头孢克洛分散片中聚合物测定

Determination of the Polymer in Cefaclor

关键词:  头孢克洛分散片  聚合物  分子排阻色谱法

Key words:  cefaclor dispersible tablets  polymer  HPSEC

摘要:

目的 建立2种头孢克洛聚合物有效的测定方法并对结果进行比较。方法 方法1：采用TSKgel G2000SWxl色谱柱（7.8 mm×300 mm，5 μm），流动相为0.01 mol·L^-1磷酸盐缓冲液[0.01 mol·L^-1 NaH₂PO₄溶液-0.01 mol·L^-1 Na₂HPO₄溶液（50︰50），调节pH值为7.0]-乙腈（95︰5），流速为0.5 mL·min^-1柱温35℃，检测波长为254 nm，进样量20 μL；方法2：采用Sephadex G-10色谱柱（10 mm×300 mm，40~120 μm），以0.05 mol·L^-1磷酸盐缓冲液[取0.05 mol·L^-1 Na₂HPO₄溶液-0.05 mol·L^-1 NaH₂PO₄溶液（50︰50），调节pH至7.0]为流动相A，水为流动相B，流速为1 mL·min^-1，柱温35℃，检测波长为254 nm，进样量100 μL。结果 方法1：头孢克洛主峰与聚合物峰分离度>1.5，头孢克洛质量浓度在0.25~20 μg·mL^-1内线性关系良好（r=0.999 9）；定量限0.21 μg，检测限0.07 μg。重复性较好（RSD为1.8%，n=6）；在拟定的色谱条件下，通过考察破坏坏性实验（高温、强酸、强碱、氧化、光照）能够满足分离度要求，辅料无干扰；方法2：质量浓度在2.5~20 μg·mL^-1线性关系良好（r=0.999 7）；检测限0.13 μg，定量限0.40 μg。重复性良好（RSD为1.8%，n=6）。结论 新建立的2种方法对于头孢克洛分散片聚合物的分离度好，分离效率高，重复性好，均可以作为头孢克洛分散片的质量控制的依据。

Abstract:

OBJECTIVE To establish two efficient method to determine the polymers in cefaclor dispersible tablets and compare the results of two methods. METHODS Method 1:TSK-GEL G2000_SWXL column (7.8 mm×300 mm, 5 μm) was used. Mobile phase was 0.01 mol·L^-1 phosphate buffer solution[0.01 mol·mL^-1 disodium hydrogen phosphate-0.01 mol·mL^-1 sodium dihydrogen phosphate (50︰50), pH=7.0]-acetonitrile (95︰5), and the flow rate was 0.5 mL·min^-1, the temperature of column was kept at 35℃, the detection wavelength was at 254 nm, the injection volume was 20 μL. Method 2:Sephadex G-10 column (10.0 mm×300 mm, 40-120 μm) was used. Mobile phase A was 0.05 mol·L^-1 phosphate solution[0.05 mol·mL^-1 disodium hydrogen phosphate and 0.05 mol·mL^-1 sodium dihydrogen phosphate (50︰50), pH=7.0], mobile phase B was water and the flow rate was 1 mL·min^-1, the temperature of column was kept at 35,℃ the detection wavelength was at 254 nm, the injection volume was 100 μL. RESULTS Method 1:the resolution between main peak of cefaclor and polymer impurity peak was >1.5; the linear range of cefaclor was 0.25-20 μg·mL^-1 (r=0.999 9). The LOD and LOQ of were found to be 0.07 μg and 0.21 μg; the repeatability RSD (n=6) was 1.8%. Method 2:the linear of cefotaxime was 2.5-20 μg·mL^-1 (r=0.999); the LOD and LOQ of were found to be 0.13 μg and 0.40 μg; the repeatability RSD (n=6) was 1.8%. CONCLUSION The two method can be used in determination of the polymer in cefaclor. The two improved methods show higher sensitivity, better separation ability, simple application and good reproducibility for cefaclor dispersible tablets. They can be used as the quality control of cefaclor dispersible tablets foundation.