高效毛细管电泳法分离测定苯磺酸氨氯地平片中的消旋体
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摘要
目的建立分离并同时测定苯磺酸氨氯地平片中消旋体的方法。方法采用高效毛细管电泳法,使用熔融硅胶毛细管柱,5 mmol·L~(-1)磷酸二氢钠-β-环糊精缓冲液,分离电压20 k V,进样电压10 k V,持续5 s,检测波长230 nm,柱温25℃。结果苯磺酸氨氯地平消旋体成功实现基线分离,方法精密度RSD分别为0.72%(左旋)和2.32%(右旋);稳定性RSD分别为0.69%,1.79%;加样回收率为100.62%(RSD 2.90%)和98.93%(RSD 2.56%)。10批苯磺酸氨氯地平片中,左旋氨氯地平的含量在4.32～4.77 mg·g~(-1)之间,占87.33%,右旋氨氯地平的含量在0.64～0.67 mg·g~(-1)之间,占12.67%。结论本研究实现了氨氯地平消旋体的手性拆分和含量测定,方法快速、准确,能够为后续该制剂的质量和有效性评价提供参考。
OBJECTIVE To establish a separation and simultaneous determination method for racemes in amlodipine benzene sulfonate tablet. METHODS High performance capillary electrophoresis( HPCE) was adopted by using fused-silica capillary,the running buffer was 5 mmol·L~(-1) sodium dihydrogen phosphate-β-cyclodextrin,the separation voltage was 20 kV,injection voltage was10 kV for 5 s,the detection wavelength was 230 nm,the column temperature was 25 ℃,a certain type amlodipine benzene sulfonate tablet( code name: AL017) was chosen as sample. RESULTS The racemes achieved baseline separation,precision of the method had an RSD of 0. 72%( for levamlodipine) and 2. 32%( for dextromethorphan); for stability,the RSD was 0. 69% and 1. 79%,respectively; for recovery,the mean value was 100.62%( RSD 2.90%) and 98.93%( RSD 2.56%).In 10 batches of the tablet,mean content of levamlodipine was 4.55 mg·g-1( 87.33%),dextromethorphan was 0.66 mg·g-1( 12.67%); CONCLUSION The study achieved baseline separation and quantitative determination for amlodipine benzene sulfonate racemes,the method used was fast and accurate,which provided reference for further evaluation of its quality and efficacy.
OBJECTIVE To establish a separation and simultaneous determination method for racemes in amlodipine benzene sulfonate tablet. METHODS High performance capillary electrophoresis( HPCE) was adopted by using fused-silica capillary,the running buffer was 5 mmol·L~(-1) sodium dihydrogen phosphate-β-cyclodextrin,the separation voltage was 20 kV,injection voltage was10 kV for 5 s,the detection wavelength was 230 nm,the column temperature was 25 ℃,a certain type amlodipine benzene sulfonate tablet( code name: AL017) was chosen as sample. RESULTS The racemes achieved baseline separation,precision of the method had an RSD of 0. 72%( for levamlodipine) and 2. 32%( for dextromethorphan); for stability,the RSD was 0. 69% and 1. 79%,respectively; for recovery,the mean value was 100.62%( RSD 2.90%) and 98.93%( RSD 2.56%).In 10 batches of the tablet,mean content of levamlodipine was 4.55 mg·g-1( 87.33%),dextromethorphan was 0.66 mg·g-1( 12.67%); CONCLUSION The study achieved baseline separation and quantitative determination for amlodipine benzene sulfonate racemes,the method used was fast and accurate,which provided reference for further evaluation of its quality and efficacy.
引文
[1]杭亮,张永刚,田慧娟.左旋氨氯地平联合天麻钩藤颗粒对高血压病人NT-Pro BNP与颈部血管内膜厚度的影响[J].中西医结合心脑血管病杂志,2018,16(10):1327-1330.
[2]贾德安,王志坚,杨士伟,等.缬沙坦/氨氯地平或氨氯地平单药治疗高危高血压患者[J].中华高血压杂志,2013,21(6):569-572.
[3]许会,汤卫国,黄春玉,等.HPLC法测定复方氨氯地平缬沙坦氢氯噻嗪片剂溶出度[J].药物分析杂志,2015,35(1):46-51.
[4]潘华玲,林丽珊,丁珏芳,等.LC-HESI/MS/MS法同时测定人血浆中氨氯地平、贝那普利和贝那普利拉[J].药学学报,2014,49(1):95-100.
[5]李杨杰,欧国灯,李泳雪,等.HPLC-MS-MS法测定降压类中成药和保健食品中非法添加氨氯地平和乐卡地平的研究[J].中成药,2013,35(5):956-960.
[6]Constantina P K C,Zhu X F,Isiah M W.Analytical separations in open-tubular capillary electrochromatography[J].Electrophoresis,2003,24:3917-3934.
[7]Sebastiaan E,Wim T K.Recent applications in capillary electrochromatography[J].Electrophoresis,2006,27:84-96.
[2]贾德安,王志坚,杨士伟,等.缬沙坦/氨氯地平或氨氯地平单药治疗高危高血压患者[J].中华高血压杂志,2013,21(6):569-572.
[3]许会,汤卫国,黄春玉,等.HPLC法测定复方氨氯地平缬沙坦氢氯噻嗪片剂溶出度[J].药物分析杂志,2015,35(1):46-51.
[4]潘华玲,林丽珊,丁珏芳,等.LC-HESI/MS/MS法同时测定人血浆中氨氯地平、贝那普利和贝那普利拉[J].药学学报,2014,49(1):95-100.
[5]李杨杰,欧国灯,李泳雪,等.HPLC-MS-MS法测定降压类中成药和保健食品中非法添加氨氯地平和乐卡地平的研究[J].中成药,2013,35(5):956-960.
[6]Constantina P K C,Zhu X F,Isiah M W.Analytical separations in open-tubular capillary electrochromatography[J].Electrophoresis,2003,24:3917-3934.
[7]Sebastiaan E,Wim T K.Recent applications in capillary electrochromatography[J].Electrophoresis,2006,27:84-96.