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[摘要]
目的 建立同时测定加味逍遥丸(JXP)中栀子苷、甘草苷、丹皮酚、西红花苷I、西红花苷II、芍药苷、甘草酸、阿魏酸8种成分的HPLC-DAD方法。方法 采用Plastisil ODS(250mm×4.6mm,5μm);流动相为乙腈-0.2%磷酸水溶液,梯度洗脱,体积流量1.0mL/min,柱温37℃,检测波长栀子苷为238nm,甘草苷和丹皮酚为274nm,西红花苷I和西红花苷II为440nm,芍药苷和甘草酸为228nm,阿魏酸为324nm,进样量10μL。结果 被测定的8种成分在设定的色谱条件下均有良好的分离度,方法精密度,重复性RSD值均<2%,被测定样品在室温条件下12h内稳定,各成分均有较宽的线性范围和良好的线性关系,栀子苷、甘草苷、丹皮酚、西红花苷I、西红花苷II、芍药苷、甘草酸、阿魏酸线性范围分别为48~288μg/mL(r=0.9994)、60~360μg/mL(r=0.9992)、64~384μg/mL(r=0.9998)、19.2~115.2μg/mL(r=0.9995)、4~24μg/mL(r=0.9992)、96~576μg/mL(r=0.9996)、64~384μg/mL(r=0.9997)、20~120μg/mL(r=0.9994),平均加样回收率在99.13%~100.25%,RSD值均<2.0%。6批JXP中栀子苷、甘草苷、丹皮酚、西红花苷I、西红花苷II、芍药苷、甘草酸、阿魏酸质量分数分别在2.34~2.82mg/g、2.63~3.28mg/g、3.66~4.55mg/g、1.05~1.41mg/g、0.34~0.41mg/g、4.78~5.32mg/g、2.83~3.37mg/g、1.36~1.73mg/g。结论 本方法操作简单,经方法学验证测定结果准确可靠,是可用于JXP质量控制的一种有效方法。
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[Abstract]
Objective To establish an HPLC-DAD method for the simultaneous determination of eight components in Jiaowei Xiaoyao Pill (JXP), such as jasminoidin, liquiritin, paeonol, crocin I, crocin II, peoniflorin, glycyrrhizic acid, and ferulic acid.Methods The chromatographic separation was performed on a Plastisil ODS column (250 mm × 4.6 mm, 5 μm) with acetonitrile (B)-0.2% phosphate acid solution (D) as mobile phase at the flow rate of 1.0 mL/min for gradient elution and the column temperature was 37℃. The detection wavelength was set at 238 nm for jasminoidin, 274 nm for liquiritin and paeonol, 440 nm for crocin I and crocin II, 228 nm for peoniflorin and glycyrrhizic acid, and 324 nm for ferulic acid. The volume of sample injection was 10 μL.Results The eight compounds were well separated under the determined chromatographic conditions. The RSD of precision and repeatability experiment were all less than 2% and the sample solution was stable during 12 h. All the compounds had a wide linear range and good linearity: the linear range of jasminoidin, liquiritin, paeonol, crocin I, crocin II, peoniflorin, glycyrrhizic acid, and ferulic acid were 48—288μg/mL (r= 0.999 4), 60—360μg/mL (r= 0.999 2), 64—384μg/mL (r= 0.999 8), 19.2—115.2μg/mL (r= 0.999 5), 4—24μg/mL (r= 0.999 2), 96—576μg/mL (r= 0.999 6), 64—384μg/mL(r= 0.999 7), and 20—120μg/mL (r= 0.999 4), respectively. The average recoveries were between 99.13%—100.25% and the RSD were all less than 2.0%. The content ranges of jasminoidin, liquiritin, paeonol, crocin I, crocin II, peoniflorin, glycyrrhizic acid, and ferulic acid in six batches of JXP were 2.34—2.82 mg/g, 2.63—3.28 mg/g, 3.66—4.55 mg/g, 1.05—1.41 mg/g, 0.34—0.41 mg/g, 4.78—5.32 mg/g, 2.83—3.37 mg/g, and 1.36—1.73 mg/g, respectively.Conclusion The method is simple and convenient, and the methodology validation shows that determination result of the method is accurate and reliable and it can be an effective approach for the quality control of JXP.
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