超高效液相色谱-质谱法检测海参中2种头孢类药物的残留

Determination of 2 kinds of cephalosporins residues in sea cucumber by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  头孢类药物  头孢曲松  头孢噻肟  超高效液相色谱-串联质谱法  海参

英文关键词:cephalosporins  ceftriaxone  cefotaxime  ultra performance liquid chromatography-tandem mass spectrometry  sea cucumber

中文摘要:

      目的 建立超高效液相色谱-串联质谱法检测海参中头孢曲松和头孢噻肟的分析方法。方法 样品经磷酸盐缓冲溶液提取, 过HLB固相萃取柱净化。采用0.1%甲酸和甲醇作为流动相进行梯度洗脱, 通过电喷雾离子源正离子检测模式和多重反应监测模式对头孢曲松和头孢噻肟进行定性和定量测定, 基质匹配外标法定量。结果 本方法在6 min内完成头孢曲松和头孢噻肟的分离分析。在5~200 ng/mL浓度范围内线性良好, 相关系数r2大于0.995。2种头孢类药物在5、10和25 μg/kg添加水平的回收率为78.1%~95.3%, 相对标准偏差为3.05%~7.27% (n=6)。方法检出限为2 μg/kg, 定量限为5 μg/kg。结论 该方法快速、准确、灵敏, 适合海参中头孢曲松和头孢噻肟残留的测定。

英文摘要:

      Objective To establish a analytical method for the determination of ceftriaxone and cefotaxime in sea cucumber by ultra performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS). Methods The samples were extracted with phosphate buffer solution and purified by HLB solid-phase extraction column. Gradient elution was performed using 0.1% formic acid and methanol as mobile phases. Ceftriaxone and cefotaxime were qualitatively and quantitatively determined in positive ion detection mode and multiple reaction monitoring mode of electrospray ion source, and quantified by matrix matching external standard method. Results This method completed the analysis of ceftriaxone and cefotaxime within 6 min. The linearity was good over the range of 5? 200 ng/mL, and the correlation coefficient r2 was greater than 0.995. The recoveries of the 2 kinds of cephalosporins at the 5, 10, 25 μg/kg levels were 78.1%?95.3%, and the relative standard deviation was 3.05%?7.27% (n=6). The limit of detection was 2 μg/kg and the limit of quantitation was 5 μg/kg. Conclusion This method is rapid, accurate and sensitive, and is suitable for the determination of ceftriaxone and cefotaxime residues in sea cucumber.