机构地区:[1]中国中医科学院中药研究所中药质量控制技术国家工程实验室,北京100700
出 处:《中国中药杂志》2021年第23期6196-6203,共8页China Journal of Chinese Materia Medica
基 金:国家“重大新药创制”科技重大专项(2018ZX09721004)。
摘 要:建立当归中2种有机酸和5种苯酞类成分的HPLC含量测定方法,明确当归药材与饮片中主要成分传递规律。选用Welch Ultimate C_(8)色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.085%磷酸水(B)为流动相进行梯度洗脱,流速1.1 mL·min^(-1),柱温25℃,检测波长280 nm,进样量10μL。在此条件下对15批当归药材及其相应饮片中绿原酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、洋川芎内酯A、藁本内酯和丁烯基苯酞共7种成分进行含量测定并计算其从药材到饮片的转移率。结果显示绿原酸的平均含量饮片中稍有降低,阿魏酸的平均含量在药材和饮片中基本持平,饮片中洋川芎内酯I、洋川芎内酯H、洋川芎内酯A和丁烯基苯酞4种挥发性成分的含量较药材中均呈升高的趋势,藁本内酯含量在饮片中显著降低,含量变化最为明显,其在药材中的质量分数均在0.7%以上,平均为0.94%,符合《香港中药材标准》中的规定(0.6%),而其在饮片中的平均质量分数仅为0.47%,含量下降近50%,进一步研究表明新鲜切制的当归饮片中藁本内酯的含量与药材相比变化并不明显,这提示当归饮片中的藁本内酯是在储藏过程中大量损失的。因此非必需情况下当归更适合以药材形式储藏或者应该现用现制饮片,此外应同时对当归药材和饮片中的挥发油或藁本内酯的含量进行控制以保证其临床使用的有效性。A HPLC method was established for simultaneous determination of two organic acids(chlorogenic acid and ferulic acid)and five phthalides(senkyunolide I,senkyunolide H,senkyunolide A,ligustilide,and butylidenephthalide)in Angelicae Sinensis Radix and its processed products to clarify the underlying material transferring rules.The analysis was performed on a Welch Ultimate C_(8) column(4.6 mm×250 mm,5μm)with acetonitrile(A)-0.085%phosphoric acid water(B)as the mobile phase in a gradient elution mode at the flow rate of 1.1 mL·min^(-1),the column temperature of 25℃,the detection wavelength of 280 nm,and the injection volume of 10μL.Under these conditions,the content of the above-mentioned seven components was analyzed in 15 batches of Angelicae Sinensis Radix and its processed products,and the transfer rate of each compound was calculated.As a result,in the processed products,the average content of chlorogenic acid was slightly decreased and that of ferulic acid was equivalent to the medicinal materials.The content of senkyunolide I,senkyunolide H,senkyunolide A,and butylidenephthalide showed an increasing trend in the processed products as compared with the medicinal materials.The mass fraction of ligustilide in the medicinal materials was above 0.7%(0.94%on average),meeting the requirement of 0.6%in the Hong Kong Chinese Materia Medica Standards,but was 0.47%on average in the processed products,which was decreased by 50%approximately.Further investigation showed that the content of ligustilide in freshly made processed products of Angelicae Sinensis Radix did not change significantly compared with that in the medicinal materials,indicating that the loss of ligustilide in the processed products mainly occurred in the storage.Therefore,Angelicae Sinensis Radix is suitable for storing in the form of medicinal materials and the freshly made processed products should be used except for special cases.Additionally,it is recommended to control the content of volatile oils or ligustilide in medicinal materials and pro
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