食品科学

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分散固相萃取-超高效液相色谱-串联质谱检测水产品中14 种喹诺酮类药物

李佩佩,张小军,梅光明,严忠雍,龙 举,刘 琴,郭远明*   

  1. 浙江省海洋水产研究所,浙江省海水增养殖重点实验室,浙江 舟山 316100
  • 出版日期:2014-12-25 发布日期:2014-12-29
  • 通讯作者: 郭远明
  • 基金资助:

    浙江省重点科技创新团队项目(2010R50028);浙江省科技计划项目(2013C37072;2012F20026)

Determination of 14 Quinolone Antibiotics in Aquatic Products by Dispersive Solid-phase Extraction and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

LI Pei-pei, ZHANG Xiao-jun, MEI Guang-ming, YAN Zhong-yong, LONG Ju, LIU Qin, GUO Yuan-ming*   

  1. Zhejiang Province Key Laboratory of Mariculture and Enhancement,
    Marine Fisheries Research Institute of Zhejiang, Zhoushan 316100, China
  • Online:2014-12-25 Published:2014-12-29
  • Contact: GUO Yuan-ming

摘要:

采用基质固相分散的前处理技术,建立一种超高效液相色谱-串联质谱同时检测水产品中14 种喹诺酮类药物的分析方法。样品用5%甲酸-乙腈溶液提取和盐析剂盐析后加入N-丙基乙二胺和十八烷基键合硅胶吸附剂(C18)净化剂进行基质固相分散净化,氮吹复溶后经Waters ACQUITY UPLC BEH C18柱(50 mm×2.1 mm,1.7 μm)分离,以0.2%甲酸溶液和甲醇为流动相梯度洗脱,采用电喷雾离子源正离子多反应监测模式测定,外标法定量。14 种药物在0.50~20.0 μg/L质量浓度范围内呈良好线性,线性相关系数不小于0.995,方法检出限为0.4~1.0 μg/kg,定量限为1.0~3.0 μg/kg。14 种药物在3 个加标水平下的平均回收率为82%~90%,相对标准偏差(n=5)均小于11.0%。本方法简便快速、灵敏度高、实用性强,可作为水产品中14 种喹诺酮类药物残留的快速确证和定量分析。

关键词: 基质固相分散, 超高效液相色谱-串联质谱, 水产品, 喹诺酮类药物

Abstract:

A method for the simultaneous analysis of 14 quinolone (QN) residues in aquatic products by dispersive solidphase
extraction and liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) was established. The sample was
extracted with acetonitrile (containing 5% formic acid) and followed by salting-out. Clean up of the extracts was performed
using PSA and C18 during the dispersive solid-phase extraction procedure. After evaporated to dryness under a stream of
nitrogen, the analytes were then separated on a Waters ACQUITY UPLCTM BEH C18 column (50 mm × 2.1 mm, 1.7 μm)
using binary mobile phase gradient with water containing 0.2% formic acid and methanol. The targeted compounds were
detected under a multiple reaction monitoring (MRM) mode and quantified by an external standard method. The linearity of
all 14 QNs in the range from 0.50 to 20.0 μg/L exhibited correlation coefficients greater than 0.995. The limits of detection
(LOD) and the limits of quantification (LOQ) were 0.4–1.0 and 1.0–3.0 μg/kg, respectively. The average recoveries of 14
QNs at three level spiked concentrations ranged from 82% to 90%, with relative standard deviations (n = 5) less than 11.0%.
This method was simple, rapid, sensitive and reliable, and could be applied to determine 14 QNs in aquatic products.

Key words: dispersive solid-phase extraction, ultra performance liquid chromatography-tandem mass spectrometry (UPLCMS- MS), aquatic products, quinolones

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