摘要
建立了硝酸钾.硫氰酸铵.水体系萃取浮选铜间接测定头孢拉定的新方法。结果表明,在SCN^-、KNO,存在下及控制溶液pH值为4.0~6.0,头孢拉定完全降解为巯基(-SH)化合物,且巯基(-SH)能使Cu(Ⅱ)还原为Cu(Ⅰ),所生成的Cu(Ⅰ)与SCN^-形成CuSCN白色乳状沉淀而浮选至水相表面,根据溶液中剩余Cu(Ⅱ)的量可间接测定头孢拉定的含量。CuSCN的浮选率E(%)与头孢拉定的含量之间存在良好的线性关系。当Cu(Ⅱ)加入量为50μg时,线性范围为0.3~12.0mg/L。检出限为0.25mg/L。方法用于胶囊、血清、尿样中头孢拉定含量的测定,结果令人满意。
A novel method for indirect determination of cefradine by extraction flotation of CuCSN with potassium nitrate-ammonium thiocyanate-woter system was developed. At pH 4. 0 to 6. 0, in the existence of SCN^-, the thiol group(-SH) of the degradation product of cefradine could reduce Cu( Ⅱ ) to Cu( Ⅰ ), and the resulting Cu( Ⅰ ) could react with SCN^- to form white emulsion precipitate CuSCN. In the presence of KNO3 , this precipitate ascended and floated on the surface of water. The amount of cefradine can be determined by, measuring the flotation yield of Cu( Ⅱ ). When the amount of added Cu( Ⅱ ) is 50 μg, the linear range is maintained in the range 0. 3 - 12.0 mg/L with a correlation coefficient of 0. 999 2. The detection limit is 0. 25 mg/L. This proposed method was successfully applied to the determination of cefradine in capsules and the recovery of cefradine in urine and human plasma with satisfactory results.
出处
《应用化学》
CAS
CSCD
北大核心
2008年第9期1095-1100,共6页
Chinese Journal of Applied Chemistry
关键词
头孢拉定
硝酸钾
硫氰酸铵
铜
萃取浮选
cefradine, potassium nitrate, ammonium thiocyanate, copper( 11 ), extraction and flotation