Development and validation of a simple solid‐phase extraction method coupled with liquid chromatography–triple quadrupole tandem mass spectrometry for simultaneous determination of lincomycin, tylosin A and tylosin B in royal jelly

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EarlyView Article

  • Published: Dec 11, 2017
  • Author: Weijia Zheng, Jin‐A Park, A. M. Abd El‐Aty, Seong‐Kwan Kim, Sang‐Hyun Cho, Jeong‐Min Choi, Mohamad Warda, Jing Wang, Jae‐Han Shim, Ho‐Chul Shin
  • Journal: Biomedical Chromatography

Abstract

We have developed an analytical method for the determination of lincomycin, tylosin A and tylosin B residues in royal jelly using liquid chromatography–triple quadrupole tandem mass spectrometry analysis. For extraction and purification, we employed 1% trifluoroacetic acid and 0.1 m Na2EDTA solutions along with an Oasis HLB cartridge. The target antibiotics were well separated in a Kinetex EVO C18 reversed‐phase analytical column using a combination of 0.1% formate acid in ultrapure water (A) and acetonitrile (B) as the mobile phase. Good linearity was achieved over the tested concentration range (5–50 μg/kg) in matrix‐matched standard calibration. The coefficients of determination (R2) were 0.9933, 0.9933 and 0.996, for tylosin A, tylosin B and lincomycin, respectively. Fortified royal jelly spiked with three different concentrations of the tested antibiotics (5, 10 and 20 μg/kg) yielded recoveries in the range 80.94–109.26% with relative standard deviations ≤4%. The proposed method was applied to monitor 11 brand of royal jelly collected from domestic markets and an imported brand from New Zealand; all the samples tested negative for lincomycin, tylosin A and tylosin B residues. In conclusion, 1% trifluoroacetic acid and 0.1 m Na2EDTA aqueous solvents combined with solid‐phase extraction could effectively complete the sample preparation process for royal jelly before analysis. The developed approach can be applied for a routine analysis of lincomycin, tylosin A and tylosin B residues in royal jelly.

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