Chinese Journal of Applied Chemistry ›› 2018, Vol. 35 ›› Issue (6): 722-728.DOI: 10.11944/j.issn.1000-0518.2018.06.170245

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Quantitative Analysis of Cephalosporin C in Soil by High Performance Liquid Chromatography with Ultrasound-assisted Extraction and Solid-Phase Extraction

WANG Yuea,CAI Chenb,LIU Huilingb,SUN Lic,LI Yanchaod,MENG Zhaohonga*()   

  1. aCollege of Geographic Science,Harbin Normal University,Harbin 150025,China
    bState Key Laboratory of Urban Water Resources and Environment,Harbin Institute of Technology,Harbin 150090,China
    cCollege of Geographic Science,Harbin Normal University,Harbin 150025,China
    dElectronic Engineering College,Heilongjang University,Harbin 150080,China
  • Received:2017-07-12 Accepted:2017-11-09 Published:2018-06-01 Online:2018-05-28
  • Contact: MENG Zhaohong
  • Supported by:
    Supported by the National Natural Science Foundation of China(No.41401589), the Natural Science Foundation of Heilongjiang Province, Special Research Funds for the Universities of Heilongjiang Province(No.HDRCCX-2016Z10)

Abstract:

A rapid and simple method based on ultrasound-assisted extraction, solid-phase extraction followed by high performance liquid chromatography(UAE-SPE-HPLC) was proposed for the determination of cephalosporin C(CPC) in soil. The optimum pre-treatment parameters for the soil samples contaminated with CPC are as follow: ultra-pure water as extraction solvent for CPC, SPE as solid phase extraction cartridge, 5.0 mL 10% methanol as rinse solvent, 2.0 mL 5% formic acid/methanol solution(volume ratio 50:50) as eluent. The results show that when 0.1% formic acid and methanol(95:5), 30 ℃ column temperature, and 254 nm detection wavelength were applied during the isocratic elution process, HPLC assay offeres a good potential for the sensitive and selective determination of CPC. The recovery rates for seven different treatments are 77.9%~98.8%, and the precision is 5.0%~6.3%(n=5). The limit of determination(LOD) and the limit of quantification(LOQ) in soil are 340.4 μg/kg and 1126.8 μg/kg, respectively. At the same time, this method was used to detect the positive soil near the pharmaceutical factory in Xinjiang. The experimental results of different batches show detected(below LOQ), 1532.1 μg/kg and detected(below LOQ), respectively. In conclusion, UAE-SPE-HPLC is simple and rapid. Its accuracy and precision are in line with the quality control requirements. It is suitable for the detection of trace CPC in soil.

Key words: cephalosporin C, soil, ultrasound-assisted extraction, solid-phase extraction, high performance liquid chromatography