图雅,崔建平,赵宏.同位素内标-超高效液相色谱-串联质谱法测定蜂蜜中氯霉素及甲硝唑[J].中国食品卫生杂志,2017,29(4):450-453. 本文二维码信息
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同位素内标-超高效液相色谱-串联质谱法测定蜂蜜中氯霉素及甲硝唑
Determination of chloramphenicol and metronidazolel in honey by ultra performance liquid chromatography-mass spectrometry with isotope-labelled internal standards
投稿时间:2017-05-20  
DOI:
中文关键词:  超高效液相色谱-串联质谱  同位素内标  甲硝唑  氯霉素  蜂蜜  食品污染物  兽药残留
Key Words:Ultra performance liquid chromatography-tandem mass spectrometry  isotope labelled internal standards  metronidazolel  chloramphenicol  honey  food contaminants  veterinary drug residues
基金项目:
作者单位E-mail
图雅 内蒙古呼和浩特市疾病预防控制中心,内蒙古 呼和浩特 010070 tuya1983@126.com 
崔建平 内蒙古呼和浩特市疾病预防控制中心,内蒙古 呼和浩特 010070  
赵宏 内蒙古呼和浩特市疾病预防控制中心,内蒙古 呼和浩特 010070  
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中文摘要:
      目的 采用同位素内标-超高效液相色谱-串联质谱法测定蜂蜜中氯霉素及甲硝唑的残留量。方法 样品经乙酸乙酯提取,MCS复合型固相萃取柱(500 mg/6 ml)净化,采用ZORBAXSB-C18色谱柱(2.1 mm×100 mm,1.8 μm)分离,以甲醇和5 mmol/L乙酸铵溶液(含0.05%甲酸)为流动相进行梯度洗脱,采用电喷雾正/负离子多反应监测模式检测,同位素内标法定量。结果 氯霉素、甲硝唑的浓度为0.05~5.00 ng/ml时,线性关系良好,相关系数r>0.999。添加0.5、2.0、5.0 μg/kg三个不同水平时,氯霉素、甲硝唑的回收率为79.3%~96.7%,相对标准偏差(RSD)为5.5%~14.8%,定量限均为0.15 μg/kg,检出限均为0.05 μg/kg。结论 该方法灵敏度及准确度良好,可应用于日常大批量样品的高灵敏分析。
Abstract:
      Objective To determine chloramphenicol and metronidazolel in honey by isotope-labelled internal standards ultra performance liquid chromatography-mass spectrometry. Methods Samples were extracted with ethyl acetate solution, and cleaned up on a MCS cartridge. The target analytes were separated on a ZORBAX SB-C18 column with gradient elution using a mobile phase made up of methanol and 5 mmol/L ammonium acetate solution (containing 0.05% formic acid). Detection was carried out using positive and negative electrospray ionization and multiple reaction monitoring (MRM), and quantified with isotope internal standardmethod . Results The chloramphenicol and metronidazolel showed good linearity in the range of 0.05-5.00 ng/ml. The recovery at three spiked levels of 0.5,2.0 and 5.0 μg/kg were in the range of 79.3%-96.7%. The relative standard deviation (RSD) was 5.5%-14.8%. The limits of quantitation were 0.15 μg/kg, the limits of detection were 0.05 μg/kg. Conclusion The method is sensitive and accurate. It could be applied to the high-throughput analysis of chloramphenicol and metronidazolel.
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