色谱 ›› 2019, Vol. 37 ›› Issue (2): 177-182.DOI: 10.3724/SP.J.1123.2018.10036

• 研究论文 • 上一篇    下一篇

分散固相萃取-超高效液相色谱-串联质谱法测定奶粉中7种非选择性环氧化酶抑制药物

励炯, 孙岚, 金朦娜, 王红青, 邱红钰   

  1. 杭州市食品药品检验研究院, 浙江 杭州 310017
  • 收稿日期:2018-10-26 出版日期:2019-02-09 发布日期:2014-12-31
  • 通讯作者: 励炯,Tel:(0571)85463893,E-mail:jokelee2@126.com
  • 基金资助:

    浙江省食品药品监管系统科技计划项目(2018004);杭州市农业与社会发展科研项目(20180533B19).

Determination of seven non-selective cyclooxygenase inhibitors in milk powder by ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction

LI Jiong, SUN Lan, JIN Mengna, WANG Hongqing, QIU Hongyu   

  1. Hangzhou Institute for Food and Drug Control, Hangzhou 310017, China
  • Received:2018-10-26 Online:2019-02-09 Published:2014-12-31
  • Supported by:

    Science and Technology Plan of Zhejiang Food and Drug Administration (No. 2018004); Agricultural and Social Development Research Project of Hangzhou (No. 20180533B19).

摘要:

建立并优化了使用分散固相萃取-超高效液相色谱-串联质谱(dSPE-UPLC-MS/MS)检测奶粉中7种非选择性环氧化酶(COX)抑制药物残留的方法。样品用0.01 mol/L pH 2.5抗坏血酸溶液-乙腈-乙酸乙酯(2:5:5,v/v/v)溶液提取后,加入无水硫酸钠、十八烷基键合硅胶吸附剂(C18-N)及NH2-丙基乙二胺吸附剂(NH2-PSA)组成的盐包进行净化。以Waters CORTECS UPLC C18(100 mm×2.1 mm,1.6 μm)色谱柱分离,流动相为0.1%(体积分数)甲酸水溶液和0.1%(体积分数)甲酸乙腈,配合多反应监测(MRM)模式定性定量分析水杨酸、布洛芬、双氯芬酸钠、吲哚美辛、吡罗昔康、萘普生和保泰松7种成分。结果表明:7种化合物线性相关性良好,相关系数(r2)≥ 0.9957。高、中、低3个水平下,加标回收率为76.4%~89.8%。定量限为2~5 μg/kg。该方法前处理简单,回收率高,重现性好,可作为奶粉中7种非选择性COX抑制药物残留的有效检测方法。

关键词: 超高效液相色谱-串联质谱, 非选择性环氧化酶抑制药物, 分散固相萃取, 奶粉

Abstract:

An ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction (dSPE-UPLC-MS/MS) method was developed to determine seven non-selective cyclooxygenase inhibitors in milk powder. The samples were extracted with 0.01 mol/L pH 2.5 ascorbic acid-acetonitrile-ethyl acetate solution (2:5:5, v/v/v), and then purified with a mixture of anhydrous sodium sulfate, octadecyl carbon silica gel (C18-N) sorbent and ethylenediamine-N-propyl carbon silica gel (NH2-PSA) sorbent. The analysis was performed using a UPLC-MS/MS system with Waters CORTECS UPLC C18 (100 mm×2.1 mm, 1.6 μm) column. The mobile phase consisted of 0.1% (v/v) formic acid aqueous solution and acetonitrile containing 0.1% (v/v) formic acid by gradient elution, and the multiple reaction monitoring (MRM) mode was used. Five linear calibration curves were obtained with correlation coefficients (r2) ≥ 0.9965. The recoveries were determined at three spiked levels and ranged from 76.4% to 89.8%. The limits of quantification (LOQs) were from 2 to 5 μg/kg. This method is suitable for the determination of seven non-selective cyclooxygenase inhibitors in milk powder.

Key words: dispersive solid phase extraction (dSPE), milk powder, non-selective cyclooxygenase inhibitor, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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