| 赵敬丹,张含智,闻宏亮,秦 峰,刘 浩.HPLC-加校正因子的主成分自身对照法测定注射用头孢孟多酯钠的有关物质[J].中国药品标准,2018,19(5):382-387 |
| HPLC-加校正因子的主成分自身对照法测定注射用头孢孟多酯钠的有关物质 |
| Determination of Related Substances in Cefamandole Nafate for Injectionby HPLC with correction factor |
| 投稿时间：2018-06-19 修订日期：2018-09-25 |
| DOI： |
| 中文关键词: 校正因子 注射用头孢孟多酯钠 杂质D 有关物质 |
| 英文关键词: correction factor cefamandole nafate for injection impurity D related substance |
| 基金项目: |
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| 中文摘要: |
| 目的：采用自建的方法测定注射用头孢孟多酯钠中杂质A、杂质C、杂质D和杂质E相对于头孢孟多酯的校正因子，以确定最佳的定量方式，提高有关物质测定结果的准确度。方法：用十八烷基硅烷键合硅胶为填充剂，以0.05 mol·L-1甲酸铵溶液（用甲酸调至pH值至4.5）为流动相A，乙腈为流动相B，线性梯度洗脱，柱温30℃，检测波长254 nm。分别采用不同品牌的高效液相色谱仪及不同规格和来源的色谱柱对杂质A、杂质C、杂质D和杂质E的校正因子进行测定，并将测定结果和主成分自身对照法及外标法进行对比。结果：各色谱系统中主成分头孢孟多酯与相邻杂质及各已知杂质之间分离均良好，头孢孟多酯、杂质A、杂质C、杂质D和杂质E在0.05~2.5μg·mL-1浓度范围内线性关系均良好（r>0.999），杂质A、杂质C、杂质D和杂质E的校正因子分别为1.10，1.12，0.59和1.17，杂质D和杂质E的定量方式以加校正因子的主成分自身对照法为宜。6批样品杂质A结果均约为0.2%，杂质C均约为0.1%，杂质D均约为0.02%，杂质E分别为0.06%、0.04%、0.05%、0.05%、0.08%和0.08%，其它单个最大杂质均约为0.1%，校正后总杂质分别为0.9%、0.8%、0.9%、0.8%、0.8%和0.8%。结论：通过对各已知杂质校正因子的测定，无需持续提供杂质对照品，即可准确测定注射用头孢孟多酯钠的有关物质，本方法操作简单，结果准确可靠，可为含类似结构的抗生素类药物定量方法的改进提供参考。 |
| 英文摘要: |
| Objective: To improve the accuracy of quantitative results by measuring the relative correction factors of the related substances in cefamandole nafate for injection with established method. Method: The determination was carried out on a C18 column and ammonium formate solution (pH 4.5) as mobile phase A, acetonitrile as mobile phase B, with gradient elution; the column temperature was 30℃, the detection wavelength was 254 nm. Four HPLC systems and several columns with different length or particle diameter were used to determine the correlation factors of impurity A, impurity C, impurity D and impurity E. And the results were compared. Results: The resolutions between cefamandole nafate and the adjacent peaks as well as the known impurities all met the requirement. The calibration curves were linear in the range of 0.05-2.5μg·mL-1 (r>0.999).The correction factors of impurity A，C，D and E were 1.10，1.12，0.59 and 1.17. The quantitative results of impurity D and E were suggested to use corrected peak areas. The results of impurity A were all about 0.2%，impurity C were all about 0.1%，impurity D were all about 0.02%，impurity E were 0.06%、0.04%、0.05%、0.05%、0.08% and 0.08% respectively，the maximum unknown impurity were all about 0.1%，corrected total impurities were 0.9%、0.8%、0.9%、0.8%、0.8% and 0.8% respectively。Conclusion: The method was proved to be simple, accurate and reliable to determine the related substances of cefamandole nafate for injection without standard substances of impurity D and E. and it could be an example to improve the quantitative method of antibiotics with similar structures. |
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