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目的:建立同时测定妇乐颗粒中没食子酸、绿原酸、芍药苷、丹皮酚含量的方法。方法:采用高效液相色谱法。色谱柱为月旭XB-C18,流动相为甲醇-0.05%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为270 nm(没食子酸、丹皮酚)、325 nm(绿原酸)、230 nm(芍药苷),柱温为30 ℃,进样量为10 μL。结果:没食子酸、绿原酸、芍药苷和丹皮酚检测进样量线性范围分别为0.076 2~1.524 μg(r=0.999 7)、0.037 6~0.751 μg(r=0.999 9)、0.030 3~0.606 μg(r=0.999 7)、0.020 6~0.412 μg(r=0.999 8);定量限分别为0.353、0.276、0.421、0.540 μg/mL,检测限分别为0.121、0.104、0.148、0.186 μg/mL;精密度、稳定性、重复性试验的RSD≤2.04%;加样回收率分别为95.24%~100.47%(RSD=1.59%,n=9)、99.49%~103.70%(RSD=2.27%,n=9)、96.27%~101.09%(RSD=1.94%,n=9)、95.05%~98.90%(RSD=1.22%,n=9)。结论:该方法操作简单、结果准确、重复性良好,可用于妇乐颗粒中没食子酸、绿原酸、芍药苷、丹皮酚含量的同时测定。
OBJECTIVE: To establish a method for simultaneous determination of gallic acid, chlorogenic acid, paeoniflorin and paeonol in Fule granules. METHODS: HPLC method was adopted. The determination was performed on Ultimate XB-C18 column with mobile phase consisted of acetonitrile-0.05% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were 270 nm(gallic acid,paeonol), 325 nm (chlorogenic acid) and 230 nm (paeoniflorin). The column temperature was 30 ℃, and sample size was 10 μL. RESULTS: The linear ranges of gallic acid, chlorogenic acid, paeoniflorin and paeonol were 0.076 2-1.524 μg(r=0.999 7), 0.037 6-0.751 μg (r=0.999 9), 0.030 3-0.606 μg (r=0.999 7), 0.020 6-0.412 μg(r=0.999 8), respectively. The limits of quantification were 0.353, 0.276, 0.421, 0.540 μg/mL, and the limits of detection were 0.121, 0.104, 0.148, 0.186 μg/mL. RSDs of precision, stability and reproducibility tests were all no more than 2.04%. The recoveries were 95.24%-100.47%(RSD=1.59%,n=9),99.49%-103.70%(RSD=2.27%, n=9), 96.27%-101.09%(RSD=1.94%,n=9), 95.05%-98.89%(RSD=1.22%,n=9), respectively. CONCLUSIONS: The method is simple, accurate and reproducible, and can be used for the simultaneous determination of gallic acid, chlorogenic acid, paeoniflorin and paeonol in Fule granules.
妇乐颗粒高效液相色谱法没食子酸绿原酸芍药苷丹皮酚含量
Fule granulesHPLCGallic acidChlorogenic acidPaeoniflorinPaeonolContent
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