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HPLC法测定福多司坦原料药及其制剂中有关物质的含量
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| 篇名： | HPLC法测定福多司坦原料药及其制剂中有关物质的含量 |
| TITLE： | |
| 摘要： | 目的：建立福多司坦原料药及其制剂中有关物质含量测定的方法。方法：以国内8家企业生产的福多司坦原料药或制剂为样品。采用高效液相色谱（HPLC）法（外标法）测定杂质A、B、C的含量，色谱柱为MGⅡ C18，流动相为0.12％己烷磺酸钠溶液（pH 2.0），流速为1.0 mL/min，检测波长为210 nm，柱温为35 ℃，进样量为20 μL。采用HPLC法（加校正因子的主成分自身对照法）测定杂质E、F、G的含量，色谱柱为Altech Altima C18，流动相为0.05 mol/L磷酸盐缓冲液-乙腈-水（梯度洗脱），流速为0.5 mL/min，检测波长为200 nm，柱温为30 ℃，进样量为20 μL。结果：杂质A、B、C、E、F、G的检测质量浓度线性范围分别为0.446～22.291、0.202～20.158、0.101～12.082、0.111 0～11.100、0.210 4～10.520、0.221 6～11.080 μg/mL，检测限分别为5.57、1.01、1.99、2.22、4.21、4.43 ng，定量限分别为11.14、2.02、3.98、4.45、8.42、8.85 ng；杂质E、F、G的校正因子分别为0.91、1.42、1.73，相对保留时间分别为0.88、1.95、3.08；精密度（n＝6）、稳定性[杂质A（4 h，n＝3），其余各杂质（24 h，n＝7）]试验的RSD均小于2.0％，平均加样回收率分别为98.0％、97.3％、102.4％、99.4％、98.9％、96.4％，RSD分别为1.4％、1.5％、1.1％、0.9％、1.2％、0.5％（n＝9）；8家福多司坦原料药或制剂生产企业中杂质总含量均＜1.1％。结论：该方法灵敏度高、专属性好，可用于福多司坦原料药及其制剂中有关物质的定量研究。 |
| ABSTRACT： | OBJECTIVE： To establish the method for content determination of the related substance in fudosteine raw material and its preparations. METHODS： Fudosteine or its preparations produced by 8 domestic enterprises were taken as samples. HPLC method （external standard） was used to determine the contents of impurities A， B and C. The separation was performed on MGⅡ C18 column with mobile phase consisted of 0.12％ sodium hexane sulfonate solution （pH 2.0） at flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm， column temperature was 35 ℃ and sample size was 20 μL. The contents of impurities E， F， G were determined by HPLC method （principal component self-contrast method with correction factor）. The separation was performed on Altech Altima C18 column with mobile phase consisted of 0.05 mol/L phosphate buffer-acetonitrile- water （gradient elution） at the flow rate of 0.5 mL/min. The detection wavelength was set at 200 nm， and the column temperature was 30 ℃. The sample size was 20 μL. RESULTS： The linear ranges of impurity A， B， C， E， F and G were 0.446-22.291， 0.202-20.158， 0.101-12.082， 0.111 0-11.100， 0.210 4-10.520， 0.221 6-11.080 μg/mL， respectively. The limits of detection were 5.57， 1.01， 1.99， 2.22， 4.21， 4.43 ng， respectively. The limits of quantitation were 11.14， 2.02， 3.98， 4.45， 8.42， 8.85 ng， respectively. The relative correction factors of impurities E， F and G were 0.91， 1.42 and 1.73， respectively； their relative retention time were 0.88， 1.95 and 3.08. RSDs of precision （n＝6） and stability [impurity A （4 h，n＝3）， other impurities （24 h，n＝7）] tests were all lower than 2.0％. The average recoveries were 98.0％， 97.3％， 102.4％， 99.4％， 98.9％， 96.4％， respectively； RSDs were 1.4％， 1.5％， 1.1％， 0.9％， 1.2％， 0.5％ （n＝9）， respectively. Total contents of substances in fudosteine raw material or its preparation produced by 8 enterprises were all lower than 1.1％. CONCLUSIONS： Established method is sensitive and specific. The method can be used for the quantitative study on related substances in fudosteine raw material and its preparations． |
| 期刊： | 2019年第30卷第13期 |
| 作者： | 郭志渊，赵欣庆，朱恒怡，袁军 |
| AUTHORS： | GUO Zhiyuan，ZHAO Xinqing，ZHU Hengyi，YUAN Jun |
| 关键字： | 福多司坦；有关物质；高效液相色谱法；含量测定；原料药 |
| KEYWORDS： | Fudosteine； Related substances； HPLC； Content determination； Raw material |
| 阅读数： | 416 次 |
| 本月下载数： | 14 次 |
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