HPLC-DAD同时测定藏药洁白丸中4种成分的含量
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摘要
目的:建立同时测定藏药洁白丸中没食子酸、丁香酚、土木香内酯、异土木香内酯含量的方法。方法:采用高效液相色谱法。色谱柱为CAPCELL PAK MGⅡC18,流动相为甲醇-乙腈-0.2%磷酸溶液(梯度洗脱),流速为0.8 m L/min,检测波长为220 nm(土木香内酯、异土木香内酯)和280 nm(没食子酸、丁香酚),柱温为30℃,进样量为10μL。结果:没食子酸、丁香酚、土木香内酯、异土木香内酯检测质量浓度线性范围分别为46.50～2 325.00、21.28～1 064.00、4.38～219.20、4.17～208.40μg/m L(r均≥0.999 1),检测限分别为0.26、0.09、0.28、0.35μg/m L,定量限分别为0.74、0.25、0.95、1.06μg/m L;精密度、稳定性(48 h)、重复性试验的RSD均≤2.0%(n=6或n=7),加样回收率分别为98.5%、97.6%、97.1%、101.6%,RSD分别为1.4%、1.9%、1.6%、1.7%(n=6);6批洁白丸样品中没食子酸、丁香酚、土木香内酯、异土木香内酯含量范围分别为4.28～7.02、1.09～4.90、0.25～0.60、0.30～0.72 mg/g。结论:建立的方法可用于藏药洁白丸中没食子酸、丁香酚、土木香内酯、异土木香内酯含量的同时测定。
OBJECTIVE:To establish a method for content determination of gallic acid,eugenol,alantolatone and isoalantolactone in Tibetan medicine Jiebai pills simultaneously. METHODS: HPLC method was adopted. The separation was performed on CAPCELL PAK MGⅡ C18 column with of mobile phase composed of methanol-acetonitrile-0.2% phosphoric acid solution(gradient elution)at the flow rate of 0.8 m L/min. The detection wavelengths were 220 nm for alantolatone and isoalantolactone,280 nm for gallic acid and eugenol. The column temperature was at 30 ℃,and sample size was 10 μL. RESULTS:The linear ranges of gallic acid,eugenol,alantolatone and isoalantolactone were 46.50-2 325.00,21.28-1 064.00,4.38-219.20 and 4.17-208.40 μg/m L,respectively(all r≥0.999 1). The limits of detection were 0.26,0.09,0.28,0.35 μg/m L,and the limits of quantitation were 0.74,0.25,0.95,1.06 μg/m L,respectively. RSDs of precision,stability(48 h)and reproducibility tests were all lower than 2.0%(n=6 or n=7). The recoveries were 98.5%,97.6%,97.1% and 101.6%,and RSDs were 1.4%,1.9%,1.6%,1.7%(n=6),respectively. The content of gallic acid,eugenol,alantolatone and isoalantolactone in 6 batches of Baijie pills were 4.28-7.02,1.09-4.90, 0.25-0.60, 0.30-0.72 mg/g, respectively. CONCLUSIONS: The established method can be used for content determination of gallic acid,eugenol,alantolatone and isoalantolactone in Tibetan medicine Jiebai pills simultaneously.
OBJECTIVE:To establish a method for content determination of gallic acid,eugenol,alantolatone and isoalantolactone in Tibetan medicine Jiebai pills simultaneously. METHODS: HPLC method was adopted. The separation was performed on CAPCELL PAK MGⅡ C18 column with of mobile phase composed of methanol-acetonitrile-0.2% phosphoric acid solution(gradient elution)at the flow rate of 0.8 m L/min. The detection wavelengths were 220 nm for alantolatone and isoalantolactone,280 nm for gallic acid and eugenol. The column temperature was at 30 ℃,and sample size was 10 μL. RESULTS:The linear ranges of gallic acid,eugenol,alantolatone and isoalantolactone were 46.50-2 325.00,21.28-1 064.00,4.38-219.20 and 4.17-208.40 μg/m L,respectively(all r≥0.999 1). The limits of detection were 0.26,0.09,0.28,0.35 μg/m L,and the limits of quantitation were 0.74,0.25,0.95,1.06 μg/m L,respectively. RSDs of precision,stability(48 h)and reproducibility tests were all lower than 2.0%(n=6 or n=7). The recoveries were 98.5%,97.6%,97.1% and 101.6%,and RSDs were 1.4%,1.9%,1.6%,1.7%(n=6),respectively. The content of gallic acid,eugenol,alantolatone and isoalantolactone in 6 batches of Baijie pills were 4.28-7.02,1.09-4.90, 0.25-0.60, 0.30-0.72 mg/g, respectively. CONCLUSIONS: The established method can be used for content determination of gallic acid,eugenol,alantolatone and isoalantolactone in Tibetan medicine Jiebai pills simultaneously.
引文
[1]才让措,郭登海.藏药“智托洁白丸”功能主治及方解浅述[J].中国民族民间医药,2012,21(18):9.
[2]陈来.藏药洁白丸简介[J].河南中医,2012,32(10):1371.
[3]卓玛草.浅析关于“拉卜楞洁白丸”独具特色的方剂组成及临床应用[J].西藏科技,2015(10):47-48.
[4]包桂芬.藏药“洁白丸”主要药物分析[J].甘肃中医学院学报,1996,13(4):50-51.
[5]李玉宝,华尔老.藏药洁白丸治疗胃溃疡[J].中国民族医药杂志,1999,5(1):36.
[6]苏雅拉图.蒙药洁白丸治疗慢性胰腺炎疗效分析[J].临床医药文献杂志,2018,5(17):161-162.
[7]尕藏久美.藏药洁白丸(日格尔)治疗胆汁返流性胃炎56例[J].中国民族医药杂志,2004,10(1):7.
[8]黄平,毛坤军,叶颖俊.HPLC法同时测定胃肠宁片中5个活性成分含量[J].药物分析杂志,2017,37(8):1530-1534.
[9]仇朝红,魏玉海,李文渊.藏药智托洁白丸中没食子酸的定性与定量检测[J].郑州大学学报(医学版),2012,47(1):88-91.
[10]余小平.RP-HPLC法测定中药丁香中丁香酚的含量[J].中华中医药学刊,2009,27(4):880-881.
[11]纪松岗,金柔男,赵亮,等.用HPLC法同时测定六味安消胶囊中土木香内酯、异土木香内酯、大黄素和大黄酚的含量[J].药学服务与研究,2008,8(6):446-449.
[12]倪琳,杨锡.HPLC法同时测定达斯玛保丸中木香烃内酯、异土木香内酯和土木香内酯[J].中成药,2012,34(4):664-666.
[13]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,2015:1290-1291.
[14]陈静,索朗次仁,石云,等.藏药土木香化学成分、药理活性及其藏药方的研究进展[J].西部中医药,2017,30(10):137-138.
[15]杨雁.诃子化学成分、生物活性及分析方法研究进展[J].西藏科技,2016(9):34-39.
[16]臧亚茹.丁香及其有效成分药理作用的实验研究[J].承德医学院学报,2007,24(1):71-73.
[17]朱小牧,马静,王曙.HPLC测定藏木香中的内酯类成分[J].华西药学杂志,2014,29(1):100-101.
[18]陈瑞生.RP-HPLC法测定藏成药智托洁白丸中没食子酸的含量[J].陕西中医,2007,28(12):1679-1681.
[19]曹伟宇,贺文娟,雷丸,等.HPLC法同时测定干髓糊剂中丁香酚和麝香草酚的含量[J].中国药房,2017,28(30):4268-4271.
[20]康慧,刘亚蓉.HPLC法同时测定六味能消丸中8种成分的含量[J].中国药房,2017,28(24):3433-3436.
[2]陈来.藏药洁白丸简介[J].河南中医,2012,32(10):1371.
[3]卓玛草.浅析关于“拉卜楞洁白丸”独具特色的方剂组成及临床应用[J].西藏科技,2015(10):47-48.
[4]包桂芬.藏药“洁白丸”主要药物分析[J].甘肃中医学院学报,1996,13(4):50-51.
[5]李玉宝,华尔老.藏药洁白丸治疗胃溃疡[J].中国民族医药杂志,1999,5(1):36.
[6]苏雅拉图.蒙药洁白丸治疗慢性胰腺炎疗效分析[J].临床医药文献杂志,2018,5(17):161-162.
[7]尕藏久美.藏药洁白丸(日格尔)治疗胆汁返流性胃炎56例[J].中国民族医药杂志,2004,10(1):7.
[8]黄平,毛坤军,叶颖俊.HPLC法同时测定胃肠宁片中5个活性成分含量[J].药物分析杂志,2017,37(8):1530-1534.
[9]仇朝红,魏玉海,李文渊.藏药智托洁白丸中没食子酸的定性与定量检测[J].郑州大学学报(医学版),2012,47(1):88-91.
[10]余小平.RP-HPLC法测定中药丁香中丁香酚的含量[J].中华中医药学刊,2009,27(4):880-881.
[11]纪松岗,金柔男,赵亮,等.用HPLC法同时测定六味安消胶囊中土木香内酯、异土木香内酯、大黄素和大黄酚的含量[J].药学服务与研究,2008,8(6):446-449.
[12]倪琳,杨锡.HPLC法同时测定达斯玛保丸中木香烃内酯、异土木香内酯和土木香内酯[J].中成药,2012,34(4):664-666.
[13]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,2015:1290-1291.
[14]陈静,索朗次仁,石云,等.藏药土木香化学成分、药理活性及其藏药方的研究进展[J].西部中医药,2017,30(10):137-138.
[15]杨雁.诃子化学成分、生物活性及分析方法研究进展[J].西藏科技,2016(9):34-39.
[16]臧亚茹.丁香及其有效成分药理作用的实验研究[J].承德医学院学报,2007,24(1):71-73.
[17]朱小牧,马静,王曙.HPLC测定藏木香中的内酯类成分[J].华西药学杂志,2014,29(1):100-101.
[18]陈瑞生.RP-HPLC法测定藏成药智托洁白丸中没食子酸的含量[J].陕西中医,2007,28(12):1679-1681.
[19]曹伟宇,贺文娟,雷丸,等.HPLC法同时测定干髓糊剂中丁香酚和麝香草酚的含量[J].中国药房,2017,28(30):4268-4271.
[20]康慧,刘亚蓉.HPLC法同时测定六味能消丸中8种成分的含量[J].中国药房,2017,28(24):3433-3436.