基于QuEChERS法-超高效液相色谱-串联质谱同位素标记内标法测定动物源性食品中11种喹诺酮类药物残留
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摘要
目的建立同时测定动物源性食品中11种喹诺酮类药物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法结合QuEChERS技术,优化样品前处理方法,采用同位素标记内标法,以甲醇-乙腈(2∶3,V/V)与0.2%甲酸水溶液为流动相梯度洗脱,质谱分析采用电喷雾电离,正离子多反应监测(MRM)模式。结果 11种喹诺酮类药物在2.5～100.0μg/L范围内具有良好的线性关系,检测限范围为0.21～1.16μg/kg,平均回收率在82.7%～118.6%之间,相对标准差<15%。结论本法操作简便,精密度和准确度好,适用于动物源性食品中喹诺酮类药物残留的大批量样品快速检测。
Objective To establish an UPLC-MS/MS method for the simultaneous determination of eleven quinolone drug residues in animal-sourced foods. Methods The procedure for the pretreatment of samples was optimized by the QuEChERS method,and the isotope-labeled standards were used in UPLC-MS/MS. In the UPLC-MS/MS,the ultra performance liquid chromatography was performed using a gradient methanol-acetonitrile(2∶3,V/V)and 0.2% formic acid solution as mobile phase,and the detector of the electrospray ionization-tandem mass spectrometry was set in the positive and multiple reaction monitoring(MRM)mode. Results The calibration curves of the eleven quinolones showed a good linearity in the range of 2.5-100.0 μg/L. The limits of detection ranged from 0.21 to 1.16 μg/kg,the average recoveries were in the range of 82.7% to 118.6%,and the relative standard deviations were less than 15.0%. Conclusion The method could be simply put into operation,with a good precision and accuracy,which is suitable for rapid detection of quinolone drug residues in a large number of animal-sourced food samples.
Objective To establish an UPLC-MS/MS method for the simultaneous determination of eleven quinolone drug residues in animal-sourced foods. Methods The procedure for the pretreatment of samples was optimized by the QuEChERS method,and the isotope-labeled standards were used in UPLC-MS/MS. In the UPLC-MS/MS,the ultra performance liquid chromatography was performed using a gradient methanol-acetonitrile(2∶3,V/V)and 0.2% formic acid solution as mobile phase,and the detector of the electrospray ionization-tandem mass spectrometry was set in the positive and multiple reaction monitoring(MRM)mode. Results The calibration curves of the eleven quinolones showed a good linearity in the range of 2.5-100.0 μg/L. The limits of detection ranged from 0.21 to 1.16 μg/kg,the average recoveries were in the range of 82.7% to 118.6%,and the relative standard deviations were less than 15.0%. Conclusion The method could be simply put into operation,with a good precision and accuracy,which is suitable for rapid detection of quinolone drug residues in a large number of animal-sourced food samples.
引文
[1]高何刚,王瑞,杜赛,等.液相色谱-质谱/质谱联用在磺胺和喹诺酮类兽药残留检测中的应用概述[J].中国卫生检验杂志,2017,27(12):1821-1823.
[2]张元,周伟娥,李绍辉,等.动物源性食品中喹诺酮类残留前处理及分析方法的研究进展[J].食品工业科技,2017,37(5):378-383.
[3]仇玉洁,李晓月,李博恩,等.水产品中氟喹诺酮类药物残留检测技术研究进展[J].湖南农业科学,2018(1):115-118.
[4]廖洁丹,李智丽,张济培.高效液相色谱荧光检测法测定牛奶中4种氟喹诺酮类药物残留[J].中国兽医杂志,2018,54(3):104-111.
[5]赵飞,高广慧,贾宏新.超高效液相色谱-串联四极杆质谱法测定麻辣烫中喹诺酮类药物残留[J].分析测试学报,2017,36(6):768-772.
[6]张中印,赵柳微,曹葳蕤,等.QuEChERS前处理方法结合高效液相色谱-串联质谱测定蜂蜜和蜂王浆中14种喹诺酮类药物残留[J].食品科学,2016,37(16):242-248.
[7]樊晓博,谢兰心.酶标抗原直接竞争ELISA检测食品中氟喹诺酮类药物多残留[J].食品科学,2015,36(24):265-269.
[8]张代辉.液相色谱-串联质谱技术对食品中主要兽药残留的研究[D].吉林:吉林大学,2011.
[9]曹鹏,牟妍,高飞.分散固相萃取-超高效液相色谱-串联质谱法同时检测火锅食材中11种喹诺酮类药物[J].色谱,2013,31(9):862-868.
[10]李婧妍,郭春锋,崔立辉,等. QuEChERS HPLC-MS/MS法测定禽肉中9种喹诺酮类兽药残留量[J].食品研究与开发,2016,37(22):153-157.
[11] Matuszewski BK,Constanzer ML,Chavez-eng CM. Strategies for the assessment of matrix effect in quantitative bio-analytical methods based on HPLC-MS/MS[J]. Anal Chem,2003,75(13):3019-3030.
[12]中华人民共和国国家质量监督检验检疫总局.GB/T21312-2007动物源性食品中14种喹诺酮药物残留检测方法液相色谱-质谱/质谱法[S].北京:中国标准出版社,2007.
[2]张元,周伟娥,李绍辉,等.动物源性食品中喹诺酮类残留前处理及分析方法的研究进展[J].食品工业科技,2017,37(5):378-383.
[3]仇玉洁,李晓月,李博恩,等.水产品中氟喹诺酮类药物残留检测技术研究进展[J].湖南农业科学,2018(1):115-118.
[4]廖洁丹,李智丽,张济培.高效液相色谱荧光检测法测定牛奶中4种氟喹诺酮类药物残留[J].中国兽医杂志,2018,54(3):104-111.
[5]赵飞,高广慧,贾宏新.超高效液相色谱-串联四极杆质谱法测定麻辣烫中喹诺酮类药物残留[J].分析测试学报,2017,36(6):768-772.
[6]张中印,赵柳微,曹葳蕤,等.QuEChERS前处理方法结合高效液相色谱-串联质谱测定蜂蜜和蜂王浆中14种喹诺酮类药物残留[J].食品科学,2016,37(16):242-248.
[7]樊晓博,谢兰心.酶标抗原直接竞争ELISA检测食品中氟喹诺酮类药物多残留[J].食品科学,2015,36(24):265-269.
[8]张代辉.液相色谱-串联质谱技术对食品中主要兽药残留的研究[D].吉林:吉林大学,2011.
[9]曹鹏,牟妍,高飞.分散固相萃取-超高效液相色谱-串联质谱法同时检测火锅食材中11种喹诺酮类药物[J].色谱,2013,31(9):862-868.
[10]李婧妍,郭春锋,崔立辉,等. QuEChERS HPLC-MS/MS法测定禽肉中9种喹诺酮类兽药残留量[J].食品研究与开发,2016,37(22):153-157.
[11] Matuszewski BK,Constanzer ML,Chavez-eng CM. Strategies for the assessment of matrix effect in quantitative bio-analytical methods based on HPLC-MS/MS[J]. Anal Chem,2003,75(13):3019-3030.
[12]中华人民共和国国家质量监督检验检疫总局.GB/T21312-2007动物源性食品中14种喹诺酮药物残留检测方法液相色谱-质谱/质谱法[S].北京:中国标准出版社,2007.