HPLC法测定依达拉奉氯化钠注射液中的有关物质
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摘要
目的:建立高效液相法测定依达拉奉氯化钠注射液中的有关物质。方法:色谱柱为Kromasil C_(18)(250 mm×4.6 mm,5μm),以0.2%冰醋酸-0.2%三乙胺水溶液为流动相A,以甲醇为流动相B,梯度洗脱,流速为0.8 ml·min~(-1),检测波长为244nm,柱温为30℃,进样量为20μl。结果:在该色谱条件下,依达拉奉与各已知杂质可完全分离,依达拉奉和各杂质在0.1~3μg·ml~(-1)范围内,峰面积与浓度的线性关系均良好(r>0.998),平均回收率均在90.0%~110.0%之间,RSD<10.0%(n=9),有关物质含量均低于限度(0.3%)。结论:该方法简便快速,准确可靠,专属性强,可作为有效控制依达拉奉氯化钠注射液中有关物质的方法。
Objective: To establish an HPLC method for the determination of the related substances in edaravone and sodium chloride injection. Methods: The column was Kromasil C_(18)( 250 mm×4. 6 mm,5 μm) at the temperature of 30℃. The mobile phase A for gradient elution was a solution containing 0. 2% acetic acid and 0. 2% trimethylamine,and methanol was used as the mobile phase B.The flow rate was 0. 8 ml·min~(-1),the detection wavelength was 244 nm,and the injection volume was 20 μl. Results: Under the described chromatographic conditions,edaravone was completely separated from its impurities. Edaravone and its impurities had good linear relationships within the range of 0. 1 μg·ml~(-1)-3 μg·ml~(-1)( r>0. 998). The average recoveries ranged from 90. 0% to 110. 0%( RSD<10%,n=9),and the contents of their related substances were all below the limits( 0. 3%). Conclusion: The method is accurate,simple and convenient,which can be used for the determination of the related substances in edaravone and sodium chloride injection.
Objective: To establish an HPLC method for the determination of the related substances in edaravone and sodium chloride injection. Methods: The column was Kromasil C_(18)( 250 mm×4. 6 mm,5 μm) at the temperature of 30℃. The mobile phase A for gradient elution was a solution containing 0. 2% acetic acid and 0. 2% trimethylamine,and methanol was used as the mobile phase B.The flow rate was 0. 8 ml·min~(-1),the detection wavelength was 244 nm,and the injection volume was 20 μl. Results: Under the described chromatographic conditions,edaravone was completely separated from its impurities. Edaravone and its impurities had good linear relationships within the range of 0. 1 μg·ml~(-1)-3 μg·ml~(-1)( r>0. 998). The average recoveries ranged from 90. 0% to 110. 0%( RSD<10%,n=9),and the contents of their related substances were all below the limits( 0. 3%). Conclusion: The method is accurate,simple and convenient,which can be used for the determination of the related substances in edaravone and sodium chloride injection.
引文
1 Watanabe K,Morinaka Y,Iseki K,et al.Structure-activity relationship of 3-methyl-1-phenyl-2-pyrazolin-5-one(edaravone)[J].Redox Rep,2003,8(3):151-155
2 Watana be T,Tahara M,Todo S.The novel antioxidant edaravone:from bench to bedside[J].Cardiovase Ther,2008,26(2):101-114
3 Amemiya S,Kamiya T,Nito C,et al.Anti-apoptotic and neuroprotective effects of edaravone following transient focal ischemia in rats[J].Eur J Pharma,2005,516(2):125-130
4 Watanabe T,Tahara M,Todo S.The novel antioxidant edaravone:from bench to bedside[J].Cardiovasc Ther,2008,26(2):101-114
5 郭涛,宋洪涛,孙学惠,等.依达拉奉氯化钠注射液的制备和稳定性考察[J].沈阳部队医药,2013,5(16):206-208
6 刘伟芬,李禄辉,陈运来,等.依达拉奉氯化钠注射液处方及工艺研究[J].河南大学学报(医学版).2015,9(34):175-177
7 付桂英,温明玲,贾立华,等.处方因素对依达拉奉注射液稳定性的影响[J].中国新药杂志,2005,14(6):726-728
8 马利萍,孙建国,彭英,等.依达拉奉清除自由基机制及临床应用[J].中国临床药理学与治疗学,2011,16(3):345-346
9 日本独立行政法人医药品及医疗器械综合管理机构(PMDA).依达拉奉注射液30mg[EB/OL].(2001-06-05)[2015-06-10]http://www.info.pmda.go.jp/go/pack/1190401A1023_3_04
10 许真玉.依达拉奉注射液杂质谱分析[J].中国执业药师,2014,11(8):27-30
11 孙莹,姜波,林大专,等.依达拉奉注射液中有关物质检查方法的研究[J].中国医药指南,2015,4(13):66-67
12 赵珍珍,党小佛.RP-HPLC法测定依达拉奉的含量和有关物质[J].沈阳药科大学学报,2012,29(5):359-363
13 谷铁波,陈贵平.高效液相色谱法测定依达拉奉注射液中依达拉奉及有关物质的含量[J].中国当代医药,2013,20(21):61-65
14 中国药典[S].2015年版.二部.670-672
15 日本药局方[S].2016版.一部.852-853
2 Watana be T,Tahara M,Todo S.The novel antioxidant edaravone:from bench to bedside[J].Cardiovase Ther,2008,26(2):101-114
3 Amemiya S,Kamiya T,Nito C,et al.Anti-apoptotic and neuroprotective effects of edaravone following transient focal ischemia in rats[J].Eur J Pharma,2005,516(2):125-130
4 Watanabe T,Tahara M,Todo S.The novel antioxidant edaravone:from bench to bedside[J].Cardiovasc Ther,2008,26(2):101-114
5 郭涛,宋洪涛,孙学惠,等.依达拉奉氯化钠注射液的制备和稳定性考察[J].沈阳部队医药,2013,5(16):206-208
6 刘伟芬,李禄辉,陈运来,等.依达拉奉氯化钠注射液处方及工艺研究[J].河南大学学报(医学版).2015,9(34):175-177
7 付桂英,温明玲,贾立华,等.处方因素对依达拉奉注射液稳定性的影响[J].中国新药杂志,2005,14(6):726-728
8 马利萍,孙建国,彭英,等.依达拉奉清除自由基机制及临床应用[J].中国临床药理学与治疗学,2011,16(3):345-346
9 日本独立行政法人医药品及医疗器械综合管理机构(PMDA).依达拉奉注射液30mg[EB/OL].(2001-06-05)[2015-06-10]http://www.info.pmda.go.jp/go/pack/1190401A1023_3_04
10 许真玉.依达拉奉注射液杂质谱分析[J].中国执业药师,2014,11(8):27-30
11 孙莹,姜波,林大专,等.依达拉奉注射液中有关物质检查方法的研究[J].中国医药指南,2015,4(13):66-67
12 赵珍珍,党小佛.RP-HPLC法测定依达拉奉的含量和有关物质[J].沈阳药科大学学报,2012,29(5):359-363
13 谷铁波,陈贵平.高效液相色谱法测定依达拉奉注射液中依达拉奉及有关物质的含量[J].中国当代医药,2013,20(21):61-65
14 中国药典[S].2015年版.二部.670-672
15 日本药局方[S].2016版.一部.852-853