藏药“松蒂”的质量标准提升研究

Improvement of Quality Standard for Tibetan Medicine“Songdi”

目的对藏药“松蒂”的质量标准进行提升研究,为全面评价其质量提供科学依据。方法对“松蒂”药材进行粉末显微鉴别;采用薄层色谱(Thin layer chromatography,TLC)法以绿原酸、山奈苷和sutchuenoside A(山奈酚-3-O-α-L-(3-O-乙酰基)-鼠李糖基-7-O-α-鼠李糖苷)为对照品对12批不同产地药材进行定性鉴别;并按《中国药典》(2020版)要求增加了各检查项;建立高效液相色谱法(High Performance Liquid Chromatography,HPLC)测定药材中3种成分(绿原酸、山奈苷、sutchuenoside A)的含量;结果“松蒂”药材粉末呈棕褐色,腺毛常见,腺头扁球形或球形,叶表皮细胞呈波状弯曲,气孔多为平轴式,偶见不定式,副卫细胞4-6个;花粉粒,具有3个萌发孔,散在;导管多为螺纹型;茎表皮细胞呈梭形,镶嵌状紧密排列。TLC结果显示,供试品与3种对照品在色谱的同位置出现同色的荧光斑点。12批药材中药材水分含量为5.94%-10.97%,总灰分含量为9.44%-17.72%,酸不溶性灰分为2.44%-4.08%,醇溶性浸出物含量为25.68%-35.20%;含量测定方法学考察显示,绿原酸、山奈苷、sutchuenoside A的质量浓度分别在18.80-521.60、16.50-528.40、15.30-492.00μg·mL^(-1)范围内与各自峰面积呈良好线性关系(r>0.9990);精密度、稳定性、重复性试验的RSD均小于3.00%(n=6);平均加样回收率分别为98.75%、97.82%、99.03%(RSD均小于3.00%,n=6)。12批药材中上述3种成分含量范围分别为0.25%-0.38%、0.27%-0.90%、0.11%-0.38%。结论该方法有良好的精密度、稳定性和重复性,能为科学、全面评价该药品质量提供依据。

Objective To enhance the quality criteria of Tibetan Medicine"Songdi",and to provide scientific basis for comprehensive quality evaluation.Methods The powder microscopic identification of"Songdi"was carried out.chlorogenic acid,kaempferin and Sutchuenoside A were used as control materials for qualitative identification by TLC.Andaccording to the method stated in 2020 edition of Chinese Pharmacopoeia,the water content,total ash content,acid insoluble ash content and extract were examined.HPLC method was used to the determination of chlorogenic acid,kaempferin and Sutchuenosidea A in"Songdi".Results The powder of was brown,with common glandular hair,and the glandular head was flat or spherical;The leaf epidermal cells were wavy and curved,and the stomata were mostly flat axis and occasionally infinitive;there were 4 to 6 accessory cells;Pollen grains,with three germination pores,scattered;The conduit is mostly thread type;The stem epidermal cells were fusiform and closely arranged in Mosaic shape.Results of TLC showed that the spots of thesame color were found in the corresponding positions of chromatogram for 3 substance control and samples.The average contents of water,total ash,acid-insoluble ash content and alcohol soluble extract were 5.94%-10.97%,9.44%-17.72%,2.44%-4.08%,25.68%-35.20%,respectively.The mass concentrations of chlorogenic acid,kaempferin and sutchuenoside A were 18.8-521.6,16.5-528.4 and 15.3-492.0μg/mL,respectively showed a good linear relationship with the peak area(r>0.9990).The RSD of related items of methodology verification was less than 3%(n=6).The average recoveries were 98.75%、97.82%、99.03%(all RSDs<3.00%,n=6).The average percentage of contents of the aforementioned 3 compounds in all samples were 0.25%-0.38%、0.27%-0.90%、0.11%-0.38%respectively.Conclusions The method is precise,stable and repeatable,which can offer a basis for scientific and comprehensive appraisement of the quality of"Song di".