摘要
目的建立衍生化高效液相色谱(HPLC)法、气相色谱-质谱联用(GC-MS)法测定大黄䗪虫丸7种动物药质量标志物的含量。方法选取10批次市售大黄䗪虫丸,采用酸水解法、正己烷提取法,提取其中的氨基酸和脂肪酸成分,衍生化HPLC法测定谷氨酸、缬氨酸、亮氨酸及色氨酸的含量,衍生化GC-MS法测定油酸、亚油酸及硬脂酸的含量。结果该方法经线性范围、加样回收率、精密度、稳定性和重复性等考察确证适合用于大黄䗪虫丸中7种动物药质量标志物的测定。两种方法的加样回收率分别为99.17%~101.53%,95.18%~98.07%;精密度的RSD分别为1.22%~2.72%,1.87%~2.92%;稳定性的RSD分别为1.17%~2.48%,1.58%~2.95%;重复性的RSD分别为1.12%~1.68%,1.20%~2.65%。结论所建立的方法精密度、稳定性、重复性符合测定要求,可用于大黄?虫丸动物药质量标志物的含量测定。
Objective To establish a derivatization HPLC and GC-MS method for the determination of seven animal drug quality markers in Dahuang Zhechong pills(DHZCP).Methods Ten batches of commercial DHZCP were selected.Amino acids and fatty acids were extracted by acid hydrolysis and n-hexane extraction.The contents of glutamic acid,valine,leucine and tryptophan were determined by derivatization HPLC,and the contents of oleic acid,linoleic acid and stearic acid were determined by derivatization GC-MS.Results The linear ranges,recoveries,precisions,stabilities and reproducibility of the method were confirmed to be suitable for the determination of the above components in DHZCP.The recoveries were 99.17%-101.53%,95.18%-98.07%,RSDs of precisions were1.22%-2.72%,1.87%-2.92%,RSDs of stabilities were 1.17%-2.48%,1.58%-2.95%,RSDs of reproducibility were 1.12%-1.68%,1.20%-2.65%.Conclusion The method has good precision,stability and repeatability,and can be used for the determination of quality markers of DHZCP.
作者
吴丽
付传奎
张子蒙
许珂嘉
黄艳
WU Li;FU Chuankui;ZHANG Zimeng;XU Kejia;HUANG Yan(School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023 Jiangsu,China;Inflammation and Immune Mediated Diseases Laboratory of Anhui Province,Hefei 230032 Anhui,China)
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2021年第11期1720-1725,共6页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
国家自然科学基金资助项目(81873287)
江苏省高校自然科学研究重点项目(18KJA360009)
安徽医科大学炎症免疫性疾病安徽省实验室开放课题(IMMDL202009)。
