胶束毛细管电泳法同时测定小青龙颗粒中的盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱与芍药苷含量
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摘要
目的:建立同时测定小青龙颗粒中盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱、芍药苷含量的方法。方法:采用胶束毛细管电泳法。分离通道为熔融石英毛细管柱,缓冲溶液为10 mmol/L硼砂-10 mmol/L十二烷基硫酸钠的混合溶液(95∶5,pH为10.5),检测波长为195 nm,分离电压为20 kV,毛细管柱温为15℃,压力进样0.5 psi×5 s。取2个厂家各2批小青龙颗粒测定其中盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱、芍药苷的含量,并将测定结果与采用2015年版《中国药典》规定的高效液相色谱法的测定结果进行比较。结果:盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱、芍药苷检测质量浓度线性范围分别为10～160、10～160、1～100、10～500μg/mL(r为0.997 9～0.999 8);精密度、重复性和稳定性试验中的RSD均≤2.74%(n=5～6),平均回收率分别为101.55%、101.62%、100.15%、101.85%,RSD均≤3.94%(n=6);4种成分采用胶束毛细管电泳法与高效液相色谱法测定结果基本一致。结论:建立的胶束毛细管电泳法简捷、快速、灵敏,可同时测定小青龙颗粒中上述4种成分的含量。
OBJECTIVE:To establish the method for simultaneous determination of ephedrine hydrochloride,pseudoephedrine hydrochloride, methamphetamine hydrochloride and paeoniflorin in Xiaoqinglong granule. METHODS: Micellar capillary electrophoresis(MCE)method was adopted. The optimum conditions for the separation were as follows as a fused silica capillary column as the separation channel,the buffer solution composed of 10 mmol/L borax-10 mmol/L SDS(95 ∶ 5,pH 10.5),detection wavelength of 195 nm,separation voltage of 20 kV,capillary column temperature of 15 ℃,the sampling at a pressure for 0.5 psi×5 s. Two batches of Xiaoqinglong granules were collected from 2 manufacturers to determine the contents of ephedrine hydrochloride, pseudoephedrine hydrochloride, methamphetamine hydrochloride and paeoniflorin. The results of content determination were compared with the results determined by HPLC method stated in Chinese Pharmacopeia of 2015 edition.RESULTS:The linear range of ephedrine hydrochloride,pseudoephedrine hydrochloride,methamphetamine hydrochloride and paeoniflorin were 10-160,10-160,1-100,10-500 μg/mL(r=0.997 9-0.999 8),respectively. RSDs of precision,reproducibilityand stability tests were all ≤2.74%(n=5-6). The average recoveries were 101.55%,101.62%,100.15%,101.85%(RSD≤3.94%,n=6),respectively. The contents of 4 components determined by micellar capillary electrophoresis were in accordance with the results of HPLC method. CONCLUSIONS:The established MCE method is simple,quick and sensitive,and can be used for simultaneous determination of 4 components mentioned above in Xiaoqinglong granule.
OBJECTIVE:To establish the method for simultaneous determination of ephedrine hydrochloride,pseudoephedrine hydrochloride, methamphetamine hydrochloride and paeoniflorin in Xiaoqinglong granule. METHODS: Micellar capillary electrophoresis(MCE)method was adopted. The optimum conditions for the separation were as follows as a fused silica capillary column as the separation channel,the buffer solution composed of 10 mmol/L borax-10 mmol/L SDS(95 ∶ 5,pH 10.5),detection wavelength of 195 nm,separation voltage of 20 kV,capillary column temperature of 15 ℃,the sampling at a pressure for 0.5 psi×5 s. Two batches of Xiaoqinglong granules were collected from 2 manufacturers to determine the contents of ephedrine hydrochloride, pseudoephedrine hydrochloride, methamphetamine hydrochloride and paeoniflorin. The results of content determination were compared with the results determined by HPLC method stated in Chinese Pharmacopeia of 2015 edition.RESULTS:The linear range of ephedrine hydrochloride,pseudoephedrine hydrochloride,methamphetamine hydrochloride and paeoniflorin were 10-160,10-160,1-100,10-500 μg/mL(r=0.997 9-0.999 8),respectively. RSDs of precision,reproducibilityand stability tests were all ≤2.74%(n=5-6). The average recoveries were 101.55%,101.62%,100.15%,101.85%(RSD≤3.94%,n=6),respectively. The contents of 4 components determined by micellar capillary electrophoresis were in accordance with the results of HPLC method. CONCLUSIONS:The established MCE method is simple,quick and sensitive,and can be used for simultaneous determination of 4 components mentioned above in Xiaoqinglong granule.
引文
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[7]黄红梅,苏菊,王芳,等.HPLC法同时测定咳速停糖浆中5个生物碱的含量[J].药物分析杂志,2018,38(4):688-695.
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[9]郑孟凯,陶雪芬,钱微微,等.不同地区市售麻黄药材中盐酸麻黄碱、盐酸伪麻黄碱和总生物碱的含量测定[J].中国药房,2015,26(12):1682-1685.
[10]李琴韵,王智华,洪筱坤.HPCE测定小青龙片中麻黄碱和伪麻黄碱的含量[J].中成药,2000,22(2):130-132.
[11]乔姗姗,王雄飞,丁月珠,等.麻黄碱和伪麻黄碱的毛细管电泳分离研究[J].中国中医药信息杂志,2016,23(11):90-93.
[12]郭鸣,李智勇,李洁环,等.HPLC法测定柴芍安神解郁颗粒中芍药苷的含量[J].江西中医药大学学报,2018,30(2):63-64.
[13]YU K,WANG Y W,CHENG YY.Determination of paeonol and paeoniflorin in Chinese medicine Cortex Moutan and‘Shuangdan’granule by micellar electrokinetic capillary chromatography[J].Journal of Pharmaceutical&Biomedical Analysis,2006,40(5):1257-1262.
[14]孙大赢,赵文法,李广华,等.LC-MS/MS法同时测定参芍胶囊中人参皂苷和芍药苷的含量[J].药物分析杂志,2018,38(1):186-190.
[15]韩园园.UPLC法测定黄芪复方愈溃胶囊中的芍药苷含量[J].天津药学,2018,30(2):23-25.
[16]温建英,李文伟,任蕾,等.紫外分光光度法测定晋产白芍芍药苷含量[J].山西中医学院学报,2017,18(3):14-16.
[17]林金明,陈子林.毛细管电泳在药物分析中的应用[J].药学学报,1999,34(9):716-720.
[18]刘训红,李俊松,张月婵,等.MEKC-DAD同时测定大黄及其炮制品中5种蒽醌的含量[J].药物分析杂志,2010,30(5):814-818.
[19]翟宏宇,王海洋,单柏宇,等.不同种类麻黄药材HPLC特征图谱的比较研究[J].时珍国医国药,2017,28(10):2428-2430.
[20]陈燕,兰树敏,林壮民,等.HPLC-UV法同时测定麻黄中5种麻黄生物碱的含量[J].今日药学,2012,22(7):388-391.
[21]李树学,郝宏兴,崔宏鹏,等.甲基麻黄碱与伪麻黄碱镇咳平喘作用比较研究[J].内蒙古中医药,2014,33(13):99-100.
[22]姚琳,邓康颖,罗佳波.甲基麻黄碱与麻黄碱镇咳平喘作用对比研究[J].中药材,2008,31(3):416-417.
[23]郭怀忠,毕开顺,孙毓庆.影响毛细管电泳分析结果重现性的因素及其控制[J].分析仪器,2005(2):42-45.
[2]吴振辉,王有鹏,孟莹.加味六味小青龙颗粒剂治疗小儿急性支气管炎痰湿蕴肺证疗效观察[J].河北中医,2015,37(2):201-203.
[3]于莹,张功,黄海量,等.小青龙汤治疗肺炎临床疗效系统评价[J].山东中医药大学学报,2016,40(6):499-503.
[4]豆红玉.小青龙颗粒治疗小儿哮喘急性发作期(寒哮证)的临床观察[D].济南:山东中医药大学,2015.
[5]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:567.
[6]朱燕飞.HPLC测定小青龙颗粒中麻黄碱、伪麻黄碱的含量[J].中国中药杂志,2008,33(7):848-849.
[7]黄红梅,苏菊,王芳,等.HPLC法同时测定咳速停糖浆中5个生物碱的含量[J].药物分析杂志,2018,38(4):688-695.
[8]罗奕,姚文丽,吴琳琳,等.HPLC法同时测定咳速停胶囊中4种成分[J].中成药,2017,39(1):102-106.
[9]郑孟凯,陶雪芬,钱微微,等.不同地区市售麻黄药材中盐酸麻黄碱、盐酸伪麻黄碱和总生物碱的含量测定[J].中国药房,2015,26(12):1682-1685.
[10]李琴韵,王智华,洪筱坤.HPCE测定小青龙片中麻黄碱和伪麻黄碱的含量[J].中成药,2000,22(2):130-132.
[11]乔姗姗,王雄飞,丁月珠,等.麻黄碱和伪麻黄碱的毛细管电泳分离研究[J].中国中医药信息杂志,2016,23(11):90-93.
[12]郭鸣,李智勇,李洁环,等.HPLC法测定柴芍安神解郁颗粒中芍药苷的含量[J].江西中医药大学学报,2018,30(2):63-64.
[13]YU K,WANG Y W,CHENG YY.Determination of paeonol and paeoniflorin in Chinese medicine Cortex Moutan and‘Shuangdan’granule by micellar electrokinetic capillary chromatography[J].Journal of Pharmaceutical&Biomedical Analysis,2006,40(5):1257-1262.
[14]孙大赢,赵文法,李广华,等.LC-MS/MS法同时测定参芍胶囊中人参皂苷和芍药苷的含量[J].药物分析杂志,2018,38(1):186-190.
[15]韩园园.UPLC法测定黄芪复方愈溃胶囊中的芍药苷含量[J].天津药学,2018,30(2):23-25.
[16]温建英,李文伟,任蕾,等.紫外分光光度法测定晋产白芍芍药苷含量[J].山西中医学院学报,2017,18(3):14-16.
[17]林金明,陈子林.毛细管电泳在药物分析中的应用[J].药学学报,1999,34(9):716-720.
[18]刘训红,李俊松,张月婵,等.MEKC-DAD同时测定大黄及其炮制品中5种蒽醌的含量[J].药物分析杂志,2010,30(5):814-818.
[19]翟宏宇,王海洋,单柏宇,等.不同种类麻黄药材HPLC特征图谱的比较研究[J].时珍国医国药,2017,28(10):2428-2430.
[20]陈燕,兰树敏,林壮民,等.HPLC-UV法同时测定麻黄中5种麻黄生物碱的含量[J].今日药学,2012,22(7):388-391.
[21]李树学,郝宏兴,崔宏鹏,等.甲基麻黄碱与伪麻黄碱镇咳平喘作用比较研究[J].内蒙古中医药,2014,33(13):99-100.
[22]姚琳,邓康颖,罗佳波.甲基麻黄碱与麻黄碱镇咳平喘作用对比研究[J].中药材,2008,31(3):416-417.
[23]郭怀忠,毕开顺,孙毓庆.影响毛细管电泳分析结果重现性的因素及其控制[J].分析仪器,2005(2):42-45.
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