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[摘要]
目的 建立同时测定八味沉香散中没食子酸、原儿茶酸、木香烃内酯、去氢木香内酯、去氢二异丁香酚、11-羰基-β-乙酰乳香酸6种成分的HPLC-DAD方法.方法 采用RP-HPLC法,Waters XBridge-C18色谱柱(250 mm×4.6 mm,5.0 μm),甲醇-乙腈(50:50,A)和甲醇-0.1%乙酸水溶液(10:90,B)为流动相,体积流量0.8 mL/min,梯度洗脱;柱温35 ℃;进样量10 μL.分别对线性关系、精密度、重复性、稳定性及加样回收率进行考察.结果 被测定的6种指标成分没食子酸在1.5~30.0 mg/L(r=0.999 0)、原儿茶酸在1.0~20.0 mg/L(r=0.999 2)、木香烃内酯在2.0~40.0 mg/L(r=0.999 1)、去氢木香内酯在2.0~40.0 mg/L(r=0.999 3)、去氢二异丁香酚在0.2~4.0 mg/L(r=0.999 4)、11-羰基-β-乙酰乳香酸在3.5~70.0 mg/L(r=0.999 1)线性关系良好;精密度、重复性良好,RSD均小于2.0%;在室温条件下24 h内稳定;平均加样回收率在98.49%~101.55%(RSD≤2.0%).结论 该方法简便、准确,重复性好,为八味沉香散的质量控制提供实验依据.
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[Abstract]
Objective To develop an HPLC method for simultaneous determination of gallic acid, protocatechuic acid, costunolide, dehvdrocostuslactone, ehydrodiisoeugenol, and acetyl-11-keto-β-boswellic acid in Bawei Chenxiang Powder (BCP). Methods The chromatographic separation was achieved on a Waters XBridge-C18 column (250 mm × 4.6 mm, 5.0 μm) with methanol-acetonitrile (50:50, A) and methanol-0.1% acetic acid (10:90, B) as mobile phases at the flow rate of 0.8 mL/min for gradient elution, and the column temperature was 35 ℃. Its linear relationship, precision, repeatability, stability, and recoveries were investigated. Results The seven components were well separated and showed good linearity, such as gallic acid 1.5—30.0 mg/L (r = 0.999 0), protocatechuic acid 1.0—20.0 mg/L (r= 0.999 2), costunolide 2.0—40.0 mg/L (r= 0.999 1), dehvdrocostuslactone 2.0—40.0 mg/L (r= 0.999 3), ehydrodiisoeugenol 0.2—4.0 mg/L (r= 0.999 4), and acetyl-11-keto-β-boswellic acid 3.5—70.0 mg/L (r= 0.999 1). The precision was good, and RSD value was less than 2.0%. The repeatability was good, and RSD was less than 2.0%. The stability was good in 24 h. The average recoveries were between 98.49% and 101.55% (RSD ≤ 2.0%). Conclusion The method is accurate, sensitive, credible, and repeatable. It can be applied to the quality control of BCP.
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