Citation: ZHANG Xiaogang, WANG Xia, DAI Chunfeng, CHEN Meilian. Determination of six cephalosporin residues in milk by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2018, 36(4): 345-350. doi: 10.3724/SP.J.1123.2017.11007 shu

Determination of six cephalosporin residues in milk by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry

Shanghai Agricultural Products Quality and Safety Testing Center, Ministry of Agriculture Food Quality Supervision and Inspection Center(Shanghai), Ministry of Agriculture-Milk Risk Assessment Laboratory(Shanghai), Shanghai 201708, China

Received Date: 6 November 2017

Fund Project: Special Public Welfare Industry (Agriculture) Research (No. 201403071).

A simple, rapid and sensitive method for the simultaneous determination of six cephalosporin (cephalexin, cephapirin, cefotaxime, cefazolin, cefalonium and cefquinome) residues in milk was developed by QuEChERS coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The milk samples were extracted with 10 mL acetonitrile containing 1%(v/v) acetic acid, and then centrifuged for 10 min.The supernatant was cleaned up with 100 mg C18 adsorbent powder.The analytes were separated on a reversed phase HSS T3 column (100 mm×2.1 mm, 1.8 μm) using acetonitrile and water containing 0.1%(v/v) formic acid as mobile phases with gradient elution.An electrospray ionization (ESI) source was used in the multiple reaction monitoring (MRM) mode.The analytes were quantified using an external standard method.The linear relationships of the six cephalosporins were good and the correlation coefficients (r) were greater than 0.999.The limits of detection (LODs) and the limits of quantification (LOQs) for the analytes were in the range of 0.2-0.6 μg/kg and 0.8-2 μg/kg, respectively.The recoveries of the target analytes were between 75.1% and 94.4% at spiked levels of 8, 16, 80 μg/kg.The relative standard deviations (RSDs) were no more than 8.3%(n=6).The method is simple and sensitive, and can be suitable for the analysis of the cephalosporin residues in milk.
- ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- QuEChERS,
- cephalosporins,
- milk
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