摘要
目的:建立同时测定加味补阳还五汤剂中芍药苷、苦杏仁苷、阿魏酸、川芎嗪含量的方法。方法:采用反相高效液相色谱法。色谱柱为YMC C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 m L/min,检测波长为320 nm(阿魏酸)、230 nm(芍药苷)、207 nm(苦杏仁苷)、280 nm(川芎嗪),柱温为30℃,进样量为10μL。结果:芍药苷、苦杏仁苷、阿魏酸和川芎嗪检测质量浓度线性范围分别为0.191 2~1.912μg/m L(r=0.999 6)、0.117 4~1.174μg/m L(r=0.999 6)、0.011 5~0.115μg/m L(r=0.999 8)和0.001 66~0.016 6μg/m L(r=0.999 7);定量限分别为1.912、1.174、0.115、0.016 6μg/m L,检测限分别为0.25、0.40、0.05、0.008 5μg/m L;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为96.9%~100.3%(RSD=1.3%,n=6)、95.1%~100.3%(RSD=2.2%,n=6)、95.3%~100.2%(RSD=2.0%,n=6)、97.0%~100.0%(RSD=1.3%,n=6)。结论:该方法可靠、简便、准确,适用于同时测定加味补阳还五汤剂中芍药苷、苦杏仁苷、阿魏酸、川芎嗪的含量。
OBJECTIVE: To establish the method for simultaneous determination of paeoniflorin, amygdalin, ferulic acid and ligustrazine in Modified buying huanwu decoction. METHODS: RP-HPLC method was adopted. The determination was performed on YMC C18 column with the mobile phase consisted of acetonitrile-0.1% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 320 nm (ferulic acid), 230 nm (paeoniflorin), 207 nm (amygdalin), 280 nm (li- gustrazine). The column temperature was 30 ~C, and sample size was 10 μL. RESULTS: The linear ranges of paeoniflorin, amyg- dalin, ferulic acid and ligustrazine were 0.191 2-1.912 μg/mL (r=0.999 6),0.117 4-1.174 μg/mL (r=0.999 6),0.011 5-0.115 μg/ mL (r=0.999 8) and 0.001 66-0.016 6 μg/mL(r=0.999 7), respectively. The limits of quantitation were 1.912, 1.174, 0.115, 0.016 6 μg/mL, and the limits of detection were 0.25, 0.40, 0.05, 0.008 5 μg/mL, respectively. RSDs of precision, stability and reproducible tests were all lower than 2.0%. The recoveries were 96.9%-100.3% (RSD=l.3%, n=6), 95.1%-100.3% (RSD= 2.2%, n=6), 95.3%-100.2% (RSD=2.0%, n=6)and 97.0%-100.0% (RSD= 1.3%, n=6). CONCLUSIONS: The method is reli- able, simple and accurate, and is suitable for simultaneous determination of paeoniflorin, amygdalin, ferulic acid and ligustrazine in Modified buyang huanwu decoction.
出处
《中国药房》
CAS
北大核心
2017年第27期3849-3852,共4页
China Pharmacy
基金
江苏省中医药局科技项目(No.LZ13167)
南通市科技计划项目(No.HS2013047)