Citation: LI Shuaipeng, GUO Chunna, MENG Lei, HUANG Xianhui. Determination of cefalonium residue in milk by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(5): 519-523. doi: 10.3724/SP.J.1123.2013.12028 shu

Determination of cefalonium residue in milk by high performance liquid chromatography-tandem mass spectrometry

1.
1. National Reference Laboratory of Veterinary Drug Residues, South China Agricultural University, Guangzhou 510642, China;

Corresponding author: HUANG Xianhui,
Received Date: 25 December 2013
Available Online: 27 February 2014
Fund Project: 公益性行业(农业)科研专项(201303038-5). (农业)科研专项(201303038-5)

An analytical method was developed for the determination of cefalonium in milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A total of 1 g milk was deproteinized by acetonitrile. The supernatant was transferred into a test tube to be blown dry with N₂ at 37 ℃. Then the residue was dissolved with methanol-0.1% formic acid in water (3:7, v/v). The sample was determined by HPLC-MS/MS after the purification. The chromatographic separation was achieved on a C₁₈ column using 0.1% formic acid in water and acetonitrile as mobile phases with gradient elution. Qualitative and quantitative analyses were achieved by HPLC-MS/MS under positive ionization and multiple reaction monitoring (MRM) mode. Matrix-matched calibration curve was used for the quantification. Good correlation coefficients were obtained (r>0.999) in the mass concentration range of 2-200 μg/L. The limit of detection (LOD, S/N≥3) was 0.5 μg/kg in milk, and the limit of quantification (LOQ, S/N≥10) was 2 μg/kg. The mean recoveries at the four levels of LOQ, 1/2MRL (maximum residue level), MRL, 2MRL were between 78.5% and 86.2%, with the intra-day relative standard deviations (RSDs)of 1.5% to 6.2% and inter-day RSDs of 2.9% to 5.6%. In conclusion, the established method can be applied for the determination of cefalonium residue in milk.
- high performance liquid chromatography (HPLC),
- tandem mass spectrometry (MS/MS),
- cefalonium,
- milk,
- residue
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