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食品与发酵工业  2021, Vol. 47 Issue (18): 250-257    DOI: 10.13995/j.cnki.11-1802/ts.027385
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
超高效液相色谱-三重四级杆质谱多反应监测模式测定奶粉中56种违禁药物残留
周春红1*, 许晓辉2
1(甘肃省产品质量监督检验研究院,甘肃 兰州,730000)
2(兰州市食品药品检验检测研究院,甘肃 兰州,730000)
Determination of 56 drug residues in milk powder by high performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode
ZHOU Chunhong1*, XU Xiaohui2
1(GanSu Province Product Quality Supervision and Inspection Research Institute, Lanzhou 730000, China)
2(Lanzhou Institute for Food and Drug Control, Lanzhou 730000, China)
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摘要 建立了超高效液相色谱-串联质谱法(ultra-performance liquid chromatography-MS/MS,UPLC-MS/MS)同时分析成人奶粉中56种药物残留的方法。样品经水溶解及酸化乙腈提取,QuEchERS净化,UPLC-MS/MS测定,采用电喷雾电离源,多反应监测模式检测,外标法定量。结果表明,56种药物在各自线性范围内呈现良好的线性关系,相关系数均大于0.999,检出限为0.06~5.47 μg/kg,定量限为0.21~16.53 μg/kg;成人奶粉在2、5、10 μg/kg加标水平下平均回收率为61.3%~129.8%,相对标准偏差(n=6)为0.090%~7.171%。该方法操作简便快速,灵敏度和稳定性较好,可以广泛应用于成人奶粉样品中多种违禁药物的快速筛查和定量检测。
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周春红
许晓辉
关键词:  超高效液相色谱-质谱/质谱联用法  多反应监测  成人奶粉  药物残留    
Abstract: A high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the simultaneous analysis of 56 drug residues in milk powder. Each sample was dissolved in water and extracted with acidified acetonitrile, then purified with QuEchERS, and finally detected by LC-MS/MS with electrospray ionization in multiple reaction monitoring mode. Some compounds were quantified by the external standard method. The results showed that there were good linear relationships for 56 drugs with correlation coefficients not less than 0.999. The detection limits and quantification for 56 drug residues were 0.06-5.47 and 0.21-16.53 μg/kg respectively. The average recoveries at three spiked levels of 2, 5 and 10 μg/kg were in the range of 61.3%-129.8% which with relative standard deviations (RSD) of 0.090%-7.171% (n=6). Thus, the optimized method is rapid, simple and easy. And it can be widely used in the rapid screening and quantitative detection of multiple drug residues in adult milk powder.
Key words:  high performance liquid chromatography-tandem mass spectrometry    multiple reaction monitoring mode    adult milk powder    drug residues
收稿日期:  2021-03-22      修回日期:  2021-05-31                发布日期:  2021-10-18      期的出版日期:  2021-09-25
基金资助: 甘肃省知识产权计划资助项目(20ZSCQ041)
作者简介:  硕士,正高级工程师(本文通讯作者,E-mail:2964643202@qq.com)
引用本文:    
周春红,许晓辉. 超高效液相色谱-三重四级杆质谱多反应监测模式测定奶粉中56种违禁药物残留[J]. 食品与发酵工业, 2021, 47(18): 250-257.
ZHOU Chunhong,XU Xiaohui. Determination of 56 drug residues in milk powder by high performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode[J]. Food and Fermentation Industries, 2021, 47(18): 250-257.
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http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.027385  或          http://sf1970.cnif.cn/CN/Y2021/V47/I18/250
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