Chinese Journal of Chromatography

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Determination of Five Macrolide Antibiotic Residues in Royal Jelly Samples by Using High Performance
Liquid Chromatography Tandem Mass Spectrometry

XIE Wen1, DING Huiying1, XI Junyang2, QIAN Yan2, HUANG Leifang2   

  1. 1.Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310012, China; 2.Zhejiang Lead Product Technic CO., Ltd., Hangzhou 310012, China
  • Received:2006-09-12 Revised:2007-01-30 Online:2007-05-30 Published:1985-09-25

Abstract:

The macrolides are lipophilic molecules having a central lactone ring bearing 12 to 20 atoms to which several amino and/or neutral sugars are bound. They are broad spectrum antibiotics active against Gram-positive bacteria and mycoplasmas, as well as some Gram-negative organisms and members of the chlamydia group. Macrolides are a group of antibacterial compounds that have been widely used in medical and veterinary practices. A method of high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was developed for the confirmation of five macrolide antibiotic residues (spiramycin, oleandomycin, tylosin, roxithromycin, josamycin) in royal jelly samples. Trichloroacetic acid solution was used to precipitate the protein in the sample. The upper layer solution was extracted with acetonitrile. Then it was cleaned up with a C18 column. The one precursor/two product ion transitions for each macrolide antibiotics were monitored. The results show that the working curves for five macrolide antibiotics were linear in the range of 0.002-0.05 mg/L by HPLC-MS/MS in selective ion monitoring model. The limits of quantitation of the antibiotics in royal jelly were all 20 μg/kg. The recoveries were between 73.0%-90.2% at three spiked levels (20, 100 and 200 μg/kg for each macrolide antibiotic), and the relative standard deviations were between 5.6%-10.5%.

Key words: macrolide antibiotic residues, royal jelly , high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS)