FOOD SCIENCE ›› 2020, Vol. 41 ›› Issue (22): 330-336.doi: 10.7506/spkx1002-6630-20190717-224

• Safety Detection • Previous Articles    

Determination of Ten Cephalosporin Residues in Bee Products by Ultra-high Performance Liquid ChromatographyTandem Mass Spectrometry Coupled with PRIME HLB Solid Phase Extraction

ZHANG Hao, WU Yinliang, ZHANG Yiwen, CHEN Guo, JIANG Xiaoxiao   

  1. (1. Laboratory of Quality and Safety Risk Assessment for Agricultural Products (Ningbo), Ministry of Agriculture and Rural Affairs, Ningbo Academy of Agricultural Sciences, Ningbo 315040, China; 2. Beijing Institute of Metrology, Beijing 100012, China)
  • Online:2020-11-25 Published:2020-11-26

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry method for the simultaneous quantitative determination of residues of 10 cephalosporins in bee products, including honey, royal jelly and lyophilized royal jelly powder, was established. The samples were extracted with 10% formic acid solution. After being purified by solid-phase microextraction using an Oasis PRIME HLB cartridge, the extract was blown to dryness under a stream of nitrogen gas and then re-dissolved. The analytes were separated on an Acquity UPLC BEH C18 column with a mixture of 0.1% formic acid solution and methanol as the mobile phase by gradient elution. The analysis was carried out using a positive electrospray ion source in the multiple reaction monitoring mode. The matrix-matched external standard method was applied for the quantitative analysis. There were good linear relationships for 10 cephalosporins in certain concentration ranges, with correlation coefficients of more than 0.999. The limits of detection (LODs) for 10 cephalosporins were 0.1–1 μg/kg, and the limits of quantitation (LOQs) were 0.3–3 μg/kg. The recoveries for the analytes spiked into blank bee products were in the range of 80.0%–95.5%, with relative standard deviations of 1.5%–4.8%. This method was time-saving and suitable for the determination of cephalosporins in different bee products due to its simplicity and reliability.

Key words: bee products; cephalosporins; ultra-high performance liquid chromatography-tandem mass spectrometry; Oasis PRIME HLB cartridge

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