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目的:建立离子色谱法测定注射用氯唑西林钠中醋酸根离子的含量。方法:采用TSKgel Super IC-AP阴离子柱(4.6 mm×150 mm,6μm),流动相为6.3 mmol·L~(-1)碳酸氢钠与1.1 mmol·L~(-1)碳酸钠的混合溶液,流速为0.8 m L·min~(-1),柱温为35℃,进样体积为10μL,抑制型电导检测。结果:氟离子等常见无机离子、甲酸根离子以及强破坏(高温破坏、光照破坏、酸破坏、碱破坏及氧化破坏)降解产物均不干扰醋酸根离子的测定。醋酸根离子在0.990 0~99.00μg·m L~(-1)范围内峰面积与质量浓度线性关系良好(r=0.999 9);平均加样回收率(n=9)为99.5%,RSD为0.3%;方法最低定量限为0.002 5%。有6个厂家的22批样品采用醋酸钠作为成盐剂,相应样品中残留的醋酸根离子含量在0.07%~0.83%之间。结论:建立的离子色谱法可用于注射用氯唑西林钠中醋酸根离子的含量测定。
Objective: To establish a method for the determination of acetate ion in cloxacillin sodium for injection by ion chromatography. Methods: TSKgel Super IC-AP column (4.6 mm × 150 mm, 6 μm) was used. The mobile phase consisted of a mixed solution of 6.3 mmol·L -1 sodium bicarbonate and 1.1 mmol·L -1 sodium carbonate , The flow rate was 0.8 m L · min -1, the column temperature was 35 ℃, the injection volume was 10μL, and the inhibitory conductivity was detected. Results: The common inorganic ions such as fluoride ion, formate ion and degradation products of strong damage (high temperature damage, light damage, acid damage, alkali damage and oxidation damage) did not interfere with the determination of acetate ion. The linear relationship between the peak area and the mass concentration of acetate ion in the range of 0.990 0 ~ 99.00 μg · m L -1 was good (r = 0.999 9). The average recovery (n = 9) was 99.5% 0.3%; the lowest limit of quantification was 0.002 5%. 22 batches of samples from 6 factories used sodium acetate as salt-forming agent, and the residual acetate ion content in the corresponding samples was between 0.07% and 0.83%. Conclusion: The established ion chromatography can be used to determine the content of acetate ion in cloxacillin sodium for injection.