Guo Wei, Liu Yong, Liu Ning
College of Food Science, Northeast Agricultural University, Harbin, China.
Se Pu. 2009 Jul;27(4):406-11.
A confirmative method of ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) for the simultaneous determination of 7 fluoroquinolone residues (norfloxacin (NOR), ciprofloxacin (CIP), danofloxacin (DAN), enrofloxacin (ENR), ofloxacin (OFL), sarafloxacin (SAR) and marbofloxacin (MAR)) in chicken muscle was developed. The sample was extracted with acidified acetonitrile, defatted with n-hexane, and purified by an HLB solid phase extraction cartridge. The UPLC separation was performed on an ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) utilizing a gradient elution program of acetonitrile and water (containing 0.1% formic acid) as the mobile phase. The identification and quantification were achieved by using ESI-MS/MS in positive ion mode and multiple reaction monitoring (MRM). The linear ranges were from 5 to 100 microg/kg with the correlation coefficients above 0.99 for all the 7 fluoroquinolones. The average recoveries spiked at the 3 concentration levels of 5, 25, 50 microg/kg ranged from 79. 2% to 108.6% with the relative standard deviations of 4.2% - 8.9%. The limits of detection were 0.2 - 1.4 microg/kg. The method was proved to be good reproducibility, high sensitivity, rapid, reliable and suitable for the simultaneous determination of multi-residues of fluoroquinolones in chicken muscle.
建立了一种超高效液相色谱-电喷雾电离串联质谱(UPLC-ESI-MS/MS)同时测定鸡肉中7种氟喹诺酮类药物残留(诺氟沙星(NOR)、环丙沙星(CIP)、达氟沙星(DAN)、恩诺沙星(ENR)、氧氟沙星(OFL)、沙拉沙星(SAR)和马波沙星(MAR))的确证方法。样品用酸化乙腈提取,正己烷脱脂,并用HLB固相萃取柱净化。UPLC分离在ACQUITY UPLC BEH C18柱(50 mm×2.1 mm,1.7μm)上进行,以乙腈和水(含0.1%甲酸)为流动相,采用梯度洗脱程序。通过在正离子模式下使用ESI-MS/MS和多反应监测(MRM)进行定性和定量。7种氟喹诺酮类药物的线性范围均为5至100μg/kg,相关系数均大于0.99。在5、25、50μg/kg 3个浓度水平下的平均回收率为79.2%至108.6%,相对标准偏差为4.2% - 8.9%。检测限为0.2 - 1.4μg/kg。该方法具有良好的重现性、高灵敏度、快速、可靠,适用于鸡肉中氟喹诺酮类药物多残留的同时测定。