摘要
目的建立QuEChERS-超高效液相色谱串联质谱测定动物肌肉组织中喹乙醇及卡巴氧代谢物的方法。方法样品经盐酸酸解,乙酸乙酯提取,无水硫酸镁和氯化钠盐析,正己烷除脂净化。经Waters ACQUITY UPLC BEH C18(100 mm×2.1 mm, 1.8?m)色谱柱分离,以0.1%甲酸(A)和0.1%甲酸-甲醇(B)作为流动相,梯度洗脱。质谱(ESI+)多反应监测(multiple reaction monitoring, MRM),内标法定量。结果该方法在1~400 ng/mL浓度范围内线性良好,相关系数(r2)大于0.99。2种代谢物在0.5、1.0、5.0μg/kg的添加水平下,回收率为88.9%~109.2%,相对标准偏差值在2.18%~8.57%(n=6)。方法检出限为0.5μg/kg。结论该方法快速、准确、灵敏,可用于动物肌肉组织中的喹乙醇及卡巴氧代谢物的快速检测。
Objective To establish a method for the detection of olaquindox and carbaxyloxide metabolites in animal muscle tissue by QuEChERS-ultra high-performance liquid chromatography-tandem mass spectrometry. Methods The samples were hydrolyzed by hydrochloric acid, extracted by ethyl acetate, salted out by anhydrous magnesium sulfate and sodium chloride, and fat removed by n-hexane. Separation was carried out on a Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.8 ?m), with 0.1% formic acid(A) and 0.1% formic acid-methanol(B) as mobile phases for gradient elution. Mass spectrometry(ESI +) multiple reaction monitoring(MRM) and internal standard method were used for quantitative analysis. Results The method had good linearity in the concentration range of 1-400 ng/mL, and the correlation coefficient(r2) was greater than 0.99. The recoveries of the 2 metabolites were 88.9%-109.2% and the relative standard deviations were 2.18%-8.57%(n=6) at the addition levels of 0.5, 1.0 and 5.0 μg/kg. The detection limit was 0.5 μg/kg. Conclusion This method is rapid, accurate and sensitive, and can be used for the rapid detection of olaquindox and carbadox metabolites in animal muscle tissue.
作者
何悦
严华
崔凤云
韩深
刘韦华
顾熟琴
张朝晖
HE Yue;YAN Hua;CUI Feng-Yun;HAN Shen;LIU Wei-Hua;GU Shu-Qin;ZHANG Zhao-Hui(School of Food Science and Engineering,Beijing University of Agriculture,Beijing 102206,China;Beijing Customs Technology Center,Beijing 100026,China)
出处
《食品安全质量检测学报》
CAS
2020年第15期4989-4994,共6页
Journal of Food Safety and Quality
基金
国家重点研发计划(2019YFC1605100)。
关键词
动物肌肉组织
喹乙醇代谢物
卡巴氧代谢物
快速前处理
QUECHERS
超高效液相色谱串联质谱法
animal muscle tissue
metabolite of olaquindox
metabolite of carbadox
rapid pretreatment
QuEChERS
ultra high-performance liquid chromatography-tandem mass spectrometry
作者简介
何悦,工程师,主要研究方向为食品安全检测。E-mail:hyaiwzyfe@163.com;通讯作者:顾熟琴,硕士,副教授,主要研究方向为农产品加工及安全控制。E-mail:sq.gu@126.com;通讯作者:张朝晖,博士,研究员,主要研究方向为食品安全检测。E-mail:zhangzhaohuibiqtc@163.com。
