广东畜牧兽医科技 ›› 2022, Vol. 47 ›› Issue (5): 28-34.DOI: 10.19978/j.cnki.xmsy.2022.05.06

• 试验研究 • 上一篇    下一篇

HPLC⁃MS/MS同位素内标法测定鸡蛋中14种喹诺酮类药物残留量

刘佩怡,伍宏凯,梁祺琦,李律雯   

  1. (广东省农产品质量安全中心(广东省绿色食品发展中心),广东 广州 510230)
  • 出版日期:2022-11-01 发布日期:2022-10-18
  • 通讯作者: 白挨泉

Determination of 14 quinolones residues in eggs by HPLC⁃ MS/MS with isotopic internal standard

LIU Peiyi ,WU Hongkai ,LIANG Qiqi,LI Luwen   

  1. (Guangdong agriculture products quality and safety center,Guangzhou Guangdong 510230)
  • Online:2022-11-01 Published:2022-10-18

摘要: 本研究建立了同时测定鸡蛋中14种喹诺酮类药物残留的高效液相色谱?串联质谱方 法。样品经EDTA?Mcllvaine缓冲液提取,正己烷脱脂,HLB固相萃取柱净化,反相C 18色谱柱 分离,采用多反应监测正离子模式测定,使用同位素内标法定量。在优化条件下,14种喹诺酮 类药物均能达到检测限0.5 μg/kg,定量限2 μg/kg。在2~100 ng/mL的质量浓度范围内线性良 好,相关系数r均大于0.99。在空白鸡蛋中添加2,5,10 μg/kg水平的药物回收试验中,平均回 收率在83.9%~110.7%之间,批内变异系数在1.5% ~13.7%之间(n=6),批间变异系数在4.5%~ 13.1%之间(n=18)。结果表明,该方法灵敏、准确、重复性好,适用于鸡蛋中喹诺酮类药物残留 的定性定量检测。

关键词: 鸡蛋, 喹诺酮类药物, 同位素内标法, 高效液相色谱?串联质谱

Abstract: A high performance liquid chromatography ?tandem mass spectrometry method was developed for the simultaneous determination of 14 quinolones residues in eggs. The samples were extracted with EDTA ? Mcllvaine buffer,followed by defatted with n?hexane,and purified by HLB solid phase extraction column,separated by reversed? phase C 18 column,determined by multiple reaction monitoring positive ion mode,and quantified by isotope internal standard method. Under the optimized conditions,the detection limit and quantification limit of 14 quinolones were 0.5 μg/kg and 2 μg/kg,respectively. The linearity was fine in the range of 2~100 ng/mL,and the correlation coefficients r was greater than 0.99. Adding 2,5,and 10 μg/kg to blank eggs sample,the average recoveries were 83.9%~110.7%,the intra ?assay coefficient of variation were between 1.5% and 13.7%(n=6),and the inter ?assay coefficient of variation were from 4.5% to 13.1%(n=18). The results showed that the method was sensitive,accurate, and reproducible,and was suitable for the qualitative and quantitative detection of quinolones residues in eggs.

Key words: Eggs, Quinolones, Isotopic internal standard method, High performance liquid chromatography?tandem mass spectrometry(HPLC?MS/MS)

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