超高效液相色谱串联质谱同时测定豆芽、豆干、火锅底料中喹诺酮类、磺胺类、硝基咪唑类、四环素类42种抗生素药物
作者:
作者单位:

四川省食品检验研究院,四川 成都 611700

作者简介:

苏燕 女 助理工程师 研究方向为食品安全 E-mail: suyan2626@163.com

通讯作者:

魏宇涛 男 工程师 研究方向为食品安全 E-mail: 314474984@qq.com

中图分类号:

R155

基金项目:

食品补充检验方法项目(修订BJS201909)


Simultaneous determination of 42 antibiotics of quinolones, sulfonamides, nitroimidazoles and tetracycline in bean sprouts, dried tofu and hot pot seasoning by ultra-performance liquid chromatography tandem mass spectrometry
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Affiliation:

Sichuan Institute of Food Inspection, Sichuan Chengdu 611700, China

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    摘要:

    目的 建立并优化同时测定豆芽、豆干、火锅底料中喹诺酮类、磺胺类、硝基咪唑类、四环素类共42种抗生素的超高效液相色谱串联质谱检测方法。方法 样品经70%乙腈-水(含0.1%甲酸)提取后,经PRiME HLB净化,采用Agilent Eclipse Plus C18柱(150 mm×3.0 mm,1.8 μm)进行分离,以0.2%甲酸乙腈和0.2%甲酸水为流动相梯度洗脱,采用电喷雾离子源正离子动态多反应监测模式测定,外标法定量。结果 豆芽、豆干、火锅底料基质中喹诺酮类、磺胺类、硝基咪唑类药物的线性范围为2~80 ng/mL,方法检出限均为5 μg/kg;四环素类药物的线性范围为10~400 ng/mL,方法检出限均为25 μg/kg;相关系数均大于0.997。42种抗生素在三个加标水平下平均回收率为85.4%~119.3%,相对标准偏差(n=6) 0.4%~13.4%。结论 该方法应用范围广、操作简便,灵敏度高,可对豆芽、豆干、火锅底料中喹诺酮类、磺胺类、硝基咪唑类、四环素类多种抗生素药物的浓度进行快速筛查。

    Abstract:

    Objective A high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 42 kinds of antibiotics including quinolones, sulfonamides, nitroimidazoles and tetracyclines was developed for bean sprouts, dried bean curd and hot pot seasoning.Methods The samples were extracted with 70% acetonitrile-water (containing 0.1% formic acid), purified by PRiME HLB, and separated by an Agilent Eclipse Plus C18 column (150 mm×3.0 mm, 1.8 μm) with 0.2% formic acid acetonitrile and 0.2% formic acid water as gradient elution of mobile phase. The detection was performed under positive ion dynamic multiple reaction monitoring mode with electrospray ion source, and external standard method were used for quantification.Results The linear range of quinolones, sulfonamides and nitroimidazoles in bean sprouts, dried tofu and hot pot seasoning was 2-80 ng/mL, and the limit of detection was 5 μg/kg; the linear range of tetracyclines was 10-400 ng/mL, and the limit of detection was 25 μg/kg; the correlation coefficients were all greater than 0.997. The average recoveries of 42 kinds of antibiotics in three spiked levels were 85.4%-119.3%, and the relative standard deviations (n=6) was 0.4%-13.4%.Conclusion The method has a wide range of applications with easy operation and high sensitivity, and can rapidly screen the concentration of quinolones, sulfonamides, nitroimidazoles and tetracyclines in bean sprouts, dried tofu and hot pot seasoning.

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苏燕,魏宇涛,李澍才,余晓琴,杜钢.超高效液相色谱串联质谱同时测定豆芽、豆干、火锅底料中喹诺酮类、磺胺类、硝基咪唑类、四环素类42种抗生素药物[J].中国食品卫生杂志,2023,35(1):65-71.

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  • 收稿日期:2022-01-10
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  • 在线发布日期: 2023-03-07
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