摘要
目的:建立同时测定活血促愈胶囊中2种黄酮类(芦丁、山柰酚-3-O-芸香糖苷)和4种菲醌类成分(二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_A)含量的方法。方法:采用高效液相色谱法。色谱柱为Welch Ultimate XB-C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,柱温为20℃,检测波长为270 nm,进样量为10μL。结果:芦丁、山柰酚-3-O-芸香糖苷、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_A的检测质量浓度线性范围分别为172.13~860.66μg/mL(r=0.999 7)、15.33~76.66μg/mL(r=0.999 8)、12.81~64.06μg/mL(r=0.999 3)、5.90~29.52μg/m L(r=0.999 3)、5.12~25.60μg/mL(r=0.999 2)、6.71~33.57μg/m L(r=0.999 7),检测限分别为0.08、0.01、0.01、0.01、0.01、0.01μg/mL,定量限分别为0.27、0.02、0.03、0.03、0.03、0.03μg/m L;精密度、稳定性、重复性试验的RSD均小于2.0%(n=6);加样回收率分别为97.54%~100.25%(RSD=1.07%,n=6)、96.90%~101.91%(RSD=1.73%,n=6)、96.24%~102.89%(RSD=2.32%,n=6)、97.04%~102.18%(RSD=1.82%,n=6)、95.06%~97.73%(RSD=1.18%,n=6)、95.59%~101.40%(RSD=2.29%,n=6)。结论:该方法灵敏、快速、操作简便、重复性好,可用于活血促愈胶囊中芦丁、山柰酚-3-O-芸香糖苷、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_A含量的同时测定。
OBJECTIVE:To establish a method for simultaneous determination of two flavonoids(rutin and kaempferol-3-Orutinoside) and four phenoquinones(dihydrotanshinone Ⅰ,cryptotanshinone,tanshinone Ⅰ and tanshinone Ⅱ_A)in Huoxue cuyu capsules. METHODS:HPLC method was adopted. The determination was performed on Welch Ultimate XB-C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution(gradient elution)at the flow rate of 1.0 mL/min. The column temperature was set at 20 ℃,and detection wavelength was set at 270 nm. The sample size was 10 μL. RESULTS:The linear range of rutin,kaempferol-3-O-rutinoside,dihydrotanshinone Ⅰ,cryptotanshinone,tanshinone Ⅰ and tanshinoneⅡ_Awere 172.13-860.66 μg/m L(r=0.999 7),15.33-76.66 μg/mL(r=0.999 8),12.81-64.06 μg/mL(r=0.999 3),5.90-29.52 μg/mL(r=0.999 3),5.12-25.60 μg/m L(r=0.999 2),6.71-33.57 μg/mL(r=0.999 7),respectively. The limits of detection were 0.08,0.01,0.01,0.01,0.01,0.01 μg/mL. The limits of quantitation were 0.27,0.02,0.03,0.03,0.03,0.03 μg/mL,respectively. RSDs of precision,stability test and repetition tests were all lower than 2.0%(n=6). The recoveries were 97.54%-100.25%(RSD=1.07%,n=6),96.90%-101.91%(RSD=1.73%,n=6),96.24%-102.89%(RSD=2.32%,n=6),97.04%-102.18%(RSD=1.82%,n=6),95.06%-97.73%(RSD=1.18%,n=6),95.59%-101.40%(RSD=2.29%,n=6),respectively. CONCLUSIONS:The method is sensitive,rapid,simple and has good reproducibility. It can be used for simultaneous determination of rutin, kaempferol-3-O-rutinoside, dihydrotanshinone Ⅰ,cryptotanshinone,tanshinone Ⅰ,tanshinoneⅡ_A in Huoxue cuyu capsules.
引文
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