Tetracycline residues in royal jelly and honey by liquid chromatography tandem mass spectrometry: validation study according to Commission Decision 2002/657/EC.
A specific, sensitive and robust liquid chromatography tandem mass spectrometry method for determining oxytetracycline, tetracycline, chlortetracycline and doxycycline in royal jelly and honey samples is presented. Extraction of drug residues was performed by ammonium acetate buffer as extractant followed by a clean-up with metal chelate affinity chromatography and solid-phase extraction. Tetracycline analysis was performed using liquid chromatography-electrospray ionisation-tandem mass spectrometry. The presented method is the first validated for royal jelly and in accordance with the requirements set by Commission Decision 2002/657/EC. Recoveries of the methods, calculated spiking the samples at 5.0, 10.0, 20.0 and 30.0 μg kg(-1), were 79% to 90% for honey and 77% to 90% for royal jelly. The intra-day precision (RSD) ranged between 8.1% and 15.0% for honey and from 9.1% to 16.3% for royal jelly, while inter-day precision values were from 10.2% to 17.6% and from 10.6% to 18.4% respectively for honey and royal jelly. Linearity for the four analytes was calculated from 5.0 to 50.0 μg kg(-1). The decision limits (CCα) ranged from 6.2 to 6.4 μg kg(-1) and from 6.1 to 6.5 μg kg(-1) for honey and royal jelly, respectively. Detection capabilities values (CCβ) ranged between 7.2 and 7.7 μg kg(-1) and from 7.3 to 7.9 μg kg(-1) respectively for honey and royal jelly. The developed method is currently in use for confirmation of the official control analysis of honey and royal jelly samples.
Giannetti
L
L
Istituto Zooprofilattico Sperimentale Regioni Lazio e Toscana, Via Appia Nuova, 1411-00178, Rome, Italy. luigi.giannetti@izslt.it
Longo
F
F
Buiarelli
F
F
Russo
M V
MV
Neri
B
B
D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000302:isolation & purification; D002751:Chlortetracycline / Q000032:analysis / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods; D004318:Doxycycline / Q000032:analysis / Q000302:isolation & purification; D005227:Fatty Acids / Q000032:analysis*; D006722:Honey / Q000032:analysis*; D016014:Linear Models; D010118:Oxytetracycline / Q000032:analysis / Q000302:isolation & purification; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013752:Tetracycline / Q000032:analysis* / Q000302:isolation & purification; D000099219:Royal Jelly
D000900:Anti-Bacterial Agents; D002751:Chlortetracycline; D004318:Doxycycline; D005227:Fatty Acids; D010118:Oxytetracycline; D013752:Tetracycline; D000099219:Royal Jelly