色谱

色谱 ›› 2016, Vol. 34 ›› Issue (3): 240-248.DOI: 10.3724/SP.J.1123.2015.11003

• 研究论文 • 上一篇    下一篇

分子印迹固相萃取-超高效液相色谱-串联质谱法快速测定猪尿中15种β2-受体激动剂残留

王丽君1,2,3, 曹旭敏2,3, 孙晓亮2,3, 王淑婷2,3, 刘静2, 郝智慧1, 曲宝涵1, 赵思俊2,3   

  1. 1. 青岛农业大学化学与药学院, 山东 青岛 266109;
    2. 中国动物卫生与流行病学中心动物产品安全监测室, 山东 青岛 266032;
    3. 农业部畜禽产品质量安全风险评估实验室(青岛), 山东 青岛 266032
  • 收稿日期:2015-11-02 出版日期:2016-03-08 发布日期:2012-09-28
  • 通讯作者: 曲宝涵, 赵思俊
  • 基金资助:

    国家畜禽质量安全风险评估项目(GJFP2015007);中国动物卫生与流行病学中心创新基金项目(2014IF-0003FF).

Rapid determination of 15 β 2-agonists residues in swine urine by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

WANG Lijun1,2,3, CAO Xumin2,3, SUN Xiaoliang2,3, WANG Shuting2,3, LIU Jing2, HAO Zhihui1, QU Baohan1, ZHAO Sijun2,3   

  1. 1. School of Chemistry and Pharmaceutical Sciences, Qingdao Agricultural University, Qingdao 266109, China;
    2. Department for Safety Supervision of Animal Products, China Animal Health and Epidemiology Center, Qingdao 266032, China;
    3. Livestock and Poultry Products Quality and Safety Risk Assessment Laboratory, Ministry of Agriculture (Qingdao), Qingdao 266032, China
  • Received:2015-11-02 Online:2016-03-08 Published:2012-09-28
  • Supported by:

    National Animal Quality and Safety Risk Assessment Project (No. GJFP2015007); Innovation Fund of China Animal Health and Epidemiology Center (No. 2014IF-0003FF).

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摘要：

建立了分子印迹固相萃取(MISPE)-超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定猪尿中15种 β 2-受体激动剂的分析方法。分别优化了上样溶液的pH值、淋洗和洗脱溶液等MISPE净化条件及质谱条件。将猪尿样品离心,经MISPE柱上样,依次用水、乙腈、0.5%(v/v)乙酸乙腈溶液淋洗,10%(v/v)乙酸甲醇溶液洗脱,氮气吹干,0.1%(v/v)甲酸水-乙腈(9 : 1, v/v)复溶;采用BEH C18色谱柱分离,以乙腈-0.1%(v/v)甲酸水溶液为流动相,采用梯度洗脱,在电喷雾正离子多反应监测模式下外标法定量。考察了MISPE对15种 β 2-受体激动剂的吸附特异性;猪尿中15种 β 2-受体激动剂在0.1~20 μ g/L范围内线性关系良好(r2≥0.992);检出限和定量限分别为0.03和0.1 μ g/L; 15种 β 2-受体激动剂的加标回收率为65.6%~115.0%,批内、批间相对标准偏差分别为0.57%~16.1%和1.11%~16.8%。该方法操作简单、快速、灵敏度高、特异性好。

关键词: 2-受体激动剂, &beta, 超高效液相色谱-串联质谱, 分子印迹固相萃取, 猪尿

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with molecularly imprinted solid phase extraction (MISPE) for rapid determination of 15 β 2-agonists residues in swine urine has been established. In order to obtain the optimized purification conditions, different pH values of loading, washing and elution solvents for the MISPE procedure were optimized. Finally, the swine urine samples (pH 7.0) were performed directly by MISPE column, then the column was washed with water, acetonitrile and 0.5%(v/v) acetic acid in acetonitrile, and eluted with 10%(v/v) acetic acid in methanol. Meanwhile, the parameters of UPLC-MS/MS have been optimized.The UPLC separation was performed on a BEH C18 column, and eluted with the mobile phase consisting of 0.1%(v/v) formic acid aqueous solution and acetonitrile with linear gradient program. The analysis was in ESI positive ion scan mode and multiple reaction monitoring (MRM) mode. Under the optimum conditions, the blank swine urine was spiked with different concentrations analytes and taken for analysis to evaluate the established method. To highlight the advantage of MISPE, specificity adsorption for the 15 β 2-agonists in swine urine was investigate. The linear ranges were 0.1-20 μ g/L for the 15 β 2-agonists ( r 2≥0.992). The limits of detection (LODs) and the limits of quantification (LOQs) were 0.03 and 0.1 μ g/L, respectively. At the spiked levels of 0.1, 0.5 and 2.5 μ g/L in blank samples, the mean recoveries were 65.6%-115.0% with the relative standard deviations (RSDs, n=6) of 0.57%-16.1%. Overall, the proposed method is simple, quick, reliable,sensitive, and can be applied in large scale supervision of illegal usage of the 15 β 2-agonists.

Key words: β 2-agonists, molecularly imprinted solid phase extraction (MISPE), swine urine, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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