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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 an RP-HPLC method for the determination of related substances in cefmetazole sodium. METHODS: Diamonsil-C18 column (250 mm × 4.6 mm, 5 μm) was used as mobile phase with 0.08 mol·L-1 ammonium acetate solution (85:15) The flow rate was 1 mL.min-1, the detection wavelength was 214 nm, and the column temperature was 30 ℃. The main impurity TMT was used as a control to quantify the corresponding impurities in the sample. Cefmetazole sodium was used as a control to quantify other impurities. Results: Cefmetazole sodium was well separated from other related substances. The concentrations of TMT and Cefmetazole in the range of 0.01024 ~ 102.40μg.mL-1 and 0.02μg.mL-1 ~ 1.00 mg.mL-1, respectively, The correlation coefficient was 0.999 9. The detection limits of TMT and Cefmetazole sodium were 0.05 ng and 0.2 ng respectively. The average recoveries of TMT were 100.21% and the intermediate precision was 3.66% (n = 6 ). Conclusion: This method is simple, specific and sensitive and can be used to determine cefmetazole related substances.