固相萃取-超高效液相色谱-同位素稀释串联质谱法测定蜂蜜中的甲硝唑和氯霉素
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摘要
建立了同时测定蜂蜜中甲硝唑和氯霉素残留量的固相萃取-超高效液相色谱-同位素稀释串联质谱方法。蜂蜜样品中的甲硝唑和氯霉素经乙酸乙酯提取后,采用InertSep RP-1固相萃取柱对目标物进行富集和净化。经超高效液相色谱分离后,在三重四极杆质谱的多反应监测模式(MRM)下,甲硝唑通过正离子模式(ESI+)采集,氯霉素通过负离子模式(ESI-)采集,采用同位素稀释的内标法定量。本方法在浓度1~100ng/mL范围内具有良好的线性关系,相关系数R2>0.999。在添加水平为0.5、2.5、25μg/kg时,回收率在71.4%~123.4%之间,相对标准偏差为5.0%~12.3%。本方法采用一种前处理方式,可以同时测定蜂蜜中的甲硝唑与氯霉素残留,缩短了分析时间,提高了检测效率。
A reliable method using ultra high performance liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS)for the simultaneous identification and quantitation of metronidazole and chloramphenicol in honey was developed and validated.The two analytes were extracted by ethyl acetate.An InertSep RP-1solid-phase extraction cartridge was used for the clean-up step.After the chromatographic separation on an Endeavorsil C18 column,metronidazole was detected by a triple quadrupole instrument operating in positive mode,and chloramphenicol was analyzed in negative mode,respectively.The quantification was achieved by isotope dilution internal standard method.The method showed a good linear response in the range of1-100ng/mL,with correlation coefficients exceeding 0.999 for the two compounds.The average recoveries at three spiked levels ranged from 71.4% to 122.4% with the relative standard deviations below 12.3%.The method has been successfully evaluated through application to honey samples.
A reliable method using ultra high performance liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS)for the simultaneous identification and quantitation of metronidazole and chloramphenicol in honey was developed and validated.The two analytes were extracted by ethyl acetate.An InertSep RP-1solid-phase extraction cartridge was used for the clean-up step.After the chromatographic separation on an Endeavorsil C18 column,metronidazole was detected by a triple quadrupole instrument operating in positive mode,and chloramphenicol was analyzed in negative mode,respectively.The quantification was achieved by isotope dilution internal standard method.The method showed a good linear response in the range of1-100ng/mL,with correlation coefficients exceeding 0.999 for the two compounds.The average recoveries at three spiked levels ranged from 71.4% to 122.4% with the relative standard deviations below 12.3%.The method has been successfully evaluated through application to honey samples.
引文
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[2]Huang X,Lin J,Yuan D.Journal of Separation Science,2011,34(16-17):2138.
[3]WEI L,LI Y,CHEN S C,et al.Journal of Food Safety and Quality(魏玲,李越,陈舜琮,等.食品安全质量检测学报),2013,4(4):1095.
[4]CAO Y P,XIN C L,JI P.Journal of Analytical Science(曹艳平,辛成龙,季萍.分析科学学报),2015,31(4):545.
[5]Ministry of Agriculture.No.193Bulleting of the Ministry of Agriculture of the People’s Republic of China.(农业部.中华人民共和国农业部公告193号.食品动物禁用的兽药及其他化合物清单).[2002-4-15].http://www.moa.gov.cn/zwllm/tzgg/gg/201104/t20110422_1976324.htm.
[6]WEI N.China Inspection and Quarantine Times(魏宁.中国国门时报).2015-04-28.http://cngm.cqn.com.cn/html/2015-04/28/content_22728.htm?div=-1.
[7]ZHANG H W,JIAN H M,LIN L M,et al.Journal of Instrumental Analysis(张鸿伟,简慧敏,林黎明,等.分析测试学报),2012,31(7):763.
[8]CHEN H Y,DING L,LIU M L.Chemical Journal of Chinese Universities(陈海燕,丁兰,刘密兰.高等学校化学学报),2015,36(1):67.
[9]GB/T 23410-2009.Determination of Residues of Nitroimidazoles and Their Metabolites in Honey-LC-MS/MS Method(蜂蜜中硝基咪唑类药物及其代谢物残留量的测定液相色谱-质谱-质谱法中华人民共和国国家标准).
[10]Kanda M,Sasamoto T,Takeba K,Hayashi H,Kusano T,Matsushima Y,Nakajima T,Kanai S,Takano I.Journal of AOAC International,2012,95(3):923.
[11]LIU Y M,CAO Y Z,LI J,et al.Chinese Journal of Chromatography(刘永明,曹彦忠,李金,等.色谱),2010,28(6):596.
[12]Mitrowska K,Posyniak A,Zmudzki Jan.Analytical Letters,2014,47(10):1634.