HPLC法同时测定大黄药材中8个非蒽醌类成分的含量
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篇名: HPLC法同时测定大黄药材中8个非蒽醌类成分的含量
TITLE:
摘要: 目的:建立同时测定大黄药材中8个非蒽醌类成分含量的方法。方法:采用高效液相色谱法。色谱柱为Symmetry C18,流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),流速为1.0 mL/min,柱温为30 ℃,检测波长为280 nm,进样量为30 μL。结果:没食子酸、儿茶素、表儿茶素、白藜芦醇4′-O-葡萄糖苷、表儿茶素没食子酸酯、白藜芦醇4′-O-β-D-(6″-O-没食子酰)-葡萄糖苷、番泻苷A、4′-羟基苯基-2-丁酮-4′-O-β-D-(2″-O-没食子酰-6″-O-对羟基桂皮酰)-葡萄糖苷检测进样量的线性范围分别为6.16~2 464 ng(r=0.999 9)、37.4~14 960 ng(r=0.999 9)、7.635~3 054 ng(r=0.999 7)、7.63~3 052 ng(r=0.999 9)、8.32~3 328 ng(r=0.999 9)、11.5~4 600 ng(r=0.999 9)、16.08~6 432 ng(r=0.999 9)、29.3~11 720 ng(r=0.999 9);定量限分别为3.48、4.30、6.40、4.40、3.39、2.87、8.40、4.95 ng,检测限分别为2.32、2.58、2.40、2.64、2.26、1.23、4.20、2.97 ng;精密度、稳定性、重复性试验的RSD均小于5%;加样回收率分别为94.32%~100.54%(RSD=2.78%,n=6)、91.15%~99.36%(RSD=3.72%,n=6)、92.16%~98.04%(RSD=2.39%,n=6)、93.41%~100.73%(RSD=3.17%,n=6)、93.89%~98.40%(RSD=1.99%,n=6)、92.61%~101.74%(RSD=3.71%,n=6)、92.66%~103.40%(RSD=3.76%,n=6)、95.45%~102.70%(RSD=3.06%,n=6)。结论:所建方法简便、准确、专属性强,可用于同时测定大黄药材中8个非蒽醌类成分的含量。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of 8 non-anthraquinone constituents in Rheum palmatum. METHODS: HPLC method was adopted. The determination was performed on Symmetry C18 column with mobile phase consisted of methanol-0.1% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The column temperature was 30 ℃ and detection wavelength was 280 nm. Sample size was 30 μL. RESULTS: The linear range of gallic acid, catechin, epicatechin, resveratrol 4′-O-glucopyranoside, epicatechin gallate, resveratrol 4′-O-β-D-(6″-O-galloyl)-glucopyranoside, sennoside A, 4′-hydroxyphenyl-2-butanone-4′-O-β-D-(2″-O-galloyl-6″-O-p-hydroxy cinnamyl)-glucopyranoside were 6.16-2 464 ng(r=0.999 9), 37.4-14 960 ng(r=0.999 9), 7.635-3 054 ng(r=0.999 7), 7.63-3 052 ng(r=0.999 9), 8.32-3 328 ng(r=0.999 9), 11.5-4 600 ng(r=0.999 9), 16.08-6 432 ng(r=0.999 9), 29.3-11 720 ng(r=0.999 9), respectively. The limits of quantitation were 3.48, 4.30, 6.40, 4.40, 3.39, 2.87, 8.40 and 4.95 ng, respectively. The limits of detection were 2.32, 2.58, 2.40, 2.64, 2.26, 1.23, 4.20, 2.97 ng, respectively. RSDs of precision, stability and reproducibility tests were all lower than 5%. Recoveries were 94.32%- 100.54%(RSD=2.78%,n=6), 91.15%-99.36%(RSD=3.72%,n=6), 92.16%-98.04%(RSD=2.39%,n=6), 93.41%-100.73%(RSD=3.17%,n=6), 93.89%-98.40%(RSD=1.99%,n=6), 92.61%-101.74%(RSD=3.71%,n=6), 92.66%-103.40%(RSD=3.76%,n=6), 95.45%-102.70%(RSD=3.06%,n=6), respectively. CONCLUSIONS: The established method is simple, accurate and specific, and can be used for the simultaneous determination of 8 non-anthraquinone constituents in R. palmatum.
期刊: 2019年第30卷第14期
作者: 陆文瑾,窦志华,曹瑞,倪丽丽,戴莹
AUTHORS: LU Wenjin,DOU Zhihua,CAO Rui,NI Lili,DAI Ying
关键字: 大黄;没食子酸;儿茶素;表儿茶素;白藜芦醇4′-O-葡萄糖苷;表儿茶素没食子酸酯;白藜芦醇4′-O-β-D-(6″-O-没食子酰)-葡萄糖苷;番泻苷A
KEYWORDS: Rheum palmatum; Gallic acid; Catechin; Epicatechin; Resveratrol-4′-O-glucopyranoside; Epicatechin gallate; Resveratrol-4′-O-β-D-(6″-O-galloyl)-glucopyranoside; Sennoside A
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