,张亦菲,张婧,吴雨珊,严凤,黄士新.亲水相互作用液相色谱-串联质谱法快速测定乳粉中异噻唑啉酮类药物残留量[J].食品与生物技术学报,2025,(3):142-152.

WU Jianping, ZHANG Yifei, ZHANG Jin, WU Yushan, YAN Feng, HUANG Shixin. Rapid Determination of Isothiazolinone Residues in Milk Powder by Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Food Science and Biotechnology,2025,(3):142-152.

复制

文章指标

点击次数:
下载次数:
HTML阅读次数:
引用次数:

历史

收稿日期:2025-01-26
最后修改日期:2025-03-14
录用日期:
在线发布日期: 2025-07-15
出版日期:

文章二维码

地址：江苏省无锡市蠡湖大道1800号邮政编码：214122

电话：0510-85913526 电子邮件：xbbjb@jiangnan.edu.cn

技术支持：北京勤云科技发展有限公司

引用本文

分享

相关视频

文章指标

历史

文章二维码

微信公众号二维码

手机版网站二维码