摘要
建立了鸡组织中沃尼妙林残留的液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)检测方法。样品用乙腈提取后,过Strata-X-C固相萃取小柱净化。以乙腈-0.1%甲酸水溶液(35:65,V/V)为流动相,经LunaC18色谱柱分离,采用电喷雾电离,多反应监测(MRM)正离子模式对沃尼妙林进行定性与定量分析。采用基质匹配法,对鸡皮肤、肌肉、肾脏和肝脏中沃尼妙林的含量进行标准校正,在5(7.5)～500μg/kg范围内线性良好(r>0.998),在鸡肝脏中的检出限(LOD)及定量限(LOQ)分别为4.0和7.5μg/kg;其它3种组织中的LOD及LOQ分别为2.5和5.0μg/kg。在5(7.5),50及500μg/kg添加水平下,4中组织中沃尼妙林的平均回收率为78.5%～104.0%。日内相对标准偏差(RSD)为1.2%～9.8%,日间相对标准偏差为3.7%～13.2%。
A liquid chromatography with electrospray ionization tandem mass spectrometry detection （LC ESI MS/MS） method for the determination of valnemulin residues in chicken tissues was developed.The analyte was extracted with acetonitrile and the extract was cleaned up by the Strata-X-C solid phase extraction column.Chromatographic separation of valnemulin was performed in isocratic mode,on a C18 column using acetonitrile and 0.1% formic acid aqueous solution （35：65,V/V）.Qualitation and quantification of valnemulin were achieved with multiple reaction monitoring （MRM） in positive electrospray ionization.Matrix-matched calibration standard was used for quantification.The calibration curve was good linear from 5（7.5） to 500 μg/kg with the correlation coefficient of 0.998.The limits of detection （LOD） were 4 μg/kg in liver tissue and 2.5 μg/kg in others,and the limits of quantification （LOQ） were 7.5 and 5.0 μg/kg,respectively.The mean recoveries varied from 78.5% to 104.0% at the three spiked levels of 5（7.5）,50,and 500 μg/kg.The intra-day relative standard deviation （RSD） and inter-day RSD were in the range of 1.2%-9.8%,and 3.7%-13.2%,respectively.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第7期1031-1035,共5页
Chinese Journal of Analytical Chemistry
基金
"十一五"国家科技支撑计划课题(No.2006BAD31B01)资助
关键词
沃尼妙林
鸡组织
残留
液相色谱-串联质谱
Valnemulin
Chicken tissues
Residue
Liquid chromatography-tandem mass spectrometry
