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【作者】 闫广利; 王喜军; 吕海涛; 孙文军;【Author】 YAN Guang-li,WANG Xi-jun,LV Hai-tao,et al Research Institute of TCM,Heilongjiang University of TCM,Harbin 150040,Heilongjiang,China【机构】 黑龙江中医药大学中医药研究院; 黑龙江中医药大学药学院; 黑龙江中医药大学药学院 黑龙江哈尔滨150040; 黑龙江哈尔滨150040;【摘要】 目的:建立同时测定茵陈蒿汤中绿原酸、京尼平苷、6,7-二甲氧基香豆素、茵陈色原酮和大黄酸5个有效成分的HPLC方法,考察药材不同配伍对其溶出率的影响。方法:采用HPLC方法测定茵陈蒿汤不同配伍水煎液冻干粉中5个成分的含量,色谱柱为Diamonsil○R(钻石)C18柱,流动相为乙腈-0.1%磷酸水溶液梯度洗脱,以二极管阵列检测器在200~400nm范围内全波长检测。结果:建立的茵陈蒿汤中5个成分同时测定的HPLC方法准确、快速、重现性好。所测5个成分中,6,7-二甲氧基香豆素、茵陈色原酮和绿原酸溶出率变化不大,京尼平苷和大黄酸的溶出率在配伍茵陈蒿后明显降低。结论:茵陈蒿汤主要有效成分可能存在一定的有效比例。 更多还原【Abstract】 Object:To establish a HPLC method of determining simultaneously 6,7-dimethylesculetin,capillarisin,chlorogenic acid,geniposide and rhein in different combinations of Yinchenhao decoction to investigate their dissolution rates.Method:The contents of 5 active components were determined by RP-HPLC with a diamonsil C18 column,mobile phase of acetonitrile-0.1% phosphoric acid solution gradient elution and DAD detector at the wavelength of 200-400nm.Result:The RP-HPLC method is accurate,fast and its r... 更多还原【关键词】 茵陈蒿汤; 溶出率; 配伍; 同时测定; 【Key words】 Yinchenhao decoction; main active components; RP-HPLC; compatibility; 【基金】 国家重大基础研究发展计划(973计划);资助项目(2005CB523406)http://ng1.17img.cn/bbsfiles/images/2012/08/201208071036_382138_2352694_3.jpg
[align=center][font='times new roman'][size=18px]绵茵陈[/size][/font][font='times new roman'][size=18px]药材中[/size][/font][font='times new roman'][size=18px]绿原酸[/size][/font][font='times new roman'][size=18px]测定[/size][/font][/align][font='tahoma'][size=14px]小记:[/size][/font][font='tahoma'][size=14px]茵陈根据采收季节不同分为绵茵陈和花茵陈,[/size][/font][font='tahoma'][size=14px][color=#000000]春季采收的习称“绵茵陈”,秋季釆割的称“花茵陈”。[/color][/size][/font][align=center][img=,286,197]https://ng1.17img.cn/bbsfiles/images/2022/11/202211301559260524_4770_1858223_3.jpg!w286x197.jpg[/img][/align][font='times new roman']1 [/font][font='times new roman']材料与试剂[/font][font='times new roman']乙腈(色谱级[/font][font='times new roman'] [/font][font='times new roman']上海安谱[/font][font='times new roman'])、[/font][font='times new roman']乙醇[/font][font='times new roman'],磷酸[/font][font='times new roman'](分析纯[/font][font='times new roman'],北京化工厂[/font][font='times new roman'])、[/font][font='times new roman']绿原酸[/font][font='times new roman']标准品[/font][font='times new roman'](购自中检院)、[/font][font='times new roman']绵茵陈[/font][font='times new roman']药材[/font][font='times new roman']样品(送检样品)。[/font][font='times new roman']2 [/font][font='times new roman']色谱条件[/font][font='times new roman']LC-20AT[/font][font='times new roman'][url=https://insevent.instrument.com.cn/t/5p][color=#3333ff]液相色谱仪[/color][/url](日本岛津),色谱柱:[/font][font='times new roman'] [/font][font='times new roman']Eclipse XDB [/font][font='times new roman']C18(250mm*4.6μm*5μm)[/font][font='times new roman'](安捷伦),流动相:以乙腈[/font][font='times new roman']-[/font][font='times new roman']磷酸[/font][font='times new roman']水[/font][font='times new roman']等度[/font][font='times new roman']洗脱[/font][font='times new roman']([/font][font='times new roman']10:90[/font][font='times new roman'])[/font][font='times new roman'];柱温[/font][font='times new roman']35[/font][font='times new roman'] [/font][font='宋体']℃[/font][font='times new roman']。[/font][font='times new roman']检测波长为[/font][font='times new roman']327[/font][font='times new roman']nm[/font][font='times new roman'],[/font][font='times new roman'] [/font][font='times new roman']3[/font][font='times new roman']溶液制备[/font][font='times new roman'](按照中国药典[/font][font='times new roman']2[/font][font='times new roman']020[/font][font='times new roman']年版一部[/font][font='times new roman']茵陈[/font][font='times new roman']项下[/font][font='times new roman']绵茵陈[/font][font='times new roman']测定)[/font][font='times new roman'] 对照品溶液的制备[/font][font='times new roman'] [/font][font='times new roman']取绿原酸对照品适量,精密称定,置棕色量瓶中,加[/font][font='times new roman']50%[/font][font='times new roman']甲醇制成每[/font][font='times new roman']1m[/font][font='times new roman']L[/font][font='times new roman']含[/font][font='times new roman']40[/font][font='times new roman']μ[/font][font='times new roman']g[/font][font='times new roman']的溶液,即得。[/font][font='times new roman'] [/font][font='times new roman'] [/font][align=center][img=,569,114]https://ng1.17img.cn/bbsfiles/images/2022/11/202211301556348147_9251_1858223_3.jpg!w569x114.jpg[/img][/align][align=center]绿原酸标准品色谱图[font='times new roman'] [/font][/align][font='times new roman']样[/font][font='times new roman']品溶液的制备[/font][font='times new roman'] [/font][font='times new roman']取本品粉末(过二号筛)约[/font][font='times new roman']1g[/font][font='times new roman'],精密称定,置具塞锥形瓶中,精密加入[/font][font='times new roman']50%[/font][font='times new roman']甲醇[/font][font='times new roman']50m[/font][font='times new roman']L[/font][font='times new roman'],称定重量,超声处理(功率[/font][font='times new roman']180W[/font][font='times new roman'],频率[/font][font='times new roman']42kHz[/font][font='times new roman'])[/font][font='times new roman']30[/font][font='times new roman']分钟,放冷,再称定重量,用[/font][font='times new roman']50%[/font][font='times new roman']甲醇补足减失的重量,摇匀,离心,精密量取上清液[/font][font='times new roman']5m[/font][font='times new roman']L[/font][font='times new roman'],置[/font][font='times new roman']25m[/font][font='times new roman']L[/font][font='times new roman']棕色量瓶中,加[/font][font='times new roman']50%[/font][font='times new roman']甲醇至刻度,摇匀,滤过,取续滤液,即得。[/font][font='times new roman'] [/font][font=&][/font][align=center][img=,545,123]https://ng1.17img.cn/bbsfiles/images/2022/11/202211301556581714_1632_1858223_3.jpg!w545x123.jpg[/img][/align][font='times new roman'][/font][align=center][font=微软雅黑, sans-serif]绵茵陈样品中绿原酸色谱图[/font][/align][font=&]结论:[/font]客户送检样品绵茵陈中绿原酸含量为[font='times new roman']0.85%[/font][font='times new roman'] [/font][font='times new roman'] [/font][font='times new roman']注:[/font][font='times new roman']①茵陈的分类不一样测定的主要成分指标也不同,绵茵陈测定的为绿原酸,而花茵陈测定的指标成分为[/font][font='times new roman']滨蒿内酯[/font][font='times new roman'],测试之前一定要明确其种类,防止检测错误。[/font][font='times new roman']②绵茵陈在粉碎过程会有一定的绒,要剪碎粉碎完全再过筛。[/font]
茵陈为菌科植物, 茵陈蒿的干燥幼苗 ,能清热利湿 ,退黄疸。用于黄疸型肝炎和传染性肝炎、胆道感染、胆石症等 , 具有解热利胆利尿 ,平滑肌等作用。本文用蒸馏水浸泡提取,用乙醚提取挥发成分进行气相色谱一质谱 (GC-MS) 联用分析 , 为茵陈临床合理用药,提供了实验依据。