湖北农业科学 ›› 2024, Vol. 63 ›› Issue (5): 175-181.doi: 10.14088/j.cnki.issn0439-8114.2024.05.031

• 检测分析 • 上一篇    下一篇

UPLC-MS/MS法同时快速检测有机肥中55种抗菌药物

张柏铭1, 秦立得1,2, 王淑婷1, 刘迎春3, 孙晓亮1, 李雪萍4, 王玉东1, 王晓茵1, 赵思俊1, 曹旭敏1, 刘坤1, 王述柏5, 宋翠平1   

  1. 1.中国动物卫生与流行病学中心,山东 青岛 266032;
    2.山西农业大学动物医学院,山西 晋中 030031;
    3.青岛市畜牧兽医研究所,山东 青岛 266032;
    4.青岛九联集团股份有限公司,山东 青岛 266611;
    5.青岛农业大学动物科技学院,山东 青岛 266032
  • 收稿日期:2022-11-14 出版日期:2024-05-25 发布日期:2024-06-04
  • 通讯作者: 宋翠平(1971-),女,山东潍坊人,正高级兽医师,博士,主要从事动物产品安全监测研究,(电话)13963915205(电子信箱)1575369253@qq.com。
  • 作者简介:张柏铭(2000-),男,山东烟台人,本科生,主要从事动物产品安全监测研究,(电话)18853559551(电子信箱)1820623270@qq.com;共同第一作者,秦立得(1989-),男,山东泰安人,助理研究员,硕士,主要从事动物产品安全监测研究,(电话)15712710612(电子信箱)825149813@qq.com;
  • 基金资助:
    山东省家禽产业技术体系项目(SDAIT-11-14)

Simultaneous and rapid detection of 55 antibacterial drugs in organic fertilizer using UPLC-MS/MS

ZHANG Bai-ming1, QIN Li-de1,2, WANG Shu-ting1, LIU Ying-chun3, SUN Xiao-liang1, LI Xue-ping4, WANG Yu-dong1, WANG Xiao-yin1, ZHAO Si-jun1, CAO Xu-min1, LIU Kun1, WANG Shu-bai5, SONG Cui-ping1   

  1. 1. China Animal Health and Epidemiology Center, Qingdao 266032, Shandong, China;
    2. College of Veterinary Medicine, Shanxi Agricultural University, Jinzhong 030031, Shanxi, China;
    3. Qingdao Institute of Animal Husbandry and Veterinary Medicine, Qingdao 266032, Shandong, China;
    4. Qingdao Jiulian Group Co., Ltd, Qingdao 266611, Shandong, China;
    5. College of Animal Science and Technology, Qingdao Agricultural University, Qingdao 266032, Shandong, China
  • Received:2022-11-14 Published:2024-05-25 Online:2024-06-04

摘要: 建立了同时检测有机肥中磺胺类、大环内酯类、喹诺酮类3类55种抗菌药物残留的超高效液相色谱-串联质谱法(UPLC-MS/MS)。将有机肥研磨、过筛制成试验样品后,使用HLB固相萃取柱净化,上样后依次用去离子水、5%乙腈水溶液淋洗,甲醇/乙酸乙酯溶液(体积比7∶3,含5%氨水)洗脱,氮吹吹干,0.1%甲酸水/乙腈(体积比=9∶1)复溶;在多反应检测模式下进行测定,外标法定量。结果表明,4批有机肥中55种药物在1.0~100 μg/kg范围内线性关系良好(R2>0.990 0),该方法的检出限为2.0~7.5 μg/kg,定量限为5.0~25.0 μg/kg,各种药物的回收率为60.2%~118.7%,批内相对标准偏差(n=5)为0.5%~15.0%,批间相对标准偏差(n=20)为4.3%~24.1%。该方法简单可靠,净化效果好,适用于有机肥中磺胺类、喹诺酮类、大环内脂类药物的同时检测。

关键词: 有机肥, 超高效液相色谱-串联质谱法(UPLC-MS/MS), 快速检测, 抗菌药物

Abstract: An ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous detection of 55 types of antibacterial drugs, including sulfonamides, macrolides, and quinolones, in organic fertilizer.After grinding and sieving the organic fertilizer into experimental samples, they were purified using HLB solid-phase extraction column. After loading, the samples were sequentially washed with deionized water and 5% acetonitrile aqueous solution, eluted with methanol/ethyl acetate solution (volume ratio 7∶3, containing 5% ammonia), blown dry with nitrogen, and re-dissolved in 0.1% formic acid water/acetonitrile (volume ratio 9∶1);measurement was carried out in a multi reaction detection mode, with the external standard method for quantification. The results showed that among the four batches of organic fertilizers, 55 drugs had a good linear relationship (R2>0.990) within the range of 1.0~100 μg/kg,the detection limit of this method was 2.0~7.5 μg/kg,the quantitative limit was 5.0~25.0 μg/kg,the recovery rates of various drugs were 60.2%~118.7%,the relative standard deviation within the batch (n=5) was 0.5%~15.0%, and the relative standard deviation between batches (n=20) was 4.3%~24.1%. This method was simple and reliable, with a good purification effect, and was suitable for the simultaneous detection of sulfonamide, quinolone, and macrocyclic lipid drugs in organic fertilizer.

Key words: organic fertilizer, UPLC-MS/MS, rapid detection, antibacterial drugs

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