HPLC法测定米拉贝隆原料药中有关物质
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摘要
目的:建立米拉贝隆原料药中有关物质的高效液相色谱测定方法。方法:采用YMC-Pack ODS-A色谱柱(250 mm×4.6 mm,5μm),流动相为缓冲溶液(己烷磺酸钠一水合物5.65 g与磷酸二氢钠2.75 g,加水1 000 ml使溶解,磷酸调节pH值至2.3)–乙腈,梯度洗脱,体积流量为0.8 ml/min,柱温为30℃,检测波长为280 nm,进样量:10μl。结果:在所选定的液相色谱条件下,有关物质与主药分离良好。米拉贝隆、杂质A、杂质B、杂质C和杂质D的检出限分别为8.5、4.5、5.4、6.6和10.0 ng。结论:该方法操作简单,重复性好,专属性强,可用于控制米拉贝隆原料药中的有关物质。
Objective: To establish an RP-HPLC method for the determination of related substances in Mirabegron. Methods:The separation was performed on a YMC-Pack ODS-A column( 250 mm × 4. 6 mm,5 μm) with the mobile phase of( 5. 65 g sodium 1-hexanesulfonate monohydrate and 2. 75 g sodium dihydrogen phosphate in 1 000 ml water,adjust the pH value to 2. 3with phosphate)-acetonitrile for gradient elution. The flow rate was 0. 8 ml/min with injection volume of 10 μl,the temperature of column was set 30 ℃,and the detection wavelength was set at 280 nm. Results: Mirabegron and its related substances could be completely separated under the conditions. The detection limits of Mirabegron,impurities A,B,C and D were 8. 5,4. 5,5. 4,6. 6 and 10. 0 ng. Conclusion: The method is simple,quick,accurate,and reliable,which can control the related substances in Mirabegron.
Objective: To establish an RP-HPLC method for the determination of related substances in Mirabegron. Methods:The separation was performed on a YMC-Pack ODS-A column( 250 mm × 4. 6 mm,5 μm) with the mobile phase of( 5. 65 g sodium 1-hexanesulfonate monohydrate and 2. 75 g sodium dihydrogen phosphate in 1 000 ml water,adjust the pH value to 2. 3with phosphate)-acetonitrile for gradient elution. The flow rate was 0. 8 ml/min with injection volume of 10 μl,the temperature of column was set 30 ℃,and the detection wavelength was set at 280 nm. Results: Mirabegron and its related substances could be completely separated under the conditions. The detection limits of Mirabegron,impurities A,B,C and D were 8. 5,4. 5,5. 4,6. 6 and 10. 0 ng. Conclusion: The method is simple,quick,accurate,and reliable,which can control the related substances in Mirabegron.
引文
1唐启东,宫平.米拉贝隆[J].中国药物化学杂志,2012,22(6):544
2范鸣.膀胱过度活动症治疗药Mirabegron[J].药学进展,2012,36(3):133-135
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4 王阳贇.米拉贝隆在膀胱过度活动症治疗中的研究现状[J].现代泌尿外科杂志,2014,19(8):559-562
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9 周鑫,崔元善,闰慧磊,等.米拉贝隆治疗膀胱活动过度症的荟萃分析[J].现代泌尿外科杂志,2015,20(7):498-503
10 李海元,周逢海,马玉磊,等.膀胱过度活动症治疗新药米拉贝隆[J].中国新药杂志,2014,23(19):2215-2218
11 杜淑朋,周天舒,宋维锋,等.HPLC法测定注射用头孢孟多酯钠中有关物质[J].现代药物与临床,2015,30(10):1204-1207
12 王茉莉,宋更申,常俊山.HPLC法同时测定杆菌肽原料药中主成分的含量及有关物质[J].中国药房,2015,26(6):834-837
13 张震,孙燕.HPLC法测定阿哌沙班中的有关物质[J].天津药学,2014,26(6):9-11
2范鸣.膀胱过度活动症治疗药Mirabegron[J].药学进展,2012,36(3):133-135
3 章磊,谭支敏,焦慧荣,等.米拉贝隆有关物质的合成[J].中国医药工业杂志,2014,45(1):9-12
4 王阳贇.米拉贝隆在膀胱过度活动症治疗中的研究现状[J].现代泌尿外科杂志,2014,19(8):559-562
5 胡凡,王伸勇,贾新赞,等.一种米拉贝隆的合成方法[P].中国:103193730,2013-04-17
6 丸山龙也,铃木贵之,恩田健一,等.酰胺衍生物或其盐类[P].中国:1218045,1998-10-16
7 Kawazoe S,Sakamoto K,Awamura Y,et al.Alpha-form orbetaform crystal of acetanilide derivative[P].EP:1440969,2002-10-29
8 李杨.米拉贝隆的合成及工艺优化[D].哈尔滨:黑龙江大学,2014
9 周鑫,崔元善,闰慧磊,等.米拉贝隆治疗膀胱活动过度症的荟萃分析[J].现代泌尿外科杂志,2015,20(7):498-503
10 李海元,周逢海,马玉磊,等.膀胱过度活动症治疗新药米拉贝隆[J].中国新药杂志,2014,23(19):2215-2218
11 杜淑朋,周天舒,宋维锋,等.HPLC法测定注射用头孢孟多酯钠中有关物质[J].现代药物与临床,2015,30(10):1204-1207
12 王茉莉,宋更申,常俊山.HPLC法同时测定杆菌肽原料药中主成分的含量及有关物质[J].中国药房,2015,26(6):834-837
13 张震,孙燕.HPLC法测定阿哌沙班中的有关物质[J].天津药学,2014,26(6):9-11