摘要
在承担糖皮质激素风险监测任务时,发现2个现行有效的关于检测动物组织中糖皮质激素的国家标准(农业部1031号公告-2—2008《动物源性食品中糖皮质激素类药物多残留检测液相色谱-串联质谱法》和GB/T 21981—2008《动物源食品中激素多残留检测方法液相色谱-质谱/质谱法》)中的样品前处理均采用了固相萃取方法,从而导致了检测过程中过柱净化烦琐、氮吹浓缩时间长、检测成本高、生态环境不友好等诸多弊端。在经过大量实验研究及经实际工作应用检验的基础上,研究简化了动物组织中地塞米松和倍他米松残留检测中样品前处理固相萃取过柱和氮吹过程,建立了快速、准确、灵敏的动物组织(牛肝、牛肉、猪肝与猪肉)中残留的地塞米松和倍他米松的超高效液相色谱-串联质谱的同时检测方法。样品在盐析条件下经乙腈提取,正己烷脱脂,采用电喷雾多反应监测、负离子模式测定,对动物组织中地塞米松和倍他米松进行定性和定量。地塞米松和倍他米松的检出限可达0.5μg/kg,定量限可达1.0μg/kg。在地塞米松和倍他米松的质量浓度为0.1~50.0μg/L,峰强度与质量浓度的线性关系良好(R 2>0.99)。在地塞米松和倍他米松的1.0、2.0、5.0μg/kg添加浓度下,方法的平均回收率在83.3%~98.2%。希望该研究可为实验室大批量检测此类药物在动物组织中的残留提供一定的借鉴。
When undertaking glucocorticoid risk monitoring missions,the solid phase extraction method was used in the sample pretreatment of two currently valid national standards(Announcement 1031-2—2008 of the Ministry of Agriculture Determination of glucocorticoids residues in animal products by L C-MS/MS method and GB/T 21981—2008 Determination of hormone multiresidues in foodstuffs of animal origin:L C-MS/MS method),led to drawbacks in the testing process,such as intricacies for column purification and time consuming of nitrogen blowing concentration,high testing cost and unfriendly ecological environment and so on.Therefore,on the basis of a large number of experimental studies and practical application tests,the sample pretreatment solid phase extraction through column and nitrogen blowing in the detection of dexamethasone and betamethasone residues in animal tissues was simplified.The method for simultaneous determination of dexamethasone and betamethasone residues in animal tissues(beef liver,beef,pork liver and pork)was developed by ultra-performance liquid chromatography tandem mass spectrometry.Samples were extracted with acetonitrile in the condition of salt fractionation and degreased by hexane.Identification and quantification of dexamethasone and betamethasone were carried out by electrospray ionization in negative mode using multiple-reaction monitoring,and the limits of detection was 0.5μg/kg,limits of quantitation was 1.0μg/kg.There was a good linear relationship between the peak intensity and the mass concentrations within the range of 0.1-50.0μg/L,and the correlation coefficients were good(R 2>0.99).The average recoveries of this method for spiked samples in the levels of 1.0μg/kg,2.0μg/kg and 5.0μg/kg were in the range of 83.3%-98.2%.The research could provide reference for the large-scale detection of residues of this type of drugs in animal tissues in laboratory.
作者
刘勇军
刘洪斌
雷春娟
侯东军
田亚平
LIU Yongjun;LIU Hongbin;LEI Chunjuan;HOU Dongjun;TIAN Yaping(China Animal Disease Control Center,Beijing 102600,China)
出处
《食品科学技术学报》
EI
CAS
CSCD
北大核心
2024年第2期177-184,共8页
Journal of Food Science and Technology
