养殖虾类中呋喃西林代谢物检测方法的优化

Optimization of the detection method of furacillin metabolite residue in farmed shrimp

建立了微波辅助衍生结合超高效液相色谱-串联质谱快速测定养殖虾类中呋喃西林代谢物氨基脲的方法。样品经过盐酸水解,2-硝基苯甲醛微波辅助衍生,乙酸乙酯萃取,除杂净化后,采用超高效液相色谱-串联质谱法检测氨基脲含量,内标法定量。氨基脲质量浓度为0.5~100μg/L时,线性关系良好,相关系数为0.9996~0.9999,检出限为0.20μg/kg,测定结果的相对标准偏差为3.06%~6.56%,加标回收率为91.4%~103.6%。运用该方法测定了3种养殖虾类(斑节对虾、南美白对虾、罗氏沼虾)中的呋喃西林代谢物含量。该方法上机检测时间短,检出限低,具有良好的准确度和精密度,可用于虾类中氨基脲的检测。

The aim of this study was to establish a method based on microwave-assisted derivatization with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the determination of semicarbazide(SEM)in farmed shrimp.The sample was hydrolyzed with hydrochloric acid and microwave-assisted derivatization of 2-nitrobenzaldehyde.And then it was extracted with ethyl acetate.After the purification treatment,the content of carbamide urea was determined by UPLC-MS/MS and quanti-fied by the internal standard method.To investigate the accuracy and stability of the optimized method in different samples,standard addi-tive experiments were carried out for different matrix samples.The results showed that,when the mass concentration of SEM ranged from 0.5 to 100μg/L,the correlation coefficient was between 0.9996 and 0.9999.And the detection limit was 0.2μg/kg.In addition,the relative standard deviation was 3.06%-6.56%and the standard recovery was 91.4%-103.6%respectively.Moreover,this method was further used to determine the contents of furacillin metabolites in three kinds of farmed shrimp(Penaeus monodon,Litopenaeus Van-namei and Macrobrachium rosenbergii).This method has the advantages of low detection limit,short detection time,good precision and accuracy,and can be used for the detection of SEM in farmed shrimp.