反相高效液相色谱法测定α-(2-氨基噻唑-4-基)-α-[(叔-丁氧基羰基)异丙氧亚胺基]-乙酸  

RP-HPLC Determination of α-(2-Aminothiazol-4-yl)-α-[(Tert.-Butoxy-Carbonyl)-Iso-Propoxyimino]-Acetic Acid

作　　者：王倩倩[1] 朱智甲[1] 张海泉[1] 

机构地区：[1]东华大学化学化工学院,上海201620

出　　处：《理化检验（化学分册）》2008年第5期438-440,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：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Spherigel^TM C18色谱柱（250mm×4．6mm，5μm），以0．05g·L^-1四丁基溴化铵的甲醇-水（6＋4）溶液为流动相，流速为1mL·min^-1，柱温30℃，检测波长260nm，以外标法定量。在0．001～1．0mg范围内，ATIA的质量与峰面积呈线性关系，回归方程为A=31475．6m＋1786.7，相关系数为0．9997，以质量为0.06mg 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0．6μg，回收率的试验结果在98．8％～104．0％之间。An intermedlate 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×4.6mm,5μm）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%.

关 键 词：反相高效液相色谱法 α-(2-氨基噻唑-4-基)-α-[(叔-丁氧基羰基)异丙氧亚胺基]-乙酸 中间体化合物 

分 类 号：O657.7[理学—分析化学]