超高效液相色谱-串联质谱法测定鸭肝中的头孢曲松钠

Determination of ceftriaxone sodium in duck liver by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  头孢曲松钠  HLB固相萃取小柱  超高效液相色谱串联质谱法  鸭肝

英文关键词:ceftriaxone sodium  HLB solid phase extraction column  ultra performance liquid chromatography- tandem mass spectrometry  duck liver

中文摘要:

      目的 建立超高效液相色谱-串联三重四极杆质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定鸭肝中头孢曲松钠的分析方法。方法 样品经乙腈水溶液(8:2,V:V)提取, 以hydrophilic-lipophilic balance (HLB)固相萃取小柱净化, 采用甲醇-0.1%甲酸水溶液为流动相, Agilent EclipsePlus C18 RRHD为分离柱, 进行梯度洗脱, 串联质谱ESI正模式电离, 多反应监测(multiple reaction monitoring, MRM)模式检测, 以保留时间和子离子比定性, 外标法定量。结果 头孢曲松钠在2~40 μg/L范围内线性关系良好, 相关系数均大于 0.999, 方法检出限(S/N=3)为1.0 μg/kg, 加标水平为2~10 μg/kg (n=6)时, 平均回收率为84.5%~94.6%, 相对标准偏差(RSD)＜6%。结论 本方法准确、灵敏, 可适用于鸭肝中头孢曲松钠抗生素的测定。

英文摘要:

      Objective To establish a method for determination of ceftriaxone sodium in duck liver by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with a mixture of water-acetonitrile (8:2, V:V), and cleaned up with a hydrophilic-lipophilic balance (HLB) solid phase extraction column. The gradient elution was performed by methanol-0.1% acid solution, with Agilent EclipsePlusC18 as the separation column. The samples were analyzed by UPLC-MS/MS in positive ionization mode and multiple reaction monitoring (MRM) mode. The ratio of retention time and ion was used for qualitative analysis, and the external standard method was used for quantitative analysis. Results The calibration curve was linear in the range of 2~40 μg/L with the correlation coefficient above 0.999, and the limit of quantification (LOD, S/N=3) for ceftriaxone sodium was 1.0 μg/kg. The average recoveries for ceftriaxone sodium at spiked levels of 2~10 μg/kg were in the range of 84.5%~94.6%, with RSD＜6% (n=6). Conclusion This method is accurate and sensitive, which is suitable for the determination of ceftriaxone sodium antibiotics in duck liver.