Journal of Nuclear Agricultural Sciences ›› 2021, Vol. 35 ›› Issue (8): 1865-1874.DOI: 10.11869/j.issn.100-8551.2021.08.1865

• IFood Irradiation·Food Science • Previous Articles     Next Articles

Simultaneous Determination of Five Nitroimidazoles and Diazepam in Aquatic Products by High-Performance Liquid Chromatography-Tandem Mass Spectrometry With Pass-Through Solid Phase Extraction Purification

HE Lianjun1,*, WANG Dingnan2,3, ZHANG Yiming2, WANG Sijia2   

  1. 1Hangzhou Vocational and Technical College, Hangzhou, Zhejiang 310018;
    2College of Agricultural and Food Sciences, Zhejiang A&F University, Hangzhou, Zhejiang 311300;
    3Zhejiang Aquatic Technology Promotion Station, Hangzhou, Zhejiang 310023
  • Received:2020-11-23 Revised:2021-01-07 Online:2021-08-10 Published:2021-06-11

通过型固相萃取-高效液相色谱-串联质谱法同时测定水产品中的5种硝基咪唑和地西泮

何连军1,*, 王鼎南2,3, 张宜明2, 汪思佳2   

  1. 1杭州职业技术学院, 浙江 杭州 310018;
    2浙江农林大学,农业与食品科学学院,浙江 杭州 311300;
    3浙江省水产技术推广总站, 浙江 杭州 310023
  • 通讯作者: *同第一作者。
  • 作者简介:何连军, 男, 副教授, 主要从事色谱、光谱分析技术研究。E-mail: 446490485@qq.com
  • 基金资助:
    杭州市农业与社会发展计划项目(20191203B26),浙江省公益技术研究计划/分析测试项目(LGC20B050007)

Abstract: In order to establish an analytical method for the simultaneous detection of 5 nitroimidazoles (metronidazole, dimenidazole, lonidazole, hydroxy metronidazole, hydroxymethyl metronidazole) and diazepam in aquatic products, a kind of pass-through solid-phase extraction column Captiva EMR-Lipid (EMR) was used to purify the six compounds in aquatic products, and the residual amount was analyzed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The calibration curves of target compounds had good linearity within corresponding concentration ranges and the coefficient ≥ 0.998. Moreover, the average spiked recoveries were between 87.7% and 110.0%, with the relative standard deviations of 0.63% to 11.17%. It has been verified that the established method is suitable for simultaneously determining 5 nitroimidazoles and diazepam in aquatic products with variety of matrix. The method is simple, reliable, easy-to-operability, and is suitable for high-through tests in the laboratory.

Key words: pass-through solid phase extraction, nitroimidazole, diazepam, aquatic products

摘要: 为建立一种同时检测水产品中5种硝基咪唑(甲硝唑、地美硝唑、洛硝哒唑、羟基甲硝唑、羟甲基甲硝咪唑)和地西泮的分析方法,本研究以通过型固相萃取柱Captiva EMR-Lipid(EMR)为净化手段,采用液相色谱-串联质谱法(HPLC-MS/MS)分析水产品中6种目标化合物的残留量。结果表明,样品经缓冲盐调节pH值,乙酸乙酯提取,EMR小柱净化,能有效去除基质干扰。6种目标化合物在在2~100 ng·mL-1 浓度范围内线性良好,相关系数r均不低于0.998,该方法在不同水产品基质中的加标回收率范围为87.7%~110.0%,相对标准偏差为0.63%~11.17%。经验证,本方法适用于多种水产品中5种硝基咪唑和地西泮的同时测定,方法简单可靠,可操作性强,适合于实验室内的大批量检测。

关键词: 通过型固相萃取, 硝基咪唑, 地西泮, 水产品