蟾蜍油炮制工艺及质量评价方法研究

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。

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

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.