摘要
目的：建立反相高效液相色谱法测定头孢美唑钠中的有关物质。方法：采用Diamonsil-C18色谱柱（250 mm×4.6 mm,5μm）,以0.08 mol.L-1醋酸铵溶液-甲醇（85∶15）（混合后,冰醋酸调pH至6.0）为流动相,流速为1 mL.min-1,检测波长为214 nm,柱温为30℃;以主要杂质TMT为对照,量化样品中的相应杂质,以头孢美唑钠为对照,量化其他杂质。结果：头孢美唑钠与各有关物质分离良好;TMT和头孢美唑钠分别在0.01024~102.40μg.mL-1和0.02μg.mL-1~1.00 mg.mL-1浓度范围内,峰面积与浓度呈良好的线性关系,相关系数均为0.999 9,TMT和头孢美唑钠的检测限分别为0.05 ng和0.2 ng,TMT的平均回收率为100.21%,中间精密度为3.66%（n=6）。结论：本法简便、专属,灵敏,可用于头孢美唑钠有关物质的测定。
Objective：To establish a RP-HPLC method for the determination of related substances in cefmetazole.Methods：The HPLC conditions were as follows：Diamonsil-C18 column（250 mm×4.6 mm,5 μm） with a temperature at 30 ℃;mobile phase of 85 volumes of 0.08 mol·L-1 ammonium acetate and 15 volumes of methanol,pH=6.0（adjusted with acetic acid after mixture）;a flow rate of 1 mL·min-1;detection at 214 nm.The main impurity was quantified with TMT as the reference substance,and other impurities were quantified with cefmetazole as the principal component.Results：Cefmetazole was completely separated from related substances.The calibration curve of cefmetazole was linear within 0.02 μg·mL-1~1.0 mg·mL-1 with a correlation coefficient of 0.999 9.The calibration curve of impurity 1（TMT） was linear within 0.010 24~102.4 μg·mL-1 with a correlation coefficient of 0.999 9.The limits of detection were 0.05 ng for TMT and 0.2 ng for cefmetazole.The average recovery of TMT was 100.21%,and the RSD of precision was 3.66%（n=6）.Conclusion：This RP-HPLC method is simple,selective and sensitive,and can be used for determination of related substances in cefmetazole.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2011年第9期828-832,共5页
Chinese Journal of New Drugs
