小儿柴胡退热栓的制备及质量标准研究  

Preparation and Quality Standard of Xiaoer Chaihu Tuire Suppository

作　　者：王莉博 刘泽干 雷攀[2] 黄良永[2] 叶方[2] 黄小凤 王淑慧 杜士明[2,3] WANG Libo;LIU Zegan;LEI Pan;HUANG Liangyong;YE Fang;HUANG Xiaofeng;WANG Shuhui;DU Shiming(College of Pharmacy,Hubei University of Medicine,Shiyan,Hubei,China 442000;Affiliated Taihe Hospital of Hubei University of Medicine,Shiyan,Hubei,China 442000;Hubei Key Laboratory of Wudang Local Chinese Medicine Research,Hubei University of Medicine,Shiyan,Hubei,China 442000)

机构地区：[1]湖北医药学院药学院,湖北十堰442000 [2]湖北医药学院附属太和医院,湖北十堰442000 [3]武当特色中药研究湖北省重点实验室·湖北医药学院,湖北十堰442000

出　　处：《中国药业》2021年第16期39-43,共5页China Pharmaceuticals

基　　金：武当特色中药研究湖北省重点实验室开放课题[WDCM2019015];湖北省十堰市科技局科研项目[16Y21]。

摘　　要：目的优选小儿柴胡退热栓的最佳制备工艺,并建立其质量标准。方法采用水蒸气蒸馏法提取柴胡挥发油并采用β-环糊精进行包合,以正交试验优化柴胡挥发油提取和β-环糊精包合工艺参数,采用熔融法制备小儿柴胡退热栓;依据2015年版《中国药典(四部)》通则0107栓剂项下的质量要求拟订该制剂的质量标准。采用气相色谱串联质谱(GC-MS)法测定小儿柴胡退热栓中正己醛及正庚醛的含量。结果柴胡挥发油最佳提取工艺条件为料液比1∶10(g∶m L)、浸泡8 h、提取2 h;500 g柴胡饮片提取的挥发油精馏液250 m L,最佳包合工艺条件为β-环糊精用量50 g、50℃下包合2 h;500 g柴胡饮片制得小儿柴胡退热栓100粒,性状、质量差异、融变时限、微生物限度等均符合药典规定。正己醛、正庚醛质量浓度的线性范围分别为6.19~99.00μg/m L和4.90~78.40μg/m L(r均为0.998,n=5);精密度、稳定性、重复性试验的RSD均小于3%;平均加样回收率分别为101.69%和100.94%,RSD分别为1.84%和1.28%(n=9)。结论优选的小儿柴胡退热栓的制备工艺合理、可行,所制备栓剂符合质量标准要求。Objective To optimize the preparation process of Xiaoer Chaihu Tuire Suppository and establish its quality standard.Methods The volatile oil of Bupleurum chinense was extracted by steam distillation,and the volatile oil of Bupleurum chinense was encapsulated byβ-cyclodextrin.The extraction process of the volatile oil of Bupleurum chinense and the parameters of the inclusion process ofβ-cyclodextrin were optimized by the orthogonal test.Xiaoer Chaihu Tuire Suppository was prepared by melting method.The quality standard of the preparation was formulated according to the quality requirements of the general rule 0107 of the Chinese Pharmacopoeia(2015 Edition,VolumeⅣ).The contents of n-hexanal and n-heptanaldehyde in Xiaoer Chaihu Tuire Suppository were determined by gas chromatography-mass spectrometry(GC-MS).Results The optimum extraction conditions of the volatile oil of Bupleurum chinense were as follows:the solid-liquid ratio was 1∶10(g∶m L),the soaking time was 8 h and the extraction time was2 h.250 m L of distillation of volatile oil was extracted from 500 g of Bupleurum chinense decoction pieces,and its optimum inclusion process conditions were as follows:the amount ofβ-cyclodextrin was 50 g and the inclusion process was carried out at 50℃for 2 h.A total of 100 Xiaoer Chaihu Tuire Suppositories were prepared from 500 g of Bupleurum chinense decoction pieces,and the properties,quality differences,melting time limit and microbial limit all met the requirements of the Chinese Pharmacopoeia.The linear ranges of n-hexanal and n-heptanaldehyde were 6.19-99.00μg/m L and 4.90-78.40μg/m L(r=0.998,n=5),respectively.The RSDs of precision,stability and repeatability tests were less than 3%.The average recoveries of n-hexanal and n-heptanaldehyde were101.69%and 100.94%with RSDs of 1.84%and 1.28%(n=9),respectively.Conclusion The optimized preparation process of Xiaoer Chaihu Tuire Suppository is reasonable and feasible,and the prepared suppository can meet the requirements of quality standard.

关 键 词：柴胡挥发油 Β-环糊精 小儿柴胡退热栓 制备工艺 质量标准 

分 类 号：R932[医药卫生—生药学] R288[医药卫生—药学]