HPLC法同时测定真武汤中11种活性成分的含量
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篇名: HPLC法同时测定真武汤中11种活性成分的含量
TITLE:
摘要: 目的:建立同时测定真武汤中5-羟甲基糠醛、(+)-儿茶素、芍药苷、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰芍药苷、6-姜酚、8-姜酚、白术内酯Ⅱ、6-姜烯酚、茯苓酸含量的方法。方法:采用高效液相色谱法。色谱柱为Phenomenex Kinetex C18,流动相为乙腈-0.2%磷酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长为285 nm(4.4~7 min,5-羟甲基糠醛)、203 nm[7~12 min,(+)-儿茶素]、233 nm(12~50 min,芍药苷、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰芍药苷)、200 nm(50~62.3 min,6-姜酚、8-姜酚;62.9~90 min,6-姜烯酚、茯苓酸)、222 nm(62.3~62.9 min,白术内酯Ⅱ),柱温为35 ℃,进样量为20 μL。结果:5-羟甲基糠醛、(+)-儿茶素、芍药苷、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰芍药苷、6-姜酚、8-姜酚、白术内酯Ⅱ、6-姜烯酚、茯苓酸检测质量浓度线性范围分别为0.62~12.47 μg/mL(r=0.999 6)、2.36~47.25 μg/mL(r=0.999 7)、200.80~4 016 μg/mL(r=0.999 7)、4.45~89.04 μg/mL(r=0.999 6)、4.28~85.54 μg/mL(r=0.999 5)、5.16~103.13 μg/mL(r=0.999 9)、5.53~110.66 μg/mL(r=0.999 9)、0.84~16.89 μg/mL(r=0.999 8)、0.60~12.04 μg/mL(r=0.999 9)、0.53~10.62 μg/mL(r=0.999 5)、1.04~20.78 μg/mL(r=0.999 7);定量限分别为0.155、0.590、1.210、1.112、1.070、0.258、0.553、0.421、0.153、0.354、0.431 μg/mL,检测限分别为0.047、0.179、0.134、0.337、0.324、0.078、0.168、0.128、0.046、0.107、0.131 μg/mL,精密度、稳定性、重复性试验的RSD均小于3%;加样回收率分别为96.06%~103.01%(RSD=2.64%,n=6)、95.11%~101.57%(RSD=2.58%,n=6)、97.22%~102.11%(RSD=1.93%,n=6)、96.43%~102.78%(RSD=2.35%,n=6)、96.42%~101.43%(RSD=2.15%,n=6)、96.86%~102.05%(RSD=2.10%,n=6)、95.32%~100.55%(RSD=1.87%,n=6)、97.04%~103.25%(RSD=2.22%,n=6)、96.78%~103.22%(RSD=2.62%,n=6)、97.04%~103.14%(RSD=2.28%,n=6)、97.08%~103.51%(RSD=2.94%,n=6)。结论:该方法准确、专属性好,可用于同时测定真武汤中11种活性成分的含量。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of eleven active constituents in Zhenwutang decoction, such as 5-hydroxymethylfurfural, (+)-cianidanol, paeoniflorin, benzoylaconitine, benzoylhypacoitine, benzoylpaeoniflorin, 6-gingerol, 8-gingerol, atractylenolide Ⅱ, 6-shogaol and pachymic acid. METHODS: HPLC method was adopted. The separation was performed on Phenomenex Kinetex C18 column with mobile phase consisted of acetonitrile-0.2 % phosphoric acid solution(gradient elution) at flow rate of 1.0 mL/min. The detection wavelength was set at 285 nm (4.4-7 min, 5-hydroxymethylfurfural), 203 nm [7-12 min,(+)-cianidanol], 233 nm (12-50 min,paeoniflorin, benzoylaconitine, benzoylhypacoitine, benzoylpaeoni- florin), 200 nm (50-62.3 min, 6-gingerol, 8-gingerol; 62.9-90 min, 6-shogaol, pachymic acid) and 222 nm (62.3-62.9 min, atractylenolide Ⅱ). The column temperature was set at 35 ℃, and the sample size was 20 μL. RESULTS: The linear ranges of 5-hydroxymethylfurfural, (+) -cianidanol, paeoniflorin, benzoylaconitine, benzoylhypacoitine, benzoylpaeoniflorin, 6-gingerol, 8-gingerol, atractylenolide Ⅱ, 6-shogaol, pachymic acid were 0.62-12.47 μg/mL (r=0.999 6),2.36-47.25 μg/mL (r=0.999 7),200.80-4 016 μg/mL (r=0.999 7),4.45-89.04 μg/mL (r=0.999 6),4.28-85.54 μg/mL (r=0.999 5),5.16-103.13 μg/mL (r=0.999 9),5.53-110.66 μg/mL (r=0.999 9),0.84-16.89 μg/mL (r=0.999 8),0.60-12.04 μg/mL (r=0.999 9),0.53-10.62 μg/mL (r=0.999 5),1.04-20.78 μg/mL (r=0.999 7), respectively. The limits of quantitation were 0.155, 0.590, 1.210, 1.112, 1.070, 0.258, 0.553, 0.421, 0.153, 0.354, 0.431 μg/mL, respectively. The limits of detection were 0.047, 0.179, 0.134, 0.337, 0.324, 0.078, 0.168, 0.128, 0.046, 0.107, 0.131 μg/mL, respectively. RSDs of precision, stability and reproducibility tests were all lower than 3%. The average recovery rates were 96.06%-103.01%(RSD=2.64%,n=6), 95.11%-101.57%(RSD=2.58%,n=6), 97.22%-102.11%(RSD=1.93%,n=6), 96.43%-102.78%(RSD=2.35%,n=6), 96.42%-101.43%(RSD=2.15%,n=6), 96.86%-102.05%(RSD=2.10%,n=6), 95.32%-100.55%(RSD=1.87%,n=6), 97.04%-103.25%(RSD=2.22%,n=6), 96.78%-103.22%(RSD=2.62%,n=6), 97.04%-103.14%(RSD=2.28%,n=6), 97.08%-103.51%(RSD=2.94%,n=6), respectively. CONCLUSIONS: The method is accurate and specific, and suitable for simultaneous determination 11 active components of Zhenwutang decoction.
期刊: 2019年第30卷第18期
作者: 田萍,马开,张薇,张迪文,刘碧碧,郭晓燕,韩德恩
AUTHORS: TIAN Ping,MA Kai,ZHANG Wei,ZHANG Diwen,LIU Bibi,GUO Xiaoyan,HAN De’en
关键字: 真武汤;高效液相色谱法;5-羟甲基糠醛;(+)-儿茶素;芍药苷;苯甲酰乌头原碱;苯甲酰次乌头原碱;苯甲酰芍药苷;6-姜酚;8-姜酚;白术内酯Ⅱ;6-姜烯酚;茯苓酸;含量测定
KEYWORDS: Zhenwutang decoction; HPLC; 5-hydroxymethylfurfural; (+)-cianidanol; Paeoniflorin; Benzoylaconitine; Benzoylhypacoitine; Benzoylpaeoniflorin; 6-gingerol; 8-gingerol; Atractylenolide Ⅱ; 6-shogaol; Pachymic acid; Content determination
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