超高压液相色谱-电喷雾串联四极杆质谱内标法同时测定禽类食品中11种喹诺酮类药物
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(安徽省疾病预防控制中心,安徽 合肥 230601)

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刘柏林 男 主管技师 研究方向为食品安全的理化检验E-mail:liubolin087@163.com┣┣(中)通信作者┫┫

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Simultaneous determination of eleven quinolones drug residues in poultry products by ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry with isotope-labelled internal standards
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(Anhui Provincial Center for Disease Control and Prevention,Anhui Hefei 230601,China)

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    摘要:

    建立同时测定禽类食品中11种喹诺酮类药物残留量的超高压液相色谱-电喷雾串联四极杆质谱(UPLC-ESI-MS/MS)分析方法。方法 鸡肉和鸡蛋样品经1%乙酸乙腈(1∶100,V/V)混合液提取,冷冻离心与正己烷脱脂净化,以10 mmol/L乙酸铵(含0.1%甲酸)-甲醇为流动相,采用电喷雾电离,正离子扫描,多离子反应监测(MRM)模式,基质匹配同位素内标,标准曲线法定量。结果 11种喹诺酮类药物在0.05~50.0 μg/L的浓度范围内线性良好,相关系数R2≥0.997 4,检出限范围为0.05~0.10 μg/kg,平均回收率为82.4%~104.3%,相对标准偏差小于15.0%。结论 该方法的样品前处理过程简单,净化效果好,减少了基质效应的影响,适用于大批量禽类食品中喹诺酮类药物残留量的快速测定。

    Abstract:

    A method for the determination of eleven quinolones drug residues in chicken and egg by the ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry (UPLC-ESI-MS/MS) was established. Methods The analytes in chicken and egg were extracted by 1% acetic acid-acetonitrile, and the fat were separated by centrifugation and extraction using hexane. The eleven analytes were separated by the mobile phase of 10 mmol/L ammonium acetate (contain 0.1% formic acid)-methanol on gradient elution. The identifications were achieved by electrospray ionization in positive mode (ESI+) using multiple reaction monitoring (MRM). The quantifications were performed by the matrix matched isotope-labelled internal standards. Results The calibration curves of the eleven analytes showed a good linearity in the range of 0.05-50.0 μg/L with R2 above 0.997 4. Recoveries were between 82.4% and 104.3% with RSD less than 15.0%. The limits of detection were 0.05-0.10 μg/kg. Conclusion The method had the advantages of simple pretreatment and low matrix effects, which was suitable for the rapid, high-throughput quantitative analysis of quinolones drug residues in poultry food.

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刘柏林,谢继安,赵紫微,王秀莉,单晓梅.超高压液相色谱-电喷雾串联四极杆质谱内标法同时测定禽类食品中11种喹诺酮类药物[J].中国食品卫生杂志,2017,29(3):316-321.

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  • 收稿日期:2017-04-19
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  • 在线发布日期: 2017-07-12
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