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作 者:魏江存 谢臻 杨正腾[3] 马家宝[3] 秦祖杰 王成龙 黄冬美 朱文润 陈圣斌 韩倩 WEI Jiangcun;XIE Zhen;YANG Zhengteng;MA Jiabao;QIN Zujie;WANG Chenglong;HUANG Dongmei;ZHU Wenrun;CHEN Shengbin;HAN Qian(Zhuangyao Pharmaceutical Research and Development Center,Guangxi International Zhuang Medical Hospital,Nanning 530201,China;School of Pharmacy,Guangxi University of TCM,Nanning 530200,China;Dept.of Pharmacy,the First Affiliated Hospital of Guangxi University of TCM,Nanning 530023,China;School of Pharmacy,Sun Yat-sen University,Guangzhou 510275,China)
机构地区:[1]广西国际壮医医院壮瑶药研发中心,南宁530201 [2]广西中医药大学药学院,南宁530200 [3]广西中医药大学第一附属医院药学部,南宁530023 [4]中山大学药学院,广州510275
出 处:《中国药房》2019年第22期3053-3056,共4页China Pharmacy
基 金:国家自然科学基金资助项目(No.81360524、81660659);国家中医药管理局中医药科研实验室项目(No.国中医药发〔2009〕21号);广西高校中青年教师科研基础能力提升项目(No.2019KY0341)
摘 要:目的:建立同时测定3种不同大黄炮制品中没食子酸、桂皮酸、儿茶素含量的方法。方法:采用反相高效液相色谱法。色谱柱为Thermo Scientific^TM Hypersil GOLD Dim,流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),检测波长为278 nm,流速为1.0 mL/min,柱温为30℃,进样量为10μL。结果:没食子酸、桂皮酸、儿茶素的检测进样量线性范围分别为0.1262~1.2620μg(r=0.9999)、0.0362~0.3620μg(r=0.9999)、0.1779~1.7794μg(r=0.9998);定量限分别为25.4、28.2、62.5 ng,检测限分别为6.2、3.6、11.8 ng;精密度、稳定性、重复性、耐用性试验的RSD均小于3%;加样回收率分别为94.64%~102.71%(RSD=2.74%,n=9)、95.35%~102.49%(RSD=2.44%,n=9)、93.65%~103.66%(RSD=3.27%,n=9)。含量测定结果显示,熟大黄中没食子酸、桂皮酸含量较高,两种成分含量大小顺序均依次为熟大黄>水蒸熟大黄>生大黄;生大黄中儿茶素含量较高,该成分含量大小顺序依次为生大黄>水蒸熟大黄>熟大黄。结论:本方法灵敏、可靠、重复性好,可用于同时测定3种不同大黄炮制品中没食子酸、桂皮酸和儿茶素的含量。OBJECTIVE:To establish a method for simultaneous determination of gallic acid,cinnamic acid and catechin in 3 processed products of Rheum officinale.METHODS:RP-HPLC method was established.The determination was performed on Thermo Scientific^TM Hypersil GOLD Dim column with mobile phase consisted of methanol-0.1%phosphoric acid solution(gradient elution)at the flow rate of 1.0 mL/min.The detection wavelength was set at 278 nm,and the column temperature was 30℃.The sample size was 10μL.RESULTS:The linear range of gallic acid,cinnamic acid and catechin were 0.1262-1.2620μg(r=0.9999),0.0362-0.3620μg(r=0.9999)and 0.1779-1.7794μg(r=0.9998),respectively.Quantitative limits were 25.4,28.2,62.5 ng,and detection limits were 6.2,3.6,11.8 ng,respectively.RSDs of precision,stability,repeatability and durability tests were all less than 3%.The recoveries ranged from 94.64%-102.71%(RSD=2.74%,n=9),95.35%-102.49%(RSD=2.44%,n=9),93.56%-103.66%(RSD=3.27%,n=9).The determination results showed that the contents of gallic acid and cinnamic acid in prepared R.officinale were higher,and the order of both were prepared R.officinale>steamed R.officinale>raw R.officinale.The content of catechin in raw R.officinale was higher,and the order of it was raw R.officinale>steamed R.officinale>prepared R.officinale.CONCLUSIONS:The method is sensitive,reliable and reproducible.It can be used to determine the contents of gallic acid,cinnamic acid and catechins in 3 processed products of R.officinale simultaneously.
关 键 词:大黄 炮制品 没食子酸 桂皮酸 儿茶素 反相高效液相色谱法 含量测定
分 类 号:R917[医药卫生—药物分析学]
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