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出 处:《中国药房》2017年第12期1677-1680,共4页China Pharmacy
基 金:国家自然科学基金资助项目(No.41201526);山东省教育厅高校科研发展计划项目(No.J12LM59)
摘 要:目的:建立测定金银花药材中绿原酸和木犀草苷含量的方法,以探讨金银花在常温密封环境下的保质期。方法:采用高效液相色谱法。色谱柱为Agilent Zorbax SB-C_(18)(绿原酸)、Agilent Zorbax SB-Phenyl(木犀草苷),流动相为乙腈-0.4%磷酸溶液(13∶87,V/V,绿原酸)、乙腈-0.5%冰醋酸溶液(梯度洗脱,木犀草苷),流速为1.0 m L/min,检测波长为327 nm(绿原酸)、350 nm(木犀草苷),柱温为30℃,进样量为10μL。结果:绿原酸、木犀草苷检测质量浓度线性范围分别为10~100μg/m L(r=0.998 6)、5~50μg/m L(r=0.999 3);精密度、稳定性、重复性试验的RSD<4.0%;加样回收率分别为95.78%~99.70%(RSD=1.46%,n=6)、96.30%~104.31%(RSD=2.93%,n=6)。滚简杀青、烤房烘干、自然晾晒的药材样品中绿原酸和木犀草苷的含量在贮藏12个月后普遍降低了30%~40%。结论:该方法操作简便,精密度、稳定性、重复性好,可用于金银花药材中绿原酸和木犀草苷含量的测定;金银花在贮藏1年后有效成分的含量显著下降,有必要建立金银花保质期规范,以保证临床用药的有效性。OBJECTIVE: To establish a method for determining the contents of chlorogenic acid and luteoloside in Lonicerae japonicae, and to explore the shelf life of L. japonicae under ordinary temperature and sealed environment. METHODS : HPLC method was adopted. The determination was performed on Agilent Zorbax SB-C18 (chlorogenic acid)column and Agilent Zorbax SB-Phenyl (galuteolin) with mobile phase consisted of acetonitrile-0.4 % phosphoric acid ( 13 : 87, V/V), acetonitrile-0.5 % glacial acetic acid (gradient elution, galuteolin) at the flow rate of 1.0 mL/min. The detection wavelength was set at 327 nm (chlorogenic acid) and 350 nm (galuteolin). The column temperature was 30℃, and sample size was 10 IxL. RESULTS: The linear range of chloro- genie acid and galuteolin were 10-100 μg/mL (r=0.998 6), 5-50 μtg/mL (r=0.999 3), respectively. RSDs of precision, stability and reproducibility tests were all lower than 4.0%. Recoveries were 95.78%-99.70% (RSD=1.46%, n=6), 96.30%-104.31% (RSD=2.93%, n:6). The contents of chlorogenie acid and galuteolin in roller method, baking method and natural drying method of processed L. japonicae were all decreased by 30% -40% after stored for 12 months. CONCLUSIONS: The method is simple, precise, stable and repeatable, and can be used for simultanoue determination of chlorogenic acid and luteoloside in L. japonicae. The contents of active components in L. japonicae decrease significantly after stored for 12 months. It is necessary to establish shelf life standard of L. japonieae, so as to guarantee the effectiveness of drug use in the clinic.
分 类 号:R917[医药卫生—药物分析学] R927.2[医药卫生—药学]
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