| Title |
Determination of Veterinary Antibiotic Residues: IV. Comparable Analytical Methods with EPA Method 1694_A Review |
| Authors |
김찬식 ( Chansik Kim ) ; 류홍덕 ( Hong-duck Ryu ) ; 정유진 ( Eu Gene Chung ) ; 김용석 ( Yongseok Kim ) ; 류덕희 ( Doug Hee Rhew ) |
| DOI |
https://doi.org/10.15681/KSWE.2016.32.6.670 |
| Keywords |
Analytical methods; EPA method 1694; HPLC-MS/MS; Veterinary antibiotics |
| Abstract |
In this study, 16 antibiotics selected from top 30 veterinary antibiotics sold in South Korea, 2014 as well as among the pharmaceuticals in EPA method 1694. In order to determine trace levels of antibiotics in environmental samples including surface water, soils, animal producing foods, and manures, LC-MS/MS was heavily used. In the chromatography for the detection of the selected antibiotics, the C18 column was mostly used at the temperature of 30~40°C. Water and methanol/ acetonitrile were commonly chosen as a non-polar and a polar mobile phase, respectively. Gradient elution was applied to separate multi-class antibiotics. Volatile additives such as formic acid, acetic acid, and ammonium acetate were mixed with the mobile phase to improve the ionization efficiency of analytes and the sensitivity in MS detection. Electrospray ionization (ESI) was widely used in the LC-MS/MS and positive ionization was preferred to determine the selected antibiotics. Protonated [M+H]+ molecule was selected as a precursor ion and its two transitions were analyzed: one for quantitative determination and the other for confirmation. This study were reviewed linearity of the calibration curve, recovery, repeatability, method detection limits (MDLs) and method quantification limits (MQLs) for each target compound used to validate the developed analytical methods. |