摘要
目的建立Qu Ch ERS超高效液相色谱-串联质谱法测定水产品中的孔雀石绿、隐色孔雀石绿、结晶紫、隐色结晶紫的检测方法。方法样品加入内标,加入中性氧化铝和C18粉末作为净化剂,加入乙腈,高速均质,振荡提取,提取液经氮气吹干,初始流动相定容后,采用ZORBAX XDB C18色谱柱(100 mm×2.1 mm,1.8μm)分离,以电喷雾正离子模式质谱检测。结果 4种化合物一定浓度范围内线性关系良好,相关系数≥0.999 0。混合空白样品在0.50μg/kg、2.00μg/kg和10.0μg/kg 3种加标水平下回收率为79.5%~92.0%,相对标准偏差为2.3%~8.7%。结论本法准确、灵敏、经济实用,可满足水产品中孔雀石绿和结晶紫及其代谢物残留的同时检测要求。
Objective To establish a method for the determination of malachite green( MG),leucomalachite green( LMG),crystal violet( CV) and leucocrystal violet( LCV) in aquatic products by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry( UPLC-MS/MS). Methods The samples added with internal standard were extracted with acetonitrile and purified by C18 and neutral alumina,and then dried-up under nitrogen gas,the residue was dissolved with initial mobile phase. The target analytes were separated on an Agilent ZORBAX XDB C18,and detected under positive ion multiple reaction monitoring( MRM) mode. Results The method showed a good linearity when the four target analytes were in a certain concentration,with the correlation coefficients( r) ≥0. 999 0. The average recoveries of 4 analytes in aquatic products at three spiked concentrations of 0. 50 μg/kg,2. 00 μg/kg,10. 0 μg/kg was within 79. 5%-92. 0%,with the relative standard deviations of 2. 3%-8. 7%. Conclusion The method is accurate,efficient,sensitive and practical.Therefore,it is suitable for the determination of MG,CV and their metabolites residues in aquatic product.
作者
高何刚
杜赛
王若燕
陈理
GAO He-gang;DU Sai;WANG Ruo-yan;CHEN Li(Shaoxing Municipal Center for Disease Control and Prevention,Shaoxing,Zhejiang 312071,China)
出处
《中国卫生检验杂志》
CAS
2021年第3期276-279,共4页
Chinese Journal of Health Laboratory Technology
基金
绍兴市公益性技术应用研究计划(2015B70071)。
关键词
孔雀石绿
结晶紫
QUECHERS
超高效液相色谱-串联质谱法
Mlachite green
Crystal ciolet
QuEChERS
Ultra-high performance liquid chromatography triple quadrupole tandem mass spectrometry
