地氯雷他定原料药中元素杂质的测定
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摘要
目的建立电感耦合等离子质谱法测定地氯雷他定中元素杂质含量。方法参照ICH Q3D元素杂质指导原则确定了地氯雷他定原料药中潜在元素杂质,并使用电感耦合等离子质谱仪测定元素杂质含量。结果在考察浓度范围内线性关系良好,各元素杂质R~2均大于0.9995;各杂质回收率均在80%~120%之间,RSD均小于15%(n=9);各元素杂质精密度RSD均小于15%。结论方法学验证表明本方法简单、可靠,可对原料药中元素杂质进行有效控制。
Objective To establish a method for the determination of elemental impurities in desloratadine APIs. Methods The potential elemental impurities in desloratadine APIs were determined according to the ICH Q3 D: Guidelines for Elemental Impurities. The method for determination of potential elemental impurities by ICP-MS was established. Results All the calibration curves of the potential elemental impurities showed good linearity(r>0.9998) in the test concentration range, and R~2 of each element is greater than 0.9995. The average recoveries of the potential elemental impurities ranged 80 %-120 %, with RSDs<15 %(n=9). RSDs of the precision tests were lower than 15 %. Conclusion This method is simple, flexible and of good repeatability, which can be used for the determination of the potential elemental impurities in desloratadine APIs.
Objective To establish a method for the determination of elemental impurities in desloratadine APIs. Methods The potential elemental impurities in desloratadine APIs were determined according to the ICH Q3 D: Guidelines for Elemental Impurities. The method for determination of potential elemental impurities by ICP-MS was established. Results All the calibration curves of the potential elemental impurities showed good linearity(r>0.9998) in the test concentration range, and R~2 of each element is greater than 0.9995. The average recoveries of the potential elemental impurities ranged 80 %-120 %, with RSDs<15 %(n=9). RSDs of the precision tests were lower than 15 %. Conclusion This method is simple, flexible and of good repeatability, which can be used for the determination of the potential elemental impurities in desloratadine APIs.
引文
[1]ICH.ICH Q3D Step 4 Version Guideline For Elemental Impurities[EB/OL].(2013-06-06)http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q3D/Q3D_Step-4.pdf.2013.
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[3]刘玲玲,冯信忠,王群,等.地氯雷他定治疗慢性特发性荨麻疹临床疗效观察[J].临床皮肤科杂志,2006,35(8):540-541.
[4]庄辉传,李想,相芳.地氯雷他定药理作用及机制研究进展[J].中南药学,2010,8(1):48-51.
[5]徐文严.地氯雷他定:一种新的抗组胺药[J].中华皮肤科杂志,2003,36(11):668-670.
[6]徐道华.第三代抗组胺药地氯雷他定[J].中国新药杂志,2005,14(12):1486-1488.
[7]U.S. Pharmacopeial Convention.<233>Elemental impuritiesprocedures.[EB/OL](2012-11-15)[2013-03-25]http://www.usp.org/sites/default/files/usp_pdf/EN/USPNF/key-issues/c233_final.pdf. 2013
[8]杨晓华,陈晓霞.微波消解-原子荧光光谱法同时测定维生素B_(12)中的砷和汞的含量[J].饲料研究,2015,(10):44-46.
[9]李莉,赵桂莉.微波消解-电感耦合等离子体质谱(ICP-MS)法测定化学原料药中痕量钯含量[J].中国无机分析化学,2016,6(1):6-9.
[10]严宾.电感耦合等离子体质谱法测定索非布韦原料药锡的残留量[J].江苏工程职业技术学院学报,2017,(3):24-26.
[11]韩峰超,孙晓娟,董宇,等.电感耦合等离子体质谱法测定注射液中铝离子浓度[J].实用药物与临床,2010,13(3):195-196.
[12]甘志永,沈宁宁,李艳荣,等. ICP-MS法测定水中总汞的方法探究[J].环境科技,2017,30(3):56-58.
[13]舒凤,张远志,王宏磊,等. ICP-MS测定汞的记忆效应的研究[J].中国卫生检验杂志,2016,(2):189-191.
[14] Sima L,Wang Y,Lin Y,et al. Synthesis of loratadine[J].Chemistry, 2012, 75(4):353-356.
[15]谢艳,吾国强,郑土才,等. 8-氯-10,11-二氢-4-氮杂-5H-二苯并[a,d]-5-环庚酮的合成新方法[J].中国药物化学杂志,2006,16(1):49-50.
[16]谢艳,高建荣,王俊艳.合成8-氯-10,11-二氢-4-氮杂-5H-二苯并[a,d]-5-环庚酮研究进展[J].化工生产与技术,2008,15(4):26-28.
[2]姜小林,董素萍,舒靖能. ICH Q3D新药制剂元素杂质评估及控制的要点解读[J].中国药事,2017,31(8):854-860.
[3]刘玲玲,冯信忠,王群,等.地氯雷他定治疗慢性特发性荨麻疹临床疗效观察[J].临床皮肤科杂志,2006,35(8):540-541.
[4]庄辉传,李想,相芳.地氯雷他定药理作用及机制研究进展[J].中南药学,2010,8(1):48-51.
[5]徐文严.地氯雷他定:一种新的抗组胺药[J].中华皮肤科杂志,2003,36(11):668-670.
[6]徐道华.第三代抗组胺药地氯雷他定[J].中国新药杂志,2005,14(12):1486-1488.
[7]U.S. Pharmacopeial Convention.<233>Elemental impuritiesprocedures.[EB/OL](2012-11-15)[2013-03-25]http://www.usp.org/sites/default/files/usp_pdf/EN/USPNF/key-issues/c233_final.pdf. 2013
[8]杨晓华,陈晓霞.微波消解-原子荧光光谱法同时测定维生素B_(12)中的砷和汞的含量[J].饲料研究,2015,(10):44-46.
[9]李莉,赵桂莉.微波消解-电感耦合等离子体质谱(ICP-MS)法测定化学原料药中痕量钯含量[J].中国无机分析化学,2016,6(1):6-9.
[10]严宾.电感耦合等离子体质谱法测定索非布韦原料药锡的残留量[J].江苏工程职业技术学院学报,2017,(3):24-26.
[11]韩峰超,孙晓娟,董宇,等.电感耦合等离子体质谱法测定注射液中铝离子浓度[J].实用药物与临床,2010,13(3):195-196.
[12]甘志永,沈宁宁,李艳荣,等. ICP-MS法测定水中总汞的方法探究[J].环境科技,2017,30(3):56-58.
[13]舒凤,张远志,王宏磊,等. ICP-MS测定汞的记忆效应的研究[J].中国卫生检验杂志,2016,(2):189-191.
[14] Sima L,Wang Y,Lin Y,et al. Synthesis of loratadine[J].Chemistry, 2012, 75(4):353-356.
[15]谢艳,吾国强,郑土才,等. 8-氯-10,11-二氢-4-氮杂-5H-二苯并[a,d]-5-环庚酮的合成新方法[J].中国药物化学杂志,2006,16(1):49-50.
[16]谢艳,高建荣,王俊艳.合成8-氯-10,11-二氢-4-氮杂-5H-二苯并[a,d]-5-环庚酮研究进展[J].化工生产与技术,2008,15(4):26-28.