色谱 ›› 2019, Vol. 37 ›› Issue (3): 313-318.DOI: 10.3724/SP.J.1123.2018.11002

• 研究论文 • 上一篇    下一篇

QuEChERS-高效液相色谱-串联质谱法同时测定有机肥料中10种氟喹诺酮类药物残留

赵娜1, 梁嘉诚2, 时丽艳1, 吕运开2, 于丽青2   

  1. 1. 河北省产品质量监督检验研究院, 河北 石家庄 050091;
    2. 河北大学化学与环境科学学院, 河北 保定 071000
  • 收稿日期:2018-11-16 出版日期:2019-03-08 发布日期:2015-01-21
  • 通讯作者: 于丽青.E-mail:yuliqinghbdx@126.com.
  • 基金资助:

    河北省自然科学基金(B2016201210,B2016201213);河北省质量技术监督局科技计划(2016ZD19).

Simultaneous determination of ten fluoroquinolone residues in organic fertilizers by QuEChERS and high performance liquid chromatography-tandem mass spectrometry

ZHAO Na1, LIANG Jiacheng2, SHI Liyan1, LÜ Yunkai2, YU Liqing2   

  1. 1. Hebei Academy of Product Quality Supervision & Inspection, Shijiazhuang 050091, China;
    2. College of Chemistry and Environmental Science, Hebei University, Baoding 071000, China
  • Received:2018-11-16 Online:2019-03-08 Published:2015-01-21
  • Supported by:

    Natural Science Foundation of Hebei Province (Nos. B2016201210, B2016201213); Hebei Province Quality and Technical Supervision Bureau Science and Technology Plan (No. 2016ZD19).

摘要:

分析检测有机肥料中的兽药残留对于评价土壤微生物群落和人类健康的潜在风险至关重要。该文建立了一种QuEChERS联用高效液相色谱-串联质谱(HPLC-MS/MS)同时检测有机肥料中10种氟喹诺酮类药物残留的分析方法。样品经乙二胺四乙酸二钠(Na2EDTA)-Mcllvaine缓冲溶液(pH=4.0)和乙腈提取,采用Atlantis T3 C18色谱柱(250 mm×4.6 mm,5 μm),以0.2%(体积分数)甲酸水溶液和乙腈为梯度洗脱的流动相,采用电喷雾离子(ESI)源,在多反应监测(MRM)扫描模式下进行检测。10种氟喹诺酮类药物用内标法定量。结果表明,10种氟喹诺酮类药物在10~500 μg/kg范围内线性关系良好,相关系数均大于0.9930。方法检出限为0.5~2.5 μg/kg,定量限为1.7~8.3 μg/kg。该分析方法成功应用于9个有机肥样品的兽药污染调查。结果显示,样品的平均加标回收率为82.5%~117.1%,相对标准偏差为3.4%~10.2%。该方法准确可靠、灵敏度高,能够满足多种兽药残留的同时检测,该方法有望为有机肥料兽药风险评估提供依据。

关键词: QuEChERS, 残留, 氟喹诺酮, 高效液相色谱-串联质谱, 有机肥料

Abstract:

The analysis of veterinary drugs in organic fertilizers is crucial for an assessment of their potential risks to microbial communities in soils and to human health. A method has been developed for the simultaneous determination of ten fluoroquinolones in organic fertilizers by using the QuEChERS method coupled with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with disodium ethylenediaminetetraacetic acid (Na2EDTA)-McIlvaine buffer (pH=4.0) and acetonitrile. The target compounds were separated on an Atlantis T3 C18 column (250 mm×4.6 mm, 5 μm) with a mobile phase of 0.2% (v/v) formic acid in acetonitrile and analyzed in the multiple reaction monitoring (MRM) mode via electrospray ionization (ESI). Ten fluoroquinolones were quantified by an internal standard method. The calibration curves of the ten fluoroquinolones exhibited good linearity over the range of 10-500 μg/kg, and the correlation coefficients were above 0.9930. The limits of detection were 0.5-2.5 μg/kg; the limits of quantification were 1.7-8.3 μg/kg. The analytical method was successfully applied in a survey of veterinary drug contamination in nine compost samples. The average recoveries were 82.5%-117.1%, with relative standard deviations of 3.4%-10.2%. The method is accurate, reliable, and sensitive and supports the simultaneous detection of various veterinary drug residues. Therefore, this method can provide a basis for the risk assessment of veterinary drugs in organic fertilizers.

Key words: fluoroquinolones, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), organic fertilizers, QuEChERS, residues

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