Lopez Mayda I, Pettis Jeffery S, Smith I Barton, Chu Pak-Sin
Center for Veterinary Medicine, U.S. Food and Drug Administration, 8401 Muirkirk Road, Laurel, Maryland 20708, USA.
J Agric Food Chem. 2008 Mar 12;56(5):1553-9. doi: 10.1021/jf073236w. Epub 2008 Feb 8.
A multiclass method has been developed for the determination and confirmation in honey of tetracyclines (chlortetracycline, doxycycline, oxytetracycline, and tetracycline), fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, and sarafloxacin), macrolides (tylosin), lincosamides (lincomycin), aminoglycosides (streptomycin), sulfonamides (sulfathiazole), phenicols (chloramphenicol), and fumagillin residues using liquid chromatography tandem mass spectrometry (LC-MS/MS). Erythromycin (a macrolide) and monensin (an ionophore) can be detected and confirmed but not quantitated. Honey samples (approximately 2 g) are dissolved in 10 mL of water and centrifuged. An aliquot of the supernatant is used to determine streptomycin. The remaining supernatant is filtered through a fine-mesh nylon fabric and cleaned up by solid phase extraction. After solvent evaporation and sample reconstitution, 15 antibiotics are assayed by LC-MS/MS using electrospray ionization (ESI) in positive ion mode. Afterward, chloramphenicol is assayed using ESI in negative ion mode. The method has been validated at the low part per billion levels for most of the drugs with accuracies between 65 and 104% and coefficients of variation less than 17%. The evaluation of matrix effects caused by honey of different floral origin is presented.
已开发出一种多类方法，用于通过液相色谱串联质谱法（LC-MS/MS）测定和确证蜂蜜中的四环素类（金霉素、强力霉素、土霉素和四环素）、氟喹诺酮类（环丙沙星、达氟沙星、二氟沙星、恩诺沙星和沙拉沙星）、大环内酯类（泰乐菌素）、林可酰胺类（林可霉素）、氨基糖苷类（链霉素）、磺胺类（磺胺噻唑）、氯霉素类（氯霉素）和腐马霉素残留。红霉素（一种大环内酯类）和莫能菌素（一种离子载体）可以被检测和确证，但无法定量。将蜂蜜样品（约2 g）溶解于10 mL水中并离心。取上清液的一份用于测定链霉素。其余上清液通过细网尼龙布过滤，并用固相萃取进行净化。在溶剂蒸发和样品复溶后，使用电喷雾电离（ESI）在正离子模式下通过LC-MS/MS对15种抗生素进行测定。之后，使用ESI在负离子模式下测定氯霉素。该方法已在十亿分率的低水平对大多数药物进行了验证，准确度在65%至104%之间，变异系数小于17%。文中还介绍了对不同花源蜂蜜引起的基质效应的评估。
