Development and validation of a liquid chromatographic/ tandem mass spectrometric method for determination of chlortetracycline, oxytetracycline, tetracycline, and doxycycline in animal feeds. 2012

Liang Guo, and Yiqiang Chen, and Liying Zhang, and Wenjun Yang, and Pingli He
China Agricultural University, State Key Laboratory on Animal Nutrition, Beijing 100193, People's Republic of China.

A selective and accurate LC/MS/MS method for the simultaneous determination of chlortetracycline (CTC), oxytetracycline (OTC), tetracycline (TC), and doxycycline (DC) in animal feeds was developed. Samples were extracted with Na2EDTA-McIlvaine buffer and further purified with Oasis HLB SPE columns. The purified extract was separated on an Xbridge C18 column and detected by LC/MS/MS with positive electrospray ionization in the multiple reaction monitoring mode. This method provided average recoveries of 80.9 to 119.5%, with CVs of 1.7 to 9.8% in the range of 0.5 to 50 mg/kg CTC, OTC, TC, and DC in feeds, except the average recovery of CTC was 76.0%, with a CV of 14.6% in pig feed spiked with 0.5 mg/kg CTC. The linear ranges for the four TCs determined by LC/MS/MS ranged from 0.005 to 2.5 microg/mL with a linear correlation coefficient (R2) >0.99. The LOD and LOQ for CTC, OTC, TC, and DC in pig and poultry feeds ranged from 0.003 to 0.02 and 0.01 to 0.05 microg/g, respectively. The method was successfully applied for the analysis of 30 real feed samples, and no illegal use was detected.

UI MeSH Term Description Entries
D007477 Ions An atom or group of atoms that have a positive or negative electric charge due to a gain (negative charge) or loss (positive charge) of one or more electrons. Atoms with a positive charge are known as CATIONS; those with a negative charge are ANIONS.
D008956 Models, Chemical Theoretical representations that simulate the behavior or activity of chemical processes or phenomena; includes the use of mathematical equations, computers, and other electronic equipment. Chemical Models,Chemical Model,Model, Chemical
D010118 Oxytetracycline A TETRACYCLINE analog isolated from the actinomycete STREPTOMYCES RIMOSUS and used in a wide variety of clinical conditions. Hydroxytetracycline,Bisolvomycin,Geomycin,Oxyterracin,Oxyterracine,Oxytetracid,Oxytetracycline Anhydrous,Oxytetracycline Calcium,Oxytetracycline Dihydrate,Oxytetracycline Hydrochloride,Oxytetracycline Monohydrochloride,Oxytetracycline Sulfate (2:1),Oxytetracycline, (4a beta,5 beta,5a beta,12a beta)-Isomer,Oxytetracycline, (5 beta)-Isomer,Oxytetracycline, Anhydrous,Oxytetracycline, Calcium (1:1) Salt,Oxytetracycline, Disodium Salt, Dihydrate,Oxytetracycline, Sodium Salt,Terramycin
D011200 Poultry Domesticated birds raised for food. It typically includes CHICKENS; TURKEYS, DUCKS; GEESE; and others. Fowls, Domestic,Domestic Fowl,Domestic Fowls,Fowl, Domestic,Poultries
D012015 Reference Standards A basis of value established for the measure of quantity, weight, extent or quality, e.g. weight standards, standard solutions, methods, techniques, and procedures used in diagnosis and therapy. Standard Preparations,Standards, Reference,Preparations, Standard,Standardization,Standards,Preparation, Standard,Reference Standard,Standard Preparation,Standard, Reference
D002751 Chlortetracycline A TETRACYCLINE with a 7-chloro substitution. Aureocyclin,Aureomycin,Aureomycine,Biomycin,Chlorotetracycline,Chlortetracycline Bisulfate,Chlortetracycline Hydrochloride,Chlortetracycline Monohydrochloride,Chlortetracycline Sulfate (1:1),Chlortetracycline Sulfate (2:1),Chlortetracycline, 4-Epimer,Chlortetracycline, Calcium Salt,4-Epimer Chlortetracycline,Bisulfate, Chlortetracycline,Calcium Salt Chlortetracycline,Chlortetracycline, 4 Epimer,Hydrochloride, Chlortetracycline,Monohydrochloride, Chlortetracycline,Salt Chlortetracycline, Calcium
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D004318 Doxycycline A synthetic tetracycline derivative with similar antimicrobial activity. 2-Naphthacenecarboxamide, 4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-, (4S-(4alpha,4aalpha,5alpha,5aalpha,6alpha,12aalpha))-,Alpha-6-Deoxyoxytetracycline,Atridox,BMY-28689,BU-3839T,Doryx,Doxycycline Calcium,Doxycycline Calcium Salt (1:2),Doxycycline Hemiethanolate,Doxycycline Hyclate,Doxycycline Monohydrate,Doxycycline Monohydrochloride, 6-epimer,Doxycycline Monohydrochloride, Dihydrate,Doxycycline Phosphate (1:1),Doxycycline-Chinoin,Hydramycin,Oracea,Periostat,Vibra-Tabs,Vibramycin,Vibramycin Novum,Vibravenos,Alpha 6 Deoxyoxytetracycline,BMY 28689,BMY28689,BU 3839T,BU3839T,Doxycycline Chinoin,Doxycycline Monohydrochloride, 6 epimer,Vibra Tabs
D005504 Food Analysis Measurement and evaluation of the components of substances to be taken as FOOD. Analysis, Food,Analyses, Food,Food Analyses
D000818 Animals Unicellular or multicellular, heterotrophic organisms, that have sensation and the power of voluntary movement. Under the older five kingdom paradigm, Animalia was one of the kingdoms. Under the modern three domain model, Animalia represents one of the many groups in the domain EUKARYOTA. Animal,Metazoa,Animalia

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