黄花油点草药材的质量标准研究
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摘要
目的:建立黄花油点草药材的质量标准。方法:参照2015年版《中国药典》方法对药材样品的性状、显微结构进行鉴别,对其水分、灰分及浸出物进行检查;采用薄层色谱法(TLC)对药材样品中槲皮素、烟花苷进行定性鉴别;采用高效液相色谱法测定药材样品中葛根素、对羟基苯甲酸、烟花苷、阿魏酸、槲皮素、山柰酚的含量。结果:性状、显微鉴别具有专属性;槲皮素、烟花苷的TLC图斑点清晰,分离度好,阴性对照无干扰;10批药材样品水分含量范围为0.61%～1.89%,总灰分含量范围为6.28%～8.88%,酸不溶性灰分含量范围为0.76%～1.79%,醇溶性浸出物含量范围为1.31%～2.00%,水溶性浸出物含量范围为9.39%～14.27%。葛根素、对羟基苯甲酸、烟花苷、阿魏酸、槲皮素、山柰酚检测进样量线性范围分别为0.031 92～0.111 7μg(r=0.999 6)、0.085 3～0.298 5μg(r=0.999 5)、0.010 76～0.037 66μg(r=0.999 8)、0.070 08～0.245 3μg(r=0.999 8)、0.058 56～0.205 0μg(r=0.999 4)、0.009 860～0.033 88μg(r=0.999 4);定量限分别为1.06、0.47、0.75、1.40、1.20、0.74 ng,检测限分别为0.36、0.12、0.30、0.53、0.60、0.31 ng;精密度、稳定性、重复性试验的RSD均小于2%;平均加样回收率分别为101.54%、102.10%、101.46%、103.35%、99.36%、96.85%,RSD分别为1.76%、1.68%、1.56%、1.26%、0.91%、1.96%(n=6);样品含量分别为0.017～0.047、0.042～0.140、0.003 8～0.015 0、0.049～0.180、0.024～0.091、0.003 9～0.011 0 mg/g。结论:所建质量标准可用于黄花油点草的质量控制。
OBJECTIVE:To establish the quality standard of Tricyrtis maculata. METHODS:The character and microstructure of T. maculata were identified according to the method stated in 2015 edition of Chinese Pharmacopoeia. The contents of moisture,ash and extract were determined. TLC was used for qualitative identification of quercetin and nicotifiorin in samples. The contents of puerarin,p-hydroxybenzoic acid,nicotiflorin,ferulic acid,quercetin and kaempferol were determined by HPLC. RESULTS:The characters and microscopic identification had specificity. TLC spots of quercetin and nicotifiorin were clear and well-separated without interference from negative control. The water content,total ash content,acid insoluble ash content,alcohol soluble extract and water soluble extract for 10 batches of samples were 0.61%-1.89%,6.28%-8.88%,0.76%-1.79%,1.31%-2.00% and 9.39%-14.27%,respectively. The linear range of puerarin,p-hydroxybenzoic acid,nicotiflorin,ferulic acid,quercetin and kaeniphenol were 0.031 92-0.111 7 μg(r=0.999 6),0.085 3-0.298 5 μg(r=0.999 5),0.010 76-0.037 66 μg(r=0.999 8),0.070 08-0.245 3μg(r=0.999 8),0.058 56-0.205 0 μg(r=0.999 4),0.009 860-0.033 88 μg(r=0.999 4),respectively. The quantitation limits were 1.06,0.47,0.75,1.40,1.20,0.74 ng,and the detection limits were 0.36,0.12,0.30,0.53,0.60,0.31 ng,respectively.RSDs of precision,stability and repeatability tests were all less than 2%. The average recoveries were 101.54%,102.10%,101.46%,103.35%,99.36% and 96.85%,respectively;RSDs were 1.76%,1.68%,1.56%,1.26%,0.91% and 1.96%,respectively(n=6);the results of the content were 0.017-0.047,0.042-0.140,0.003 8-0.015 0,0.049-0.180,0.024-0.091,0.0039-0.011 0 mg/g. CONCLUSIONS:The established quality standard can be used for the quality control of T. maculata.
OBJECTIVE:To establish the quality standard of Tricyrtis maculata. METHODS:The character and microstructure of T. maculata were identified according to the method stated in 2015 edition of Chinese Pharmacopoeia. The contents of moisture,ash and extract were determined. TLC was used for qualitative identification of quercetin and nicotifiorin in samples. The contents of puerarin,p-hydroxybenzoic acid,nicotiflorin,ferulic acid,quercetin and kaempferol were determined by HPLC. RESULTS:The characters and microscopic identification had specificity. TLC spots of quercetin and nicotifiorin were clear and well-separated without interference from negative control. The water content,total ash content,acid insoluble ash content,alcohol soluble extract and water soluble extract for 10 batches of samples were 0.61%-1.89%,6.28%-8.88%,0.76%-1.79%,1.31%-2.00% and 9.39%-14.27%,respectively. The linear range of puerarin,p-hydroxybenzoic acid,nicotiflorin,ferulic acid,quercetin and kaeniphenol were 0.031 92-0.111 7 μg(r=0.999 6),0.085 3-0.298 5 μg(r=0.999 5),0.010 76-0.037 66 μg(r=0.999 8),0.070 08-0.245 3μg(r=0.999 8),0.058 56-0.205 0 μg(r=0.999 4),0.009 860-0.033 88 μg(r=0.999 4),respectively. The quantitation limits were 1.06,0.47,0.75,1.40,1.20,0.74 ng,and the detection limits were 0.36,0.12,0.30,0.53,0.60,0.31 ng,respectively.RSDs of precision,stability and repeatability tests were all less than 2%. The average recoveries were 101.54%,102.10%,101.46%,103.35%,99.36% and 96.85%,respectively;RSDs were 1.76%,1.68%,1.56%,1.26%,0.91% and 1.96%,respectively(n=6);the results of the content were 0.017-0.047,0.042-0.140,0.003 8-0.015 0,0.049-0.180,0.024-0.091,0.0039-0.011 0 mg/g. CONCLUSIONS:The established quality standard can be used for the quality control of T. maculata.
引文
[1]孙静,寇文龙,刘文文,等.陕产黄花油点草的生药鉴别[J].中药材,2012,35(5):717-719.
[2]孙静,刘洁琼,张丽梅.陕产黄花油点草化学成分初步研究[J].陕西中医,2012,33(5):605-606.
[3]杨洁,张东东,张欣,等.黄花油点草化学成分研究[J].中南药学,2017,15(7):922-924.
[4]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,2015:299.
[5]王晓飞,于玲,杜华霜,等.三白草中槲皮素的薄层色谱鉴别[J].中国民族民间医药,2010,19(23):61、64.
[6]王祥培,许士娜,吴红梅,等.天胡荽药材中槲皮素的薄层鉴别与含量测定[J].时珍国医国药,2010,21(1):44-45.
[7]盛萍,帕丽达·阿不力孜,张烃,等.维吾尔药睡莲花中烟花苷的含量测定[J].中药材,2006,29(12):1313-1314.
[8]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:104、202、204.
[9]肖楠,王路宏,赵磊. HPLC法测定五味子膏中葛根素的含量[J].中国药物评价,2018,35(4):267-270.
[10]昝珂,黄莉莉,刘杰,等. HPLC法同时测定民族药材青阳参中6种酚类成分的含量[J].药物分析杂志,2017,37(8):1447-1452.
[11]宋敏,李晨阳,谭为,等.雪白睡莲花中烟花苷的提取工艺研究[J].食品研究与开发,2016,37(9):128-131.
[12]曹晓华,沈旭斌,程先骄,等.HPLC双波长法测定豌豆尖中槲皮素和山柰酚的含量[J].食品科技,2017,42(4):270-276.
[13]高松红,单柏宇,徐阳,等. HPLC法同时测定五加生化胶囊中阿魏酸和槲皮素的含量[J].长春师范大学学报,2018,37(6):112-116.
[14]孙静,何晓娟,刘洁琼. HPLC法测定陕西产黄花油点草中烟花苷的含量[J].中国药房,2015,26(9):1246-1247.
[15]罗慧玉,闫伟伟,曾春萍,等. HPLC法同时测定杏花中阿魏酸、芦丁和异槲皮苷[J].实用药物与临床,2017,20(6):701-704.
[16]曲艳丽,刘治民,孙冶,等.山紫菀药材的质量标准研究[J].中国药房,2018,29(8):1057-1060.
[17]林海霞.竹叶柴胡的质量研究[D].成都:成都中医药大学,2012.
[18]贾田芊,王媚,崔春丽,等.超高效液相色谱指纹图谱快速测定复方丹参片与复方丹参滴丸活性成分[J].医药导报,2018,37(10):1241-1246.
[19]贾田芊,王媚,李兴欢,等.复方丹参方快速UPLC指纹图谱研究[J].中国医院药学杂志,2018,38(5):474-477、495.
[2]孙静,刘洁琼,张丽梅.陕产黄花油点草化学成分初步研究[J].陕西中医,2012,33(5):605-606.
[3]杨洁,张东东,张欣,等.黄花油点草化学成分研究[J].中南药学,2017,15(7):922-924.
[4]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,2015:299.
[5]王晓飞,于玲,杜华霜,等.三白草中槲皮素的薄层色谱鉴别[J].中国民族民间医药,2010,19(23):61、64.
[6]王祥培,许士娜,吴红梅,等.天胡荽药材中槲皮素的薄层鉴别与含量测定[J].时珍国医国药,2010,21(1):44-45.
[7]盛萍,帕丽达·阿不力孜,张烃,等.维吾尔药睡莲花中烟花苷的含量测定[J].中药材,2006,29(12):1313-1314.
[8]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:104、202、204.
[9]肖楠,王路宏,赵磊. HPLC法测定五味子膏中葛根素的含量[J].中国药物评价,2018,35(4):267-270.
[10]昝珂,黄莉莉,刘杰,等. HPLC法同时测定民族药材青阳参中6种酚类成分的含量[J].药物分析杂志,2017,37(8):1447-1452.
[11]宋敏,李晨阳,谭为,等.雪白睡莲花中烟花苷的提取工艺研究[J].食品研究与开发,2016,37(9):128-131.
[12]曹晓华,沈旭斌,程先骄,等.HPLC双波长法测定豌豆尖中槲皮素和山柰酚的含量[J].食品科技,2017,42(4):270-276.
[13]高松红,单柏宇,徐阳,等. HPLC法同时测定五加生化胶囊中阿魏酸和槲皮素的含量[J].长春师范大学学报,2018,37(6):112-116.
[14]孙静,何晓娟,刘洁琼. HPLC法测定陕西产黄花油点草中烟花苷的含量[J].中国药房,2015,26(9):1246-1247.
[15]罗慧玉,闫伟伟,曾春萍,等. HPLC法同时测定杏花中阿魏酸、芦丁和异槲皮苷[J].实用药物与临床,2017,20(6):701-704.
[16]曲艳丽,刘治民,孙冶,等.山紫菀药材的质量标准研究[J].中国药房,2018,29(8):1057-1060.
[17]林海霞.竹叶柴胡的质量研究[D].成都:成都中医药大学,2012.
[18]贾田芊,王媚,崔春丽,等.超高效液相色谱指纹图谱快速测定复方丹参片与复方丹参滴丸活性成分[J].医药导报,2018,37(10):1241-1246.
[19]贾田芊,王媚,李兴欢,等.复方丹参方快速UPLC指纹图谱研究[J].中国医院药学杂志,2018,38(5):474-477、495.