基质固相分散-液相色谱-串联质谱联用技术检测鸡蛋中14种氟喹诺酮类药物残留
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摘要
本工作建立了一种基质固相分散-液相色谱-串联质谱(LC-MS/MS)联用技术测定鸡蛋中14种氟喹诺酮类药物残留的新方法。基质固相分散提取过程中以硅胶为分散剂,氨甲醇溶剂为洗脱剂,其萃取回收率在80%以上。洗脱液浓缩定容后经Shimpack GISS C_(18)柱(50×2.1mm,1.9μm)分离,质谱采用电喷雾电离、正离子模式(ESI+),以多反应监测(MRM)模式进行检测。方法的线性范围为0.1~50μg/kg,检出限达到0.1μg/kg,相对标准偏差为8.8%~10.4%。方法检出限优于国家标准方法,可满足实际样品分析的要求。
A new method of matrix solid-phase dispersion coupled with liquid chromatography-tandem mass spectrometry was developed for the determination of fourteen kinds of fluoroquinolones residues in eggs.With silica gel as a dispersant and ammonia methanol as eluent,the recoveries of fluoroquinolones in matrix solid-phase dispersion extraction were higher than 80%.The elution solution was then concentrated and introduced into a C_(18) column for chromatographic separation.The identification and quantification of target analytes were performed using electrospray ionization in positive mode and multiple reaction monitoring(MRM).Under the optimized condition,the linear ranges were 0.1-50μg/kg with the RSDs of 8.8%-10.4%,and the limits of detection were 0.1μg/kg,which were lower than the values required by National Standards of China.
A new method of matrix solid-phase dispersion coupled with liquid chromatography-tandem mass spectrometry was developed for the determination of fourteen kinds of fluoroquinolones residues in eggs.With silica gel as a dispersant and ammonia methanol as eluent,the recoveries of fluoroquinolones in matrix solid-phase dispersion extraction were higher than 80%.The elution solution was then concentrated and introduced into a C_(18) column for chromatographic separation.The identification and quantification of target analytes were performed using electrospray ionization in positive mode and multiple reaction monitoring(MRM).Under the optimized condition,the linear ranges were 0.1-50μg/kg with the RSDs of 8.8%-10.4%,and the limits of detection were 0.1μg/kg,which were lower than the values required by National Standards of China.
引文
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[5] ZHU B,JIANG S J,HU C Q.Chinese Journal of Pharmaceutical Analysis(朱斌,蒋受军,胡昌勤.药物分析杂志),2002,5:397.
[6] YIN C,WU Y T.Chinese Journal of Pharmaceutical Analysis(尹茶,吴玉田.药物分析杂志),1997,6:371.
[7] VoL N.Journal of Aoac International,1994,77(4):871.
[8] LIAO L,RAO Y,YANG G X,et al.Scientia Agricultura Sinica(廖兰,饶勇,杨桂香,等.中国农业科学),2008,41(8):2419.
[9] ZHAO Y,ZHENG Z M,JIN S S,et.al.Journal of Agro-Environment Science(赵扬,郑志明,金社胜,等.农业环境科学学报),2011,30(6):1248.
[10]TIAN Y,ZHANG Z J,LI J,et al.Journal of China Pharmaceutical University(田媛,张尊建,李静,等.中国药科大学学报),2010,41(1):60.
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[12]Barker S A.Journal of Chromatography A,2000,880(1-2):63.
[13]Barker S A.Journal of Biochemical and Biophysical Methods,2007,70(2):151.
[14]Capriotti A L,Cavaliere C,Giansanti P,et al.Journal of Chromatography A,2010,1217(16):2521.