The Analytical Study On Chloramphenicol Residues In Honeyed Pill Liuwei Dihuang Wan

1. Rapid Determination of Chloramphenicol Residues in Honeyed Pill Liuwei Dihuang Wan by GICA.Chloramphenicol (CAP) is a widely used antibiotic, but it has serious side effects. European and American developed countries has successively prohibited and strictly banned its use. This paper established a rapid method for determining the content of Chloramphenicol residues in honeyed pill Liuwei Dihuang Wan by applying GICA technology. And it provides an effective means to the rapid detection and monitoring of chloramphenicol, thus to protect the safety of the masses on drug use.2. HPLC Determination of Chloramphenicol Residues in Honeyed Pill Liuwei Dihuang WanObjective: To establish a method to determine chloramphenicol residues in Liuwei Dihuang Wan. Methods: Liuwei Dihuang Wan samples were cleaned by chloramphenicol molecularly imprinted polymer (MIP) microspheres solid phase extraction cartridges and determined with high performance liquid chromatography. The chromatographic conditions included Hypersil BDS column (250×4.6mm,5um); the mobile phase was water-methanol with gradient elution; the flow rate was 1ml﹒min^-1; the detective wavelength was at 278nm; column temperature was 45℃; the injection volume was 20uL; the signal acquisition time was 60min. Results: There were good linear realationship of CAP in a concentration range of 0.02-2.0ug?mL^-1, r=0.9999. The recovery rates were 79.69﹪-95.40﹪; the relative standard deviation (RSD) ranged from 2.31﹪-7.15﹪; the limit of detection was up to 10.08ug﹒kg^-1.Conclusion: The method is stable, accurate, sensitive and can be used for the quality control of Liuwei Dihuang Wan.3. GC Determination of Chloramphenicol Residues in Honeyed Pill Liuwei Dihuang Wan[Objective] To establish a GC method for the determination of Chloramphenicol(CAP) in Liuwei Dihuang Wan.[Method] CAP in Liuwei Dihuang Wan was extracted by ethyl acetate and dissolved in phosphate buffer after centrifugation and evaporation. The fat was removed by n-hexane and Liuweidihuangwan purified by CAP MISPE column. CAP was eluted by dichloromethane,dried and Silylated by BSTFA-TMCS for 30 minutes at 70℃, then dried by nitrogen gas and determined in n-hexane solution by GC-ECD.[Result] The results showed that in the linear range of 1.0-100.0ng/mL,the correlation coefFicient r=0.9999.The recoverry was between 92.57-99.53%, while the coefficient of variation between 0.68-5.13%。. The low detection limit was 0.504 ug·kg-1[Conclusion] The result revealed that this method is reliable, sensitive and can be used for the determination of Chloramphenicol in Liuwei Dihuang Wan.