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

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 Na EDTA solutions along with an Oasis HLB cartridge. The target antibiotics were well separated in a Kinetex EVO C 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 (R ) 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 Na 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.

Residue analysis of tebufenozide and indoxacarb in chicken muscle, milk, egg and aquatic animal products using liquid chromatography–tandem mass spectrometry

“…The sensitivities of three other analytical columns (Phenomenex Kinetex ® EVO C 18 , Luna ® C 18 and Gemini ® ‐NX C 18 ) were compared. The Gemini‐NX C18 column produced superior results with sharp peaks and showed better chromatographic separation than the other columns (Zheng, Park, Abd El‐Aty et al, ).…”

Determination of Six Macrolide Antibiotics in Chicken Sample by Liquid Chromatography-Tandem Mass Spectrometry Based on Solid Phase Extraction

“…In comparison with various methods (Table 7), the first four ways of sample preparation were simple and fast, which used liquid extraction and a dilution step prior to direct injection into the instrument, but there was a high risk of mass spectrometry source contamination due to injecting “dirty” extracts. Compared with the last three approaches using magnetic molecularly imprinted polymers or commercial SPE cartridges (Oasis HLB cartridge and Bond-Elut C18 SPE cartridge) [5, 24, 50], the developed method in this work exhibited lower LODs and higher recoveries.…”

Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

“…Moreover, as the duck meat matrix has a fat content, n ‐hexane was employed to extract the fatty acids (Zheng et al, ). In addition, previous studies (Hamscher, Sczesny, Höper, & Nau, ; Yang, Cha, & Carlson, ; Zheng, Park, Abd El‐Aty, Kim, Cho, Choi, et al, ) reported that the addition of Na 2 EDTA is necessary to prevent complexation of the tetracyclines and macrolides with metal ions, which could lead to low recoveries; therefore, SPE methods with and without Na 2 EDTA were assayed for comparison. As shown in Figure , low recoveries of 32–38 and 35–47% were achieved for tetracyclines and macrolides, respectively, by the SPE method without Na 2 EDTA (concentration: 50 μg/kg, n = 3).…”