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HPLC-加校正因子的主成分自身对照法同时测定奥美沙坦酯氢氯噻嗪片中4种有关物质含量
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| 篇名： | HPLC-加校正因子的主成分自身对照法同时测定奥美沙坦酯氢氯噻嗪片中4种有关物质含量 |
| TITLE： | Simultaneous Determination of Four Related Substances in Olmesartan Medoxomil Hydrochlorothiazide Tablets by HPLC-Principal Component Self-Control with Correct Factor |
| 摘要： | 目的：建立同时测定奥美沙坦酯氢氯噻嗪片中4种已知有关物质（奥美沙坦、奥美沙坦酯二聚体、奥美沙坦酯烯、苯并噻二嗪杂质，简称杂质A、B、C、D）的方法。方法：采用高效液相色谱（HPLC）-加校正因子的主成分自身对照法进行测定。色谱柱为YMC-TriartC8；流动相A为乙腈-0.015mol/L磷酸二氢钾溶液（用磷酸调节pH至2.8）（70∶30，V/V），流动相B为乙腈-0.015mol/L磷酸二氢钾溶液（用磷酸调节pH至2.8）（15∶85，V/V），梯度洗脱；流速为0.8mL/min；检测波长为265nm；柱温为25℃；自动进样器温度为4℃；进样量为10μL。结果：杂质A、B、C、D的校正因子分别为1.42、1.17、0.89、0.92。奥美沙坦酯、氢氯噻嗪和杂质A、B、C、D的质量浓度线性范围分别为0.2527～7.5800、1.1521～4.5629、0.2440～18.2990、0.2447～3.6708、0.2652～3.9783、0.1499～4.4973μg/mL（r均不低于0.9997），检测限分别为0.0842、0.0507、0.0813、0.0816、0.0884、0.0500μg/mL，定量限分别为0.2527、0.1521、0.2440、0.2447、0.2652、0.1499μg/mL，中间精密度、稳定性（24h）、重复性试验结果均符合相关要求，平均回收率分别为104.00％～108.04％、102.00％～104.94％、100.99％～106.89％、92.00％～95.18％、102.00％～105.06％、103.90％～107.00％（n＝3）。3批奥美沙坦酯氢氯噻嗪片中杂质A的含量为0.90％～1.00％，杂质B的含量为0～0.11％，杂质D的含量为0.16％～0.24％，杂质C及其余杂质未检出；所建立方法测得结果与外标法测得结果无明显差异。结论：本方法灵敏度高、重复性好，可用于奥美沙坦酯氢氯噻嗪片中4种已知有关物质含量的同时测定。 |
| ABSTRACT： | OBJECTIVE： To establish the method for simultaneous determination of four known related substances （olmesartan，olmesartan ester dimer ，olmesartan ester alkene ，benzothiadiazine impurity ，called impurity A ，B，C，D for short ）in Olmesartan medoxomil hydrochlorothiazide tablets. METHODS ：HPLC-principal component self-control with correction factor were adopted. The determination was performed on YMC-Triart C 8 column with mobile phase A consisted of acetonitrile- 0.015 mol/L potassium dihydrogen phosphate solution （pH adjusted to 2.8 with phosphoric acid ）（70 ∶ 30，V/V），mobile phase B consisted of acetonitrile-0.015 mol/L potassium dihydrogen phosphate solution （pH adjusted to 2.8 with phosphoric acid ）（15 ∶ 85，V/V）at the flow rate of 0.8 mL/min（gradient elution ）. The detection wavelength was set at 265 nm，and column temperature was 25 ℃. The temperature of injector was 4 ℃；the injection volume was 10 μL. RESULTS：The correction factors of impurity A ，B，C，D were 1.42，1.17，0.89，0.92，respectively. The linear range of olmesartan medoxomil ，hydrochlorothiazide and impurity A ，B，C，D were 0.252 7-7.580 0，1.152 1-4.562 9，0.244 0-18.299 0，0.244 7-3.670 8，0.265 2-3.978 3 and 0.149 9-4.497 3 μg/mL（r≥ 0.999 7），respectively. The limits of detection were 0.084 2，0.050 7，0.081 3，0.081 6，0.088 4，0.050 0 μg/mL，respectively. The quantitative limits were 0.252 7，0.152 1，0.244 0，0.244 7，0.265 2 and 0.149 9 μg/mL，respectively. The results of intermediate precision ，stability（24 h）and repeatability tests all met the relevant requirements. The average recovery rates were 104.00％-108.04％，102.00％-104.94％，100.99％-106.89％，92.00％-95.18％，102.00％-105.06％，103.90％-107.00％（n＝3）， respectively. The contents of impurity A ，B and D in 3 batches of Olmesartan medoxomil hydrochlorothiazide tablets were 0.90％ -1.00％ ，0-0.11％ ，0.16％ -0.24％ ，respectively. The impurity C and other impurities were not detected. There is no significant difference between the results measured by the established method and by the external standard method. CONCLUSIONS：The method has been proved to be highly sensitive and reproducible. It can be used to simultaneously determine four known substances in Olmesartan medoxomil hydrochlorothiazide tablets. |
| 期刊： | 2020年第31卷第07期 |
| 作者： | 李浩贤，林华庆，李俊健，王远见，刘荣，余楚钦 |
| AUTHORS： | LI Haoxian ，LIN Huaqing ，LI Junjian ，WANG Yuanjian ，LIU Rong，YU Chuqin |
| 关键字： | 奥美沙坦酯氢氯噻嗪片；有关物质；高效液相色谱法；加校正因子的主成分自身对照法 |
| KEYWORDS： | Olmesartan medoxomil hydrochlorothiazide tablets ；Related substances ；HPLC；Principal component self-control |
| 阅读数： | 446 次 |
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