消炎癣湿药膏的质量标准提升研究
|
摘要
目的提升消炎癣湿药膏的质量标准,更好地控制产品的质量。方法分别采用薄层色谱法(TLC)及气相色谱法(GC)对消炎癣湿药膏中的蛇床子、冰片和樟脑进行定性鉴别;分别采用高效液相色谱法(HPLC)和GC对药膏中的苯酚、花椒毒素、欧前胡素、蛇床子素、升华硫5种非挥发性成分和樟脑、龙脑、异龙脑3种挥发性成分进行含量测定;并采用上述方法对自制和市售软膏进行检测。结果所建立的蛇床子、冰片的TLC鉴别方法,斑点清晰,Rf值适中,分离度良好;樟脑、冰片的GC鉴别方法,专属性强,易于操作;HPLC测定苯酚、花椒毒素、欧前胡素、蛇床子素、升华硫线性范围分别为24.98～1598.62、0.29～18.59、0.33～21.33、1.26～80.35、10.23～327.40μg·mL-1,平均加样回收率为97.9%～105.8%;GC测定樟脑、龙脑、异龙脑的线性范围分别为8.92～570.75、6.52～417.50、5.28～337.50μg·mL-1,平均加样回收率为96.2%～99.5%。结论所建方法准确灵敏,易于操作,专属性强,重复性好,较好地提升了消炎癣湿药膏的质量控制水平。
Objective To improve the quality standard for Xiaoyan Xuanshi ointment and better control the product quality. Methods Thin layer chromatography(TLC) and gas chromatography(GC) were used to qualitatively identify cnidium, borneol and camphor in Xiaoyan Xuanshi ointment, respectively. High performance liquid chromatography(HPLC) and GC were used to determine the content of the five nonvolatile components including phenol, xanthotoxin, imperatorin, osthole, and sublimed sulfur, and the three volatile components(camphor, borneol and isobornol). The homemade and marketed ointment were tested by the above method. Results The TLC qualitative identification spots of cnidium and borneol were clear, the Rf value was moderate, with good resolution. The GC qualitative identification of camphor and borneol was specific and easy to operate. For HPLC determination, the linear ranges of phenol, xanthotoxin, imperatorin, osthole, and sublimed sulfur was 24.98-1598.62, 0.29-18.59, 0.33-21.33, 1.26-80.35, and 10.23-327.40 μg·mL-1, respectively. The average recovery was 97.9%-105.8%. For GC analysis, the linear range of camphor, borneol and isoborneol were 8.92-570.75, 6.52-417.50, and 5.28-337.50 μg·mL-1, respectively. The average recovery was 96.2%-99.5%. Conclusion The method is accurate and sensitive with easy operation, strong specificity and reproducibility, and greatly improves the quality control of Xiaoyan Xuanshi ointment.
Objective To improve the quality standard for Xiaoyan Xuanshi ointment and better control the product quality. Methods Thin layer chromatography(TLC) and gas chromatography(GC) were used to qualitatively identify cnidium, borneol and camphor in Xiaoyan Xuanshi ointment, respectively. High performance liquid chromatography(HPLC) and GC were used to determine the content of the five nonvolatile components including phenol, xanthotoxin, imperatorin, osthole, and sublimed sulfur, and the three volatile components(camphor, borneol and isobornol). The homemade and marketed ointment were tested by the above method. Results The TLC qualitative identification spots of cnidium and borneol were clear, the Rf value was moderate, with good resolution. The GC qualitative identification of camphor and borneol was specific and easy to operate. For HPLC determination, the linear ranges of phenol, xanthotoxin, imperatorin, osthole, and sublimed sulfur was 24.98-1598.62, 0.29-18.59, 0.33-21.33, 1.26-80.35, and 10.23-327.40 μg·mL-1, respectively. The average recovery was 97.9%-105.8%. For GC analysis, the linear range of camphor, borneol and isoborneol were 8.92-570.75, 6.52-417.50, and 5.28-337.50 μg·mL-1, respectively. The average recovery was 96.2%-99.5%. Conclusion The method is accurate and sensitive with easy operation, strong specificity and reproducibility, and greatly improves the quality control of Xiaoyan Xuanshi ointment.
引文
[1]中华人民共和国卫生部药品标准中药成方制剂[S].第六册. 1998:148.
[2]石磊,赵志栋,关键.消炎癣湿药膏治愈顽固性疥疮3例[J].临床医学,2016,36(9):126.
[3]沙文茹.小品种的大市场[J].中国药店,2006,1(9):86-88.
[4]佘一鸣,胡永慧,韩立云,等.中药质量控制的研究进展[J].中草药,2017,48(12):2557-2563.
[5]戈勋,孙洪胜,李刚,等.妇阴康洗剂质量标准研究[J].中南药学,2017,15(10):1441-1446.
[6]谭静玲,宋爱华,覃金玲,等.洁妇尔洗剂的质量标准研究[J].中国现代中药,2015,17(10):1083-1086.
[7]宋丽娇,李晋,姜艳,等.蛇床子香豆素类成分的含量测定及指纹图谱研究[J].天津中医药,2016,33(6):368-372.
[8]Jia M,Li YM,Zhai X,et al. Qualitative analysis and quality evaluation of Cnidium monnieri using UHPLC-ESIQ-TOF/MS[J]. Chinese Herbal Medicines,2016,8(4):323-330.
[9]冯倩倩,陈飞,安靖霏,等. HPLC法测定苯酚消毒液和复方薄荷脑醑中苯酚的含量[J].实用药物与临床,2016,19(12):1523-1525.
[10]中国药典2015年版.四部[S]. 2015:57,63.
[11]贾善学,赵卫,史保荣,等.《卫生部药品标准》中药成方制剂收载情况分析[J].中国药品标准,2002,3(3):18-19.
[12]孙国祥,陈新新,孙万阳,等.中药标准制剂控制模式发展历程和构建全质量关控制中药质量模式[J].中南药学,2014,12(1):1-9.
[13]Gao FY,Hu YS,Ye XL,et al. Optimal extraction and fingerprint analysis of Cnidii fructus by accelerated solvent extraction and high performance liquid chromatographic analysis with photodiode array and mass spectrometry detections[J]. Food Chem,2013,141(3):1962-1971.
[14]Li YM,JiaM,LiHQ,etal.Cnidiummonnieri:A review of traditional uses,phytochemical and ethnopharmacological properties[J]. Am J Chinese Med,2015,43(5):835-877.
[15]韩希英.升华硫的药用经验及开发初探[J].药学实践杂志,2003,21(2):117.
[16]栗建明,袁震霆,张彤,等.气相色谱法测定舒筋理伤油中4种有效成分的含量[J].中南药学,2015,13(10):1086-1089.
[17]尚坤,李敬文,常美月,等.冰片化学成分及药理作用研究[J].吉林中医药,2018,38(1):93-95.
[2]石磊,赵志栋,关键.消炎癣湿药膏治愈顽固性疥疮3例[J].临床医学,2016,36(9):126.
[3]沙文茹.小品种的大市场[J].中国药店,2006,1(9):86-88.
[4]佘一鸣,胡永慧,韩立云,等.中药质量控制的研究进展[J].中草药,2017,48(12):2557-2563.
[5]戈勋,孙洪胜,李刚,等.妇阴康洗剂质量标准研究[J].中南药学,2017,15(10):1441-1446.
[6]谭静玲,宋爱华,覃金玲,等.洁妇尔洗剂的质量标准研究[J].中国现代中药,2015,17(10):1083-1086.
[7]宋丽娇,李晋,姜艳,等.蛇床子香豆素类成分的含量测定及指纹图谱研究[J].天津中医药,2016,33(6):368-372.
[8]Jia M,Li YM,Zhai X,et al. Qualitative analysis and quality evaluation of Cnidium monnieri using UHPLC-ESIQ-TOF/MS[J]. Chinese Herbal Medicines,2016,8(4):323-330.
[9]冯倩倩,陈飞,安靖霏,等. HPLC法测定苯酚消毒液和复方薄荷脑醑中苯酚的含量[J].实用药物与临床,2016,19(12):1523-1525.
[10]中国药典2015年版.四部[S]. 2015:57,63.
[11]贾善学,赵卫,史保荣,等.《卫生部药品标准》中药成方制剂收载情况分析[J].中国药品标准,2002,3(3):18-19.
[12]孙国祥,陈新新,孙万阳,等.中药标准制剂控制模式发展历程和构建全质量关控制中药质量模式[J].中南药学,2014,12(1):1-9.
[13]Gao FY,Hu YS,Ye XL,et al. Optimal extraction and fingerprint analysis of Cnidii fructus by accelerated solvent extraction and high performance liquid chromatographic analysis with photodiode array and mass spectrometry detections[J]. Food Chem,2013,141(3):1962-1971.
[14]Li YM,JiaM,LiHQ,etal.Cnidiummonnieri:A review of traditional uses,phytochemical and ethnopharmacological properties[J]. Am J Chinese Med,2015,43(5):835-877.
[15]韩希英.升华硫的药用经验及开发初探[J].药学实践杂志,2003,21(2):117.
[16]栗建明,袁震霆,张彤,等.气相色谱法测定舒筋理伤油中4种有效成分的含量[J].中南药学,2015,13(10):1086-1089.
[17]尚坤,李敬文,常美月,等.冰片化学成分及药理作用研究[J].吉林中医药,2018,38(1):93-95.