Citation: YANG Xiao-Ti, TANG Xiao-Yan, SHEN Xi-Xi, ZHANG Xiao-Qing. Simultaneous Determination of Cefotaxime and Its Main Metabolin Residue in Eggs by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(7): 1019-1024. doi: 10.11895/j.issn.0253-3820.170145 shu

Simultaneous Determination of Cefotaxime and Its Main Metabolin Residue in Eggs by High Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
Key Laboratory of Agrifood Safety and Quality, Ministry of Agriculture, Institute of Quality Standards and Testing Technology for Agro-products, Chinese Academy of Agricultural & Science, Beijing 100081, China;
2.
National Centre of Meat Quality and Safety Control, Nanjing Agricultural University, Nanjing 210095, China

Received Date: 13 March 2017
Revised Date: 17 May 2017

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 C₁₈ sorbent. The separation of cefotaxime and desacetylcefotaxime was performed on an Agilent Eclipse Plus C₁₈ column (100 mm × 2.1 mm, 3.5 μm) 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 μg/L (cefotaxime) and 1.0-120 μg/L (desacetylcefotaxime), respectively, with correlation coefficient R²>0.999. Limits of detection (LOD, S/N=3) for cefotaxime and desacetylcefotaxime were 0.07 and 0.14 μg/kg, and limits of quantitation (LOQ, S/N=10) for cefotaxime and desacetylcefotaxime were 0.23 and 0.99 μg/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.
- Egg,
- Cefotaxime,
- Desacetylcefotaxime,
- High performance liquid chromatography-tandem mass spectrometry
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1.
沈阳化工大学材料科学与工程学院沈阳 110142