蟾蜍油炮制工艺及质量评价方法研究  

Research on the Processing Technology and Quality Evaluation Methods of Bufonis Oviductus

作　　者：牟丽燕 高萌 陆兔林[1,2] 毛春芹[1,2] 季德[1,2] 苏联麟 郭志俊 高波 罗川 殷放宙[1,2] MU Li-yan;GAO Meng;LU Tu-lin;MAO Chun-qin;JI De;SU Lian-lin;GUO Zhi-jun;GAO Bo;LUO Chuan;YIN Fang-zhou(School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210000,China;Jiangsu Key Laboratory of Chinese Medicine Processing,Nanjing 210000,China;China Resources Sanjiu Modern Traditional Chinese Medicine Pharmaceutical Co.,Ltd.,Huizhou 516000,China;Anhui Huarun Jinchan Pharmaceutical Co.,Ltd.,Huaibei 235000,China)

机构地区：[1]南京中医药大学药学院,江苏南京210000 [2]江苏省中药炮制重点实验室,江苏南京210000 [3]华润三九现代中药制药有限公司,广东惠州516000 [4]安徽华润金蟾药业有限公司,安徽淮北235000

出　　处：《中国现代中药》2024年第2期357-363,共7页Modern Chinese Medicine

基　　金：国家重点研发计划项目(2018YFC1707000)。

摘　　要：目的:优化蟾蜍油干燥工艺,并建立以高效液相色谱法(HPLC)指纹图谱及氨基酸含量测定为主的质量评价方法。方法:以氨基酸和浸出物为指标,进行蟾蜍油热风干燥、自然阴干、冷冻干燥及真空干燥工艺的优选,分别考察了热风干燥的加热温度、加热时间、物料厚度,冷冻干燥的预冻时间、冷冻干燥时间,真空干燥的温度及时间对蟾蜍油的影响。采用HPLC建立15批蟾蜍油的指纹图谱,确定共有峰并进行相似度评价;同时,采用柱前衍生化法测定氨基酸含量。结果:蟾蜍油最佳工艺为不叠加样本,50℃热风干燥11 h。HPLC指纹图谱中共确定7个共有峰,相似度均大于0.99;异亮氨酸、亮氨酸、苯丙氨酸、赖氨酸质量分数分别为0.40%~0.57%、0.57%~0.78%、0.54%~0.75%、0.26%~0.86%。结论:所确定的工艺及质量评价方法简便、重复性好,可为蟾蜍油的加工炮制及质量评价提供参考。Objective:To optimize the drying process technology of Bufonis Oviductus,and establish a quality evaluation method based on high-performance liquid chromatography(HPLC)fingerprint and amino acid content determination.Methods:Amino acids and extracts were used as indicators in the optimization of hot-air-drying,nature-shadow-drying,freeze-drying and vacuum-drying for Bufonis Oviductus.The impacts of several factors on the Bufonis oviductus were investigated including,heating temperature,heating time,material thickness,pre-freezing time,freeze-drying time,vacuum drying temperature,and vacuum drying time.The fingerprints of 15 batches samples were established by HPLC.Common peaks were determined and their similarities were evaluated.Pre-column derivatization was also used to determine the content of amino acids.Results:The optimum conditions for processing Bufonis Oviductus were determined as hot-air-drying at 50°C for 11 h with the samples placed in a single layer.A total of 7 common peaks were identified in the HPLC fingerprint of Bufonis Oviductus,and the similarities of 15 samples were greater than 0.99.The contents of isoleucine,leucine,phenylalanine and lysine are 0.40%-0.57%,0.57%-0.78%,0.54%-0.75%,0.26%-0.86%,respectively.Conclusion:The determined drying process of Bufonis Oviductus as well as quality evaluation methods are simple and reproducible,which can provide a reference for the processing and quality evaluation of Bufonis Oviductus.

关 键 词：蟾蜍油 干燥工艺 高效液相色谱法 指纹图谱 氨基酸 

分 类 号：R283[医药卫生—中药学]