Simultaneous Determination of Cefotaxime and Its Main Metabolin Residue in Eggs by High Performance Liquid Chromatography - Tandem Mass Spectrometry
文献类型: 外文期刊
第一作者: Yang Xiao-Ti
作者: Yang Xiao-Ti;Tang Xiao-Yan;Shen Xi-Xi;Zhang Xiao-Qing;Yang Xiao-Ti;Shen Xi-Xi
作者机构:
关键词: Egg; Cefotaxime; Desacetylcefotaxime; High performance liquid chromatography-tandem mass spectrometry
期刊名称:CHINESE JOURNAL OF ANALYTICAL CHEMISTRY ( 影响因子:1.134; 五年影响因子:0.909 )
ISSN: 0253-3820
年卷期: 2017 年 45 卷 7 期
页码:
收录情况: SCI
摘要: An efficient method for the analysis of cefotaxime and its metabolite desacetylcefotaxime residues in eggs was developed based on high performance liquid chromatography. tandem mass spectrometry (HPLC-MS/MS). The samples were homogenized and extracted with acetonitrile/water (9:1, V/V) solution. The fat was removed by hexane, and the other impurities were removed with C-18 sorbent. The separation of cefotaxime and desacetylcefotaxime was performed on an Agilent Eclipse Plus C-18 column (100 mm x 2.1 mm, 3.5 mu m) using a mobile phase of 0.2% formic acid (A)-acetonitrile (B) by gradient elution. The analytes were detected by MS/MS in positive electrospray ionization mode (ESI +) and multiple reaction monitoring (MRM), quantitated by matrix. matched extemal standard method. Results showed that the calibration curves had a good linearity in the range of 1.0-143 mu g/L (cefotaxime) and 1.0-120 mu g/L (desacetylcefotaxime), respectively, with correlation coefficient R-2 > 0.999. Limits of detection (LOD, S/N = 3) for cefotaxime and desacetylcefotaxime were 0.07 and 0.14 mu g/kg, and limits of quantitation (LOQ, S/N = 10) for cefotaxime and desacetylcefotaxime were 0.23 and 0. 99 mu g/kg, respectively. At three spiked concentration levels, the recoveries of cefotaxime and desacetylcefotaxime ranged from 83.1% to 103.0% and 88.2% to 101.0%, respectively, both with RSDs (n = 6) less than 6.2%. The results demonstrated that the method was simple, quick, sensitive and reliable, and suitable for determination of cefotaxime and desacetylcefotaxime residues in eggs.
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