提出了制备头孢类抗生素的中间体α-(2-氨基噻唑-4-基)-α-[(叔-丁氧基羰基)异丙氧亚胺基]-乙酸(ATIA)的反相高效液相色谱测定方法,采用SpherigelTM C18色谱柱(250 mm×4.6 mm,5 μm),以0.05 g·L-1四丁基溴化铵的甲醇-水(6+4)溶液为流动相,流速为1 mL·min-1,柱温30 ℃,检测波长260 nm,以外标法定量.在0.001~1.0 mg范围内,ATIA的质量与峰面积呈线性关系,回归方程为A=31 475.6 m+1 786.7,相关系数为0.999 7,以质量为0.06 mg ATIA按方法测定6次,算得其相对标准偏差为3.7%,检出限(3S)为0.6 μg,回收率的试验结果在98.8%~104.0%之间.

An intermediate product used for the preparation of cephalosporin antibiotics,α-(2-aminothiazol-4-yl)-α-[(tert.-butoxy-carbonyl)-iso-propoxyimino]-acetic acid (ATIA) was determined by RP-HPLC.SpherigelTM C18 (250 mm×4.6 mm,5 μm) column was used as the stationary phase,and 0.05 g·L-1 tetrabutylammonium bromide solution disolved in CH3OH-H2O (6+4) was used as the mobile phase,with a flow-rate of 1 mL·min-1 and at column temperature of 30 ℃.UV-detection at 260 nm and the external standard method were used in the determination.Linear relationship between the peak area and mass of ATIA was found in the range of 0.001-1.0 mg corresponding to the regression equation A=31 475.6 m+1 786.7 (r=0.999 7).Precision was tested at 0.06 mg of ATIA for 6 determinations,and value of RSD obtained was 3.7%.Detection limit (3S) was found to be 0.6 μg according to the definition of IUPAC.Recovery was tested by standard addition method,and values found were in the range of 98.8%-104.0%.