复方枸橼酸喷托维林颗粒中薄荷脑和麝香草酚的定性鉴别和含量测定
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摘要
目的建立复方枸橼酸喷托维林颗粒中薄荷脑和麝香草酚的定性鉴别和含量测定方法。方法采用薄层色谱法对薄荷脑和麝香草酚进行定性鉴别,采用GC色谱法对薄荷脑和麝香草酚进行含量测定。色谱条件:使用DBWAX(30 m×0.32 mm×0.25μm)毛细柱,FID检测器,进样口温度230℃,检测器温度250℃。结果薄层鉴别斑点清晰,阴性对照无干扰。在选定的色谱条件下,两种物质分离良好,薄荷脑的回归方程为y=2681.10x-10.81(r=1.00),平均回收率为98.0%(n=6,RSD=2.3%),线性范围为:0.016~1.55 g/L;麝香草酚的回归方程为y=2762.00x-6.64(r=1.00),平均回收率为100.4%(n=6,RSD=1.5%),线性范围为:0.010~1.00 g/L。三批样品中两种组分的含量分别为0.13 mg/g和0.096 mg/g。结论该方法简单准确,可用于该制剂中的薄荷脑和麝香草酚的定性鉴别和含量测定。
Objective To establish a method of qualitative identification and content determination of menthol and thymol in Compound Pentoxyverine Citrate Granules. Methods TLC was applied for qualitative of menthol and thymol; GC was used for quantitative determination of menthol and thymol. A DB-WAX column(30 m ×0.32 mm ×0.25 μm) was used. The inlet temperature was 230℃ and the FID detector temperature was 250℃. Results TLC spots were clear and well separated, there was no interference for negative sample. A good resolution was obtained by this method between the peaks of menthol and thymol. The linearity equation of menthol was y =2681.10x-10.81(r = 1.00), the average recovery was 98.0%(n=6, RSD =2.3%), and the linear range was 0.016-1.55 g/L. The linearity equation of thymol was y = 2762.00x-6.64(r =1.00), the average recovery was 100.4%(n=6, RSD =1.5%), and the linear range was 0.010-1.00 g/L.The average contents of 3 batches of samples were 0.13 mg/g and 0.096 mg/g. Conclusion The method was simple and accurate, which can be used for qualitative identification and content determination of menthol and thymol in Compound Pentoxyverine Citrate Granules.
Objective To establish a method of qualitative identification and content determination of menthol and thymol in Compound Pentoxyverine Citrate Granules. Methods TLC was applied for qualitative of menthol and thymol; GC was used for quantitative determination of menthol and thymol. A DB-WAX column(30 m ×0.32 mm ×0.25 μm) was used. The inlet temperature was 230℃ and the FID detector temperature was 250℃. Results TLC spots were clear and well separated, there was no interference for negative sample. A good resolution was obtained by this method between the peaks of menthol and thymol. The linearity equation of menthol was y =2681.10x-10.81(r = 1.00), the average recovery was 98.0%(n=6, RSD =2.3%), and the linear range was 0.016-1.55 g/L. The linearity equation of thymol was y = 2762.00x-6.64(r =1.00), the average recovery was 100.4%(n=6, RSD =1.5%), and the linear range was 0.010-1.00 g/L.The average contents of 3 batches of samples were 0.13 mg/g and 0.096 mg/g. Conclusion The method was simple and accurate, which can be used for qualitative identification and content determination of menthol and thymol in Compound Pentoxyverine Citrate Granules.
引文
[1]国家药典委员会.国家药品标准——化学药品地方标准上升国家标准第十二册[S].WS-10001-(HD-1152)-2002.
[2]柴鑫莉,祝春仙,姜玲丽,等.顶空气相色谱法测定市售56批次强力枇杷露中薄荷脑的含量[J].中国药房,2015,26(30):4288-4290.
[3]裴香萍,裴妙荣,李慧峰,等.气相色谱法测定山西产地椒中麝香草酚及香荆芥酚的含量[J].中国实验方剂学杂志,2013,19(14):132-134.
[4]王海波,宋汉敏,李振国.气相色谱法同时测定关节止痛膏中樟脑、薄荷脑、水杨酸甲酯的含量[J].中国实验方剂学杂志,2013,19(7):77-80.
[5]刘俊丽,段松冷,曾蔚欣.氨薄荷搽剂中薄荷脑含量测定方法研究[J].安徽医药,2016,20(2):267-270.
[6]王俊丽,李加恒,盖静.毛细管气相色谱法同时测定复方樟脑搽剂中樟脑、薄荷脑含量[J].西北国防医学杂志,2016,37(3):164-166.
[7]柳梦婷,方婧,唐力英,等.苍耳子鼻炎滴丸中薄荷脑和龙脑的含量测定及指纹图谱研究[J].中国药物警戒,2016,13(1):16-23.
[8]邓康程.气相色谱法测定三红软膏中冰片、薄荷脑、樟脑的含量[J].海峡药学,2016,28(1):64-66.
[9]苟林宏,安宝文,王俊丽,等.GC法同时测定复方苯海拉明搽剂中樟脑和薄荷脑的含量[J].中国药房,2015,26(30):4297-4299.
[10]周俊,付宜和,彭柳.气相色谱法测定维C银翘片中薄荷脑的含量[J].湖北中医杂志,2015,37(6):67-68.
[11]李波.气相色谱法测定云威灵药材中麝香草酚的含量研究[J].中国民族民间医药,2016,25(11):8-9.
[12]韩晓珂,梁朝锋,祁俊.十七味大活血胶囊的质量标准研究[J].中国医药导报,2016,13(12):147-151.
[13]许本善,雷宁,马萍,等.复方痔疮栓的定性鉴别与定量分析方法研究[J].中国医药导报,2015,12(33):8-12.
[14]聂红梅,熊维政,武惠斌.气相色谱法同时测定消炎镇痛膏中5种组分含量[J].中医学报,2015,30(5):711-713.
[15]张润容,叶雪峰,陈海燕.毛细管气相色谱法同时测定活络油中8种成分的含量[J].中药新药与临床药理,2016,27(3):413-417.
[16]李凤丽,李进,高文远,等.毛细管气相色谱法同时测定暑热宁口服液中6个有效成分的含量[J].中华中医药杂志,2015,30(2):572-574.
[17]霍丽霞,鲁寅生,郭青,等.GC法测定银翘解毒系列制剂中薄荷脑、薄荷酮和胡薄荷酮[J].药物评价研究,2015,38(1):66-70.
[18]林林,刘广桢,刘洪超,等.GC法同时测定羚羊感冒片中7种成分[J].中成药,2016,38(9):1947-1951.
[19]张伟,林诗玥,吴孟华.气相色谱法同时测定消炎镇痛膏中4种成分的含量[J].中药材,2015,38(3):621-623.
[20]丁礼琴,金家骅.GC测定清凉油中薄荷脑#樟脑#桉油精和丁香酚的含量[J].中国实验方剂学杂志,2014,20(13):85-89.
[2]柴鑫莉,祝春仙,姜玲丽,等.顶空气相色谱法测定市售56批次强力枇杷露中薄荷脑的含量[J].中国药房,2015,26(30):4288-4290.
[3]裴香萍,裴妙荣,李慧峰,等.气相色谱法测定山西产地椒中麝香草酚及香荆芥酚的含量[J].中国实验方剂学杂志,2013,19(14):132-134.
[4]王海波,宋汉敏,李振国.气相色谱法同时测定关节止痛膏中樟脑、薄荷脑、水杨酸甲酯的含量[J].中国实验方剂学杂志,2013,19(7):77-80.
[5]刘俊丽,段松冷,曾蔚欣.氨薄荷搽剂中薄荷脑含量测定方法研究[J].安徽医药,2016,20(2):267-270.
[6]王俊丽,李加恒,盖静.毛细管气相色谱法同时测定复方樟脑搽剂中樟脑、薄荷脑含量[J].西北国防医学杂志,2016,37(3):164-166.
[7]柳梦婷,方婧,唐力英,等.苍耳子鼻炎滴丸中薄荷脑和龙脑的含量测定及指纹图谱研究[J].中国药物警戒,2016,13(1):16-23.
[8]邓康程.气相色谱法测定三红软膏中冰片、薄荷脑、樟脑的含量[J].海峡药学,2016,28(1):64-66.
[9]苟林宏,安宝文,王俊丽,等.GC法同时测定复方苯海拉明搽剂中樟脑和薄荷脑的含量[J].中国药房,2015,26(30):4297-4299.
[10]周俊,付宜和,彭柳.气相色谱法测定维C银翘片中薄荷脑的含量[J].湖北中医杂志,2015,37(6):67-68.
[11]李波.气相色谱法测定云威灵药材中麝香草酚的含量研究[J].中国民族民间医药,2016,25(11):8-9.
[12]韩晓珂,梁朝锋,祁俊.十七味大活血胶囊的质量标准研究[J].中国医药导报,2016,13(12):147-151.
[13]许本善,雷宁,马萍,等.复方痔疮栓的定性鉴别与定量分析方法研究[J].中国医药导报,2015,12(33):8-12.
[14]聂红梅,熊维政,武惠斌.气相色谱法同时测定消炎镇痛膏中5种组分含量[J].中医学报,2015,30(5):711-713.
[15]张润容,叶雪峰,陈海燕.毛细管气相色谱法同时测定活络油中8种成分的含量[J].中药新药与临床药理,2016,27(3):413-417.
[16]李凤丽,李进,高文远,等.毛细管气相色谱法同时测定暑热宁口服液中6个有效成分的含量[J].中华中医药杂志,2015,30(2):572-574.
[17]霍丽霞,鲁寅生,郭青,等.GC法测定银翘解毒系列制剂中薄荷脑、薄荷酮和胡薄荷酮[J].药物评价研究,2015,38(1):66-70.
[18]林林,刘广桢,刘洪超,等.GC法同时测定羚羊感冒片中7种成分[J].中成药,2016,38(9):1947-1951.
[19]张伟,林诗玥,吴孟华.气相色谱法同时测定消炎镇痛膏中4种成分的含量[J].中药材,2015,38(3):621-623.
[20]丁礼琴,金家骅.GC测定清凉油中薄荷脑#樟脑#桉油精和丁香酚的含量[J].中国实验方剂学杂志,2014,20(13):85-89.
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