HUBEI AGRICULTURAL SCIENCES ›› 2024, Vol. 63 ›› Issue (5): 175-181.doi: 10.14088/j.cnki.issn0439-8114.2024.05.031

• Detection Analysis • Previous Articles     Next Articles

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 Online:2024-05-25 Published:2024-06-04

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

CLC Number: