Determination of Chloramphenicol Residue in Animal Medicinal Herbs by UPLC-MS / 中国药房

ABSTRACT

OBJECTIVE:To establish the method for determination of chloramphenicol residue in animal medicinal herbs.METHODS:UPLC-MS method was adopted.The determination was performed on SB-C18 column with mobile phase consisted of acetonitrile-water (gradient elution) at the flow rate of 0.2 mL/min.The column temperature was 35 ℃,and sample size was 20 μL.The ion source was a jet stream ion focusing electrospray ion source.The temperature and flow of drying gas were 350 ℃ and 5 L/ min,and those of sheath gas were 250 ℃,11 L/min,and capillary voltage was 3 500 V.Negative ion scanning mode was conducted with multiple reaction monitoring (MRM) mode.RESULTS:The linear ranges of thiamphenicol,florfenicol and chloramphenicol were 0.5-15 ng/mL(r were 0.999 8,0.999 9,0.998 9,respectively).The limits of quantitation were 0.03,0.03,0.15 μg/kg,and the limits of detection were 0.01,0.01,0.05 μg/kg.RSDs of precision,stability and reproducibility tests were all lower than 3.0％.The recoveries were 84.00％-112.80％ (RSD=10.15％,n=9),88.24％-109.80％ (RSD=7.11％,n=9),88.24％-99.02％ (RSD=3.91％,n=9). CONCLUSIONS:The method is simple,precise,stable and reproducible,and can be used for determination of chloramphenicol in animal medicinal herbs.