Citation: ZHANG Hao, WU Yinliang, ZHANG Yiwen, XU Xiuqin, XU Feng. Determination of ten cephalosporins in bee products by solid phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(12): 1314-1320. doi: 10.3724/SP.J.1123.2019.07028 shu

Determination of ten cephalosporins in bee products by solid phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry

ZHANG Hao ^1, ,
WU Yinliang ¹ ,
ZHANG Yiwen ² ,
XU Xiuqin ¹ ,
XU Feng ¹

1.
Ningbo Academy of Agricultural Sciences, Laboratory of Quality and Safety Risk Assessment for Agricultural Products(Ningbo), Ministry of Agriculture and Rural Affairs, Ningbo 315040, China;
2.
Beijing Institute of Metrology, Beijing 100012, China

Received Date: 1 August 2019

Fund Project: Science and Technology Program of Ningbo (No. 2017C50014)

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous quantitative determination of ten cephalosporins in bee products, including honey, royal jelly, and lyophilized royal jelly powder, has been established. The samples were extracted with an acetonitrile-water (80:20, v/v) solution. After purification by solid phase extraction using an Oasis PRIME HLB cartridge, the extract was blown to dryness under a stream of nitrogen gas and then re-dissolved in 1 mL 0.1% (v/v) formic acid solution and methanol (95:5, v/v). The samples were separated on an Acquity UPLC BEH C18 column, using a mixture of 0.1% (v/v) formic acid solution and methanol as the mobile phase under 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 to quantitative analysis. Good linear relationships were obtained for the ten cephalosporins in certain concentration ranges, and the correlation coefficients were more than 0.999. The limits of detection and limits of quantification for the ten cephalosporins were in the ranges 0.15-1.5 μg/kg and 0.5-5 μg/kg, respectively. The recoveries for the analytes in the bee products were in the range of 75.0%to 89.8%, with relative standard deviations of 1.4% to 4.6%. This method is characterized by a short analysis time and is suitable for the determination of cephalosporins in different bee products by virtue of its simplicity and reliability.
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