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

作者：Zheng, Weijia; Park, Jin-A; Abd El-Aty, A. M.^*; Kim, Seong-Kwan; Cho, Sang-Hyun; Choi, Jeong-Min; Warda, Mohamad; Wang, Jing; Shim, Jae-Han; Shin, Ho-Chul^*

来源：Biomedical Chromatography, 2018, 32(4): e4145.

DOI：10.1002/bmc.4145

• antibiotics
• lincomycin
• royal jelly
• solid-phase extraction
• tandem mass spectrometry
• tylosin A and B

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 0.1m Na(2)EDTA solutions along with an Oasis HLB cartridge. The target antibiotics were well separated in a Kinetex EVO C-18 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 (5-50g/kg) in matrix-matched standard calibration. The coefficients of determination (R-2) 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 20g/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 0.1m Na(2)EDTA 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.

• 出版日期2018-4
• 单位中国农业科学院农业质量标准与检测技术研究所