液相色谱-串联质谱法检测雄蜂蛹粉中50种抗生素残留
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摘要
建立了液相色谱-串联质谱检测雄蜂蛹粉中50种抗生素残留(大环内酯类、喹诺酮类、磺胺类、四环素类、硝基咪唑类、林可霉素和氯霉素)的方法。样品经高氯酸溶液和醋酸铅溶液提取沉淀蛋白质,清液用磷酸氢二钾溶液调节pH值至8,经固相萃取净化后进行仪器分析。采用多反应监测正离子或负离子模式检测,可以一次完成对雄蜂蛹粉中50种目标化合物的定性和定量测定。50种抗生素的加标回收率为70. 2%～118. 3%,相对标准偏差(RSD)为1. 8%～13. 6%。该方法操作简便,灵敏度高,适用于雄蜂蛹粉中多种兽药残留的分析确证。
A method was established for the determination of 50 kinds of antibiotic residues( macrolides,quinolones,sulfonamides,tetracyclines,nitroimidazoles,lincomycin and chloramphenicol)in drone pupa powder by liquid chromatography-tandem mass spectrometry( LCMS/MS). The samples were extracted with perchloric acid and lead acetate solution,and the protein was precipitated. The extraction solution was adjusted to pH 8 using dipotassium hydrogen phosphate,then the solution was purified by solid phase extraction( SPE) and analyzed by LC-MS/MS. The target compounds in the drone pupa powder were determined quantitatively and quantitatively by using multiple reaction monitoring and positive ion or negative ion modes.The recoveries of the 50 antibiotics were in the range of 70. 2%-118. 3%,and the relative standard deviations( RSDs) were 1. 8%-13. 6%. The method is simple,selective,and can be suitable for the analysis and confirmation of veterinary drug residues in drone pupa powder.
A method was established for the determination of 50 kinds of antibiotic residues( macrolides,quinolones,sulfonamides,tetracyclines,nitroimidazoles,lincomycin and chloramphenicol)in drone pupa powder by liquid chromatography-tandem mass spectrometry( LCMS/MS). The samples were extracted with perchloric acid and lead acetate solution,and the protein was precipitated. The extraction solution was adjusted to pH 8 using dipotassium hydrogen phosphate,then the solution was purified by solid phase extraction( SPE) and analyzed by LC-MS/MS. The target compounds in the drone pupa powder were determined quantitatively and quantitatively by using multiple reaction monitoring and positive ion or negative ion modes.The recoveries of the 50 antibiotics were in the range of 70. 2%-118. 3%,and the relative standard deviations( RSDs) were 1. 8%-13. 6%. The method is simple,selective,and can be suitable for the analysis and confirmation of veterinary drug residues in drone pupa powder.
引文
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[8] Zhou F. Journal of Xinyang Agricultural College,2010,20(2):32周枫.信阳农业高等专科学校学报,2010,20(2):132
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[11] Yang A J,Geng Y X. Apiculture of China,2017(11):28杨岸军,耿玉兴.中国蜂业,2017(11):28
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[22] Wang H,Zhao L,Yang H M,et al. Chinese Journal of Chro m ato graphy,2015,33(9):995王浩,赵丽,杨红梅,等.色谱,2015,33(9):995
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