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文章摘要
超高效液相色谱-串联质谱法检测猪肉中多兽药残留
Determination of some kinds of veterinary drugs in porcine muscle by UPLC-MS/MS method
投稿时间:2019-08-20  修订日期:2019-08-20
DOI:
中文关键词: 超高效液相色谱-串联质谱  固相萃取  兽药  残留  猪肉
英文关键词: UPLC-MS/MS, solid-phase extraction, veterinary drugs, residues, porcine muscle
基金项目:国家重点研发计划(2018YFC1602804)
作者单位E-mail
杨兆甜 南京农业大学 食品科技学院 2575467419@qq.com 
吴亚婕 南京农业大学 食品科技学院  
王莹 南京农业大学 食品科技学院  
王雅静 南京农业大学 食品科技学院  
吕青骎 南京农业大学 食品科技学院  
王玮 南京农业大学 食品科技学院 wangwei821220@njau.edu.cn 
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中文摘要:
      建立一种超高效液相色谱-串联质谱(ultra performance liquid chromatography/tandem mass spectrometry, UPLC-MS/MS)法同时检测猪肉中β-受体激动剂类、磺胺类、砜类抑制剂类、喹诺酮类、糖皮质激素类以及大环内酯类的20种兽药残留。待测药物使用80%体积分数的乙腈水溶液提取,经固相萃取小柱净化和氮气吹干后使用体积分数10%甲醇水进行复溶,复溶液经微孔滤膜过滤后进行UPLC-MS/MS测定。使用BEH C18色谱柱梯度洗脱分离,选用电喷雾电离源,正离子扫描及多反应监测模式测定。20种药物检出限(limit of detection, LOD)在0.5~5 μg/kg之间,定量限(limit of quantitation, LOQ)在1.7~16.7 μg/kg之间,当加标水平为1、5、10 μg/kg时,平均回收率在62.1%~118.3%范围内,相对标准偏差(relative standard deviation, RSD)在0.4%~16.7%范围内。已建立的UPLC-MS/MS法可以同时测定20种目标药物,并且兼具简捷、灵敏和精确等优点,能用于猪肌肉中多种兽药残留的高通量检测。
英文摘要:
      An ultra performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of 20 kinds of veterinary drug residues of β-receptor excitations, sulfonamides, sulfone inhibitors, quinolones, glucocorticoids and macrolides in porcine muscle. The detected drugs was extracted with 80% acetonitrile aqueous solution, purified by the solid-phase extraction cartridge, and dissolved with 10% methanol aqueous solution after nitrogen blowing, detected by UPLC-MS/MS after filtering by microfiltration membrane. The BEH C18 column was used for the separation by gradient elution. The identifications were achieved by electrospray ionization in positive mode and detected by multiple reaction monitoring. The limit of detection(LOD) was from 0.5 to 5 μg/kg and the limit of quantitation(LOQ) was from 1.7 to 16.7 μg/kg, the recovery rate range was between 62.1%-118.3% and the relative standard deviation(RSD) was 0.4%-16.7% when the added standard substance concentration was 1, 5, 10 μg/kg. The established UPLC-MS/MS method can detect 20 kinds of targeted drugs simultaneously. This method was simple, sensitive and accurate, which can achieve the simultaneous analysis of some kinds of veterinary drugs in porcine muscle.
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