三叶青藤叶配方颗粒的质量标准研究及其5种有效成分的含量测定
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篇名: 三叶青藤叶配方颗粒的质量标准研究及其5种有效成分的含量测定
TITLE: Study on the Quality Standard of Tetrastigma hemsleyanum Stem and Leaves Dispensing Granules and Content Determination of 5 Active Ingredients
摘要: 目的:建立三叶青藤叶配方颗粒的质量标准,并同时测定其中5种有效成分的含量。方法:采用薄层色谱法(TLC)对三叶青藤叶配方颗粒中绿原酸、异荭草苷、异荭草苷-2′-O-鼠李糖苷进行定性鉴别。采用紫外分光光度法测定3批样品中总黄酮(以异荭草苷计)含量,并对其粒度、水分、溶化性及装量差异进行检查。以异荭草苷为内参物计算其余成分的相对校正因子,采用一测多评法测定样品中新绿原酸、绿原酸、荭草苷、异荭草苷、异荭草苷-2′-O-鼠李糖苷的含量,并与外标法测定结果进行比较。结果:绿原酸、异荭草苷、异荭草苷-2′-O-鼠李糖苷TLC图斑点清晰,分离度好,阴性对照无干扰。样品中异荭草苷检测质量浓度的线性范围为7.73~61.82μg/mL(r=0.9999);精密度、稳定性、重复性试验的RSD均小于2%;加样回收率为93.75%~97.85%(RSD=1.41%,n=6)。3批样品不能通过一号筛且能通过五号筛的平均百分率分别为1.51%、1.55%、1.29%(n=3),含水量分别为4.63%、5.18%、4.03%(n=3);颗粒均在5min内溶化;装量差异为4.8%~5.0%,均符合2015年版《中国药典》(四部)颗粒剂的相关规定。一测多评法测定5种成分质量浓度的线性范围分别为2.325~93μg/mL(r=0.9999)、5.125~205μg/mL(r=0.9999)、1.150~46μg/mL(r=0.9993)、2.625~105μg/mL(r=0.9999)、4.725~189μg/mL(r=0.9999);精密度、稳定性、重复性试验的RSD均小于3%;加样回收率分别为99.78%~106.13%(RSD=2.33%,n=6)、95.07%~103.32%(RSD=2.72%,n=6)、97.17%~105.43%(RSD=2.98%,n=6)、95.52%~101.33%(RSD=2.46%,n=6)、99.42%~105.56%(RSD=2.34%,n=6)。异荭草苷相对于新绿原酸、绿原酸、荭草苷、异荭草苷-2′-O-鼠李糖苷的相对校正因子分别为0.731、0.805、0.821、0.590;一测多评法测得5种成分的含量分别为0.828~1.123、2.379~3.118、0.281~0.880、1.039~1.393、2.121~3.209mg/g,外标法测得的含量分别为0.803~1.099、2.345~3.085、0.269~0.872、1.039~1.393、2.113~3.201mg/g;两种方法测定结果比较,差异均无统计学意义(P>0.05)。结论:所建质量标准简便、快速,可用于三叶青藤叶配方颗粒的质量控制;所建一测多评法准确、高效,可用于同时测定三叶青藤叶配方颗粒中5种有效成分的含量。
ABSTRACT: OBJECTIVE:To estab lish the quality standard of Tetrastigma hemsleyanum stem and leaves dispensing granules , and to determine the contents of 5 active ingredients simultaneously. METHODS : Chlorogenic acid , isoorientin and isoorientin-2′-O-rhamnoside in T. hemsleyanum stem and leaves dispensing granules were identified by TLC. The total flavonoids of the 3 batches granules were determined by UV spectrophotometry (by isoorientin ). The granule sizes ,moisture contents , dissolvability,and content uniformity were determined. Using isoorientin as internal reference ,relative correction factors of other components were established. QAMS method was adopted to determine the contents of neochlorogenic acid ,chlorogenic acid , orientin,isoorientin and isoorientin- 2′-O-rhamnoside,which were compared with the results of ESM method. RESULTS :TLC spots of chlorogenic acid ,isoorientin and isoorientin- 2′-O-rhamnoside were clear and well-separated ,without interference from negative control. The linear range of isoorientin were 7.73-61.82 μ g/mL(r=0.999 9). RSDs of precision ,stability and reproducibility tests were all lower than 2%. The recoveries were 93.75%-97.85%(RSD=1.41%,n=6). The average percentages that the 3 batches granules could not pass through sieve No. 1 - moisture contents were 4.63%,5.18% and 4.03%(n=3). were dissolved within 5 min ,and content uniformity were 4.8%-5.0%. Which were all in line with the relevant provi-sions of granules in 2015 edition of Chinese Pharmacopoeia . The linear range of 5 ingredients were 2.325-93 μg/mL(r=0.999 9),5.125-205 μg/mL(r=0.999 9),1.150- 46 μg/mL(r=0.999 3),2.625-105 μg/mL(r=0.999 9),4.725-189 μg/mL(r=0.999 9),respectively. RSD of precision ,stability and reproducibility tests were all lower than 3%. The recoveries were 99.78%-106.13%(RSD=2.33%,n=6),95.07%-103.32% (RSD=2.72%,n=6),97.17%-105.43%(RSD=2.98%,n=6),95.52%-101.33%(RSD=2.46%,n=6),99.42%-105.56% (RSD=2.34%,n=6). Using isoorientin as internal reference ,relative correction factors of neochlorogenic acid ,chlorogenic acid , isoorientin and isoorientin- 2′-O-rhamnoside were 0.731,0.805,0.821,0.590,respectively. The contents were 0.828-1.123, 2.379-3.118,0.281-0.880,1.039-1.393,2.121-3.209 mg/g by QAMS method ,while the contents were 0.803-1.099,2.345-3.085, 0.269-0.872,1.309-1.393,2.113-3.201 mg/g by ESM method ,there was no significant difference in the content determination results between QAMS and ESM method (P>0.05). CONCLUSIONS :Established quality standard is simple and rapid ,and can be used for quality control of T. hemsleyanum stem and leaves dispensing granules. Established QAMS method is accurate and efficient,and it can be used for simultaneous determination of 5 active ingredients of T. hemsleyanum stem and levels dispensing granules.
期刊: 2020年第31卷第08期
作者: 谢平,陈丹,洪丽婷,刘秀棉,余文静,熊朝栋,廖淑彬,刘永静
AUTHORS: XIE Ping, CHEN Dan,HONG Liting,LIU Xiumian,YU Wenjing,XIONG Chaodong,LIAO Shubin,LIU Yongjing
关键字: 三叶青藤叶配方颗粒;质量控制;薄层色谱法;紫外分分光光度法;一测多评法;含量测定
KEYWORDS: Tetrastigma hemsleyanvn stem and leaves dispensing granules ;Quality control ;TLC;UV;QAMS;Content
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