HPLC法比较3种土大黄中游离蒽醌和总蒽醌的含量  

Determination of free and total anthraquinones in 3 kinds of Rumex by HPLC:a comparative study

作　　者：杨娟艳 王珍珍[3] 茅向军[2] 许乾丽[2] 林瑞超[4] 戴忠[4] YANG juan-yan WANG Zhen-zhen MAO Xlang-jun XU Qian-li LIN Rui-chao DAI Zhong(Guiyang College of Traditional Chinese Medicine, Guiyang 550002, Chin Guizhou Provincial of Food and Drug Inspection Institute, Guiyang 550004, China Guizhou Medical University, Guiyang 550004, China National Institute For Food and Drug Control, Beijing 100050, China)

机构地区：[1]贵阳中医学院,贵阳550002 [2]贵州省食品药品检验所,贵阳550004 [3]贵州医科大学,贵阳550004 [4]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2017年第4期615-623,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：贵州省中药现代化科技产业研究开发专项(黔科合社字[2009]5003号)

摘　　要：目的:建立HPLC测定方法,比较贵州土大黄尼泊尔酸模(Rumex nepalensis Spreng.)、齿果酸模(Rumex dentatus Linn.)或羊蹄(Rumex crispus Linn.)中游离蒽醌和总蒽醌(以大黄素、大黄酚和大黄素甲醚的总量计)的含量。方法:采用Diamonsil C_(18)(4.6 mm×200 mm,5μm)色谱柱,以甲醇-0.1%磷酸溶液(83∶17)为流动相,流速1 m L·min^(-1),检测波长254 nm,柱温30℃。结果:大黄素、大黄酚、大黄素甲醚进样量分别在9.670~522.2 ng(r=0.999 9)、18.06~975.2 ng(r=0.999 9)、7.390~399.1 ng(r=0.999 9)范围内线性关系良好;游离蒽醌中大黄素、大黄酚、大黄素甲醚的平均回收率分别为102.6%(RSD=1.5%)、102.5%(RSD=0.80%)、97.4%(RSD=1.1%),总蒽醌中大黄素、大黄酚、大黄素甲醚的平均回收率分别为100.5%(RSD=1.2%)、97.4%(RSD=1.6%)、98.6%(RSD=1.7%)。游离蒽醌中大黄素、大黄酚和大黄素甲醚的含量分别在0.008%~0.088%、0.007%~0.289%、0.007%~0.103%范围内;总蒽醌中大黄素、大黄酚和大黄素甲醚的含量分别在0.034%~0.244%、0.076%~0.856%和0.030%~0.297%范围内。结论:结合蒽醌含量最高的是羊蹄,齿果酸模、尼泊尔酸模和未鉴定的9批样品次之,且羊蹄和齿果酸模中结合蒽醌含量均大于游离蒽醌含量。Objective： To establish an HPLC method to compare the contents of free and total anthraquinones （ total amount of emodin, chrysophanol and ararobinol ） in Rumex nepalensis Spreng, Rumex dentatus Linn and Rumex crispus Linn from Guizhou. Methods： The HPLC method was performed on a Diamonsil Cls column （ 4.6 mm × 200 mm, 5 μm ）with the mobile phase consisting of methanol-0. 1% phosphoric acid （ 83：17 ）at the flow rate of 1 mL· min^-1. The detection wavelength was set at 254 nm and the column temperature was 30 ℃. Results： Emodin, chrysophanol and ararobinol revealed a good linear relationship in the range of 9.670-522.2 ng （ r=-0.999 9 ）, 18.06-975.2 ng （ r=-0.999 9 ） and 7.390-399.1 ng （ r=-0.999 9 ）, respectively. The recoveries of emodin, chrysophanol and ararobinol in total anthraquinones were 102.6% （ RSD=1.5% ）, 102.5% （ RSD=0.80% ）and 97.4% （ RSD=1.1% ）, respectively and the recoveries of emodin, chrysophanol and ararobinol in free anthraquinones were 100.5% （ RSD=1.2% ）, 97.4% （RSD=1. 6% ）and 98.6% （RSD=1.7%）, respectively. The contents of emodin, chrysophanol and ararobinol in free anthraquinones were in the ranges of 0.008%-0.088%, 0.007%-0.289% and 0.007%-0.103%, respectively. The contents of emodin, chrysophanol and ararobinol in total anthraquinones were in the ranges of 0.034%-0.244%, 0.076%-0.856% and 0.030%-0.297%, respectively. Conclusion： Rumex crispus had more combined anthraquinones than Rumex dentatus, Rumex nepalensis and 9 batches of undefined samples. Contents of combined anthraquinones in Rumex crispus and Rumex dentatus were higher than free anthraquinones in those samples.

关 键 词：土大黄 游离蒽醌 总蒽醌 大黄素 大黄酚 大黄素甲醚 含量测定 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]