摘要
孔雀石绿和结晶紫及其代谢产物是一类我国已禁用的高毒性兽药。目前已有的检测方法操作较为繁琐、耗时较长,且结果的准确性和稳定性易受衍生装置等因素的影响。文章对超高效液相色谱-串联质谱法测定水产品中孔雀石绿和隐性孔雀石绿、结晶紫和隐性结晶紫的检测方法进行优化,同时,为降低测定中的基质效应,测定过程中加入同位素内标(氘代孔雀石绿和氘代隐性孔雀石绿),提高了检测结果的可靠性。结果表明:孔雀石绿和隐性孔雀石绿、结晶紫和隐性结晶紫在1.0-50.0 ng/mL的浓度范围之内,线性关系良好(r>0.999),检出限均为0.003 μg/kg。在5-100 μg/kg的水平之内,目标物质的平均加标回收率范围为92.25%-97.36%,相对标准偏差均小于等于4.62%。结论:该方法具有快速准确、重复性好、灵敏度高等特点,可以为提升水产品质量安全水平的检测工作提供技术支持。
Malachite green (MG),crystal violet(CV) and their metabolites are highly toxic veterinary drugs which have been banned in China.The existing detection methods are cumbersome and time-consuming,and the accuracy and stability of the results are easily affected by derivative devices and other factors.A rapid and simultaneous method was optimized for the determination of MG,CV,leuco malachite green (LMG) and leuco crystal violet (LCV) residues in aquatic products by UPLC-MS/MS.Meanwhile,isotopic internal standards (D-LMG and D-MG) were added to reduce the matrix effect and improve the reliability of results.The results show that MG,CV,LMG and LCV have a linear correlation (r>0.999) within the range of 1.0-50.0 ng/mL,and their detection limits were 0.003 μg/kg.The average recovery of MG,CV,LMG and LCV was 92.25%-97.36% and the relative standard deviations (RSD) were no more than 4.62%,within the internal standards fortification ranging from 5-100 μg/kg.In conclusion,the optimized method by UPLC-MS/MS could be applied for the detection of MG,CV,LMG and LCV residues in aquatic products with the advantages of quick,high precision,good reproducibility and high sensitivity.This method would provide technological support for the improvement of quality and safety of aquatic products.
作者
周蕾
ZHOU Lei(Chaoyang District Food and Drug Safety Monitoring Center,Beijing 100123,China)
出处
《食品科技》
CAS
北大核心
2021年第5期272-278,共7页
Food Science and Technology
基金
河北省科学技术厅重点研发计划项目-农业高质量发展关键共性技术攻关专项(20324001D)。
