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目的:建立测定丙二醇头孢曲嗪原料药中聚合物含量的方法。方法:采用高效分子排阻色谱法。色谱柱为Sephadex G-10,流动相A为0.01 mol/L磷酸盐缓冲液[0.01 mol/L磷酸氢二钠溶液-0.01 mol/L磷酸二氢钠溶液(61 ∶ 39,V/V)](pH7.0),流动相B为水,流速为1.0 ml/min,检测波长为254 nm,柱温为30 ℃,进样量为200 μl。结果:丙二醇头孢曲嗪原料药中聚合物的检测质量浓度线性范围为2.07~103.30 μg/ml(r=0.999 4);定量限为10.4 ng、检测限为4.1 ng;精密度、重复性试验的RSD<3%。结论:该方法专属性强、灵敏度高、重复性好,可用于丙二醇头孢曲嗪原料药中聚合物的含量测定。
OBJECTIVE: To establish a method for the content determination of polymer in cefatrizine propylene glycol. METHODS: High performance sephadex gel chromatography was performed on the column of Sephadex G-10 with mobile phase A of 0.01 mol/L phosphate buffer [0.01 mol/L Disodium hydrogen phosphate solution-0.01 mol/L Sodium dihydrogen phosphate solution(61 ∶ 39,V/V)](pH7.0) and mobile phase B of water at a flow rate of 1.0 ml/min, the detection wavelength was 254 nm, column temperature was 30 ℃, and volume injection was 200 μl. RESULTS: The linear range of polymer was 2.07-103.30 mg/ml(r=0.999 4); the limit of quantitation of 10.4 ng, limit of detection was 4.1 ng; RSDs of precision and reprodicibility tests were lower than 3%. CONCLUSIONS: The method is specific with high sensitivity and good reproducibility, and can be used for the content determination of polymer in active pharmacentical ingredient cefatrizine propylene glycol.
丙二醇头孢曲嗪聚合物高效分子排阻色谱法
Cefatrizine propylene glycolPolymerHigh performance size exclusion chromatography
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