分析仪器
分析儀器
분석의기
ANALYTICAL INSTRUMENTATION
2013年
6期
92-97
,共6页
液相色谱-串联质谱法%残留量%硝基呋喃代谢物%巴鱼
液相色譜-串聯質譜法%殘留量%硝基呋喃代謝物%巴魚
액상색보-천련질보법%잔류량%초기부남대사물%파어
LC-MS/MS%residues%nitrofuran metabolic%Spanish mackerel
建立巴鱼中呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因的代谢物残留量液相色谱-串联质谱的方法。分析物采用电喷雾电离正离子( ESI +)、多反应监测(M RM )模式检测,内标法定量。本实验对固相萃取法提取和乙酸乙酯提取净化前处理方法进行比对,4种硝基呋喃代谢物的混合标准溶液的浓度在0.5~50ng/mL范围线性良好,相关系数均大于0.9981,4种化合物的检测限为0.5μg/kg。添加浓度1μg/kg、2.5μg/kg、5μg/kg范围内得出4种代谢物固相萃取净化法的回收率在81.1%~104.1%之间,相对标准偏差(RSD)小于5.7%.乙酸乙酯提取净化法的回收率在88.5%~108.2%之间,相对标准偏差(RSD )小于6.1%。结论证明乙酸乙酯提取法方法前处理简单、快速、稳定性好,适用于大量样品的同时检测。
建立巴魚中呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因的代謝物殘留量液相色譜-串聯質譜的方法。分析物採用電噴霧電離正離子( ESI +)、多反應鑑測(M RM )模式檢測,內標法定量。本實驗對固相萃取法提取和乙痠乙酯提取淨化前處理方法進行比對,4種硝基呋喃代謝物的混閤標準溶液的濃度在0.5~50ng/mL範圍線性良好,相關繫數均大于0.9981,4種化閤物的檢測限為0.5μg/kg。添加濃度1μg/kg、2.5μg/kg、5μg/kg範圍內得齣4種代謝物固相萃取淨化法的迴收率在81.1%~104.1%之間,相對標準偏差(RSD)小于5.7%.乙痠乙酯提取淨化法的迴收率在88.5%~108.2%之間,相對標準偏差(RSD )小于6.1%。結論證明乙痠乙酯提取法方法前處理簡單、快速、穩定性好,適用于大量樣品的同時檢測。
건립파어중부남서동、부남타동、부남서림화부남타인적대사물잔류량액상색보-천련질보적방법。분석물채용전분무전리정리자( ESI +)、다반응감측(M RM )모식검측,내표법정량。본실험대고상췌취법제취화을산을지제취정화전처리방법진행비대,4충초기부남대사물적혼합표준용액적농도재0.5~50ng/mL범위선성량호,상관계수균대우0.9981,4충화합물적검측한위0.5μg/kg。첨가농도1μg/kg、2.5μg/kg、5μg/kg범위내득출4충대사물고상췌취정화법적회수솔재81.1%~104.1%지간,상대표준편차(RSD)소우5.7%.을산을지제취정화법적회수솔재88.5%~108.2%지간,상대표준편차(RSD )소우6.1%。결론증명을산을지제취법방법전처리간단、쾌속、은정성호,괄용우대량양품적동시검측。
A method was established to detect nitrofuran metabolic residues in Spanish mackerel by liq-uid chromatography tandem mass spetrometry (LC-MS/MS) .Theanalvtes were detected by LC-MS/MS (ESI) with multiple reaction monitoring (MRM ).The result indicated that the calibration curves were in good linearity between the peak area and the concentration of 0.5-50ng/ml for nitrofuran metabolic with correlation cofficients not less than 0.9981.The limits of detection for four nitrofuran metabolics were 0.5μg/kg. .Then analytes were extracted by spe or ethyl acetat the average recoveries were 81.1%-104.1% or 88.5%-108.2% and the related standard deviations less than 5.1 or 6.1% at the three levels 1μg/kg、2.5μg/kg、5μg/kg.The proposed method was simple ,rapid ,the stability was good and suitable for the simultaneous quantitative detection.