超高效液相色谱-电喷雾串联质谱法同时分析鸡肉中7种氟喹诺酮类药物残留

Simultaneous analysis of 7 fluoroquinolone residues in chicken muscle by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

建立了一种同时测定鸡肉中7种氟喹诺酮类药物残留的超高效液相色谱-电喷雾串联质谱确证分析方法(UPLC-ESI-MS/MS)。样品经酸化乙腈提取、正己烷脱脂和HLB固相萃取柱净化,采用ACQUITYUPLCTMBEHC18色谱柱(50mm×2.1mm,1.7μm)分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱,电喷雾质谱检测,正离子多反应监测模式进行定性和定量分析。7种药物在5～100μg/kg范围内线性关系良好,相关系数(r2)均大于0.99;以5,25,50μg/kg3个浓度水平进行添加回收试验,7种药物的平均回收率在79.2%～108.6%之间,相对标准偏差为4.2%～8.9%,方法的检出限(LOD)为0.2～1.4μg/kg。方法重现性好、灵敏度高、分析时间短、确证能力强,适用于鸡肉中氟喹诺酮类药物多残留的确证检测。

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^TM BEH C18 column （50 mm ×2. 1 mm, 1.7 μm） 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 ESIMS/MS in positive ion mode and multiple reaction monitoring （MRM）. The linear ranges were from 5 to 100 μg/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 μg/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 μg/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.