二黄栓制备工艺及其含量测定方法  

Preparation Process and Content Determination Method of Erhuang Suppository

作　　者：苟欢 刘嵘 熊微 施春阳 方建国[1] 王文清 GOU Huan;LIU Rong;XIONG Wei;SHI Chunyang;FANG Jianguo;WANG Wenqing(Department of Pharmacy,Huazhong University of Science and Technology,Wuhan 430030,China;Department of Gynecology,Tongji Hospital,Tongji Medical College,Huazhong University of Science and Technology,Wuhan 430030,China)

机构地区：[1]华中科技大学同济医学院附属同济医院药学部,武汉430030 [2]华中科技大学同济医学院附属同济医院妇科,武汉430030

出　　处：《医药导报》2023年第11期1718-1722,共5页Herald of Medicine

基　　金：国家自然科学基金资助项目(81403166);湖北省自然科学基金资助项目(2019CFB744);国家药品监督管理局中药质量控制重点实验室(湖北)开放基金资助项目(2022HBKFZ002)。

摘　　要：目的建立二黄栓制备工艺及其中二硫化二砷含量测定方法。方法采用G1-熵权法结合正交设计,以外观性状、质量差异和融变时限为评分指标,考察基质类型及用量、熔融温度、搅拌时间、注模温度,得出最佳制备工艺。样品经不同前处理方法处理后,分别采用碘量法与原子吸收分光光度法对二硫化二砷进行定量分析。结果以混合脂肪酸甘油酯为基质,在60℃水浴条件下熔融,搅拌20 min,冷却至50℃注模为最佳制备工艺。二硫化二砷取样量在59.88~249.48 mg范围内与碘滴定液消耗体积(mL)线性关系良好,Y=0.1870 X+0.5275,r=0.9990,平均加样回收率101.48%,RSD1.16%(n=6);原子吸收分光光度法中砷元素在20~100μg·mL^(-1)范围内与吸光度线性关系良好,Y=6.3530×10^(-3)X+0.0558,r=0.9986,平均加样回收率99.31%~105.20%,RSD<3.05%(n=9)。结论所建立的二黄栓制备工艺流畅、稳定,对工业化生产具有较好借鉴价值;两种含量测定方法准确,灵敏度高,重复性好,均可用于二黄栓中二硫化二砷定量分析。Objective To establish the preparation process of Erhuang Suppository and to set up a content determination method of the arsenic disulfide(As 2 S 2)in Erhuang suppository.Methods The G1-entropy weight method combined with the orthogonal design was used to optimize the preparation process,with the evaluation indexes of appearance,weight difference,and disintegration.And the matrix type,dosage,melting temperature,stirring time and filling temperature were investigated to find out best preparation process.After different pretreatment methods,the samples of As 2 S 2 in Erhuang suppository was analyzed quantitatively by iodometry and atomic absorption spectrometry(AAS).Results The best preparation process was as followed:mixed with fatty acid glyceride as a matrix,melting temperature of 60℃,stirring time of 20 min,and injection temperature of 50℃.The linearity of As 2 S 2 was good within the range of 59.88-249.48 mg,and the regression equation was Y=0.1870 X+0.5275,r=0.9990.The average recovery was 101.48%with RSD of 1.16%(n=6).The atomic absorption spectrophotometry showed good linearity ranging from 20 to 100μg·mL^(-1),the regression equation was Y=6.3530×10^(-3)X+0.0558,r=0.9986,and the average recovery ranged from 99.31%-105.20%,RSD<3.05%(n=9).Conclusion The preparation process of Erhuang suppository is smooth and stable,and it has good practical application value in industrial production.Both two determination methods are accurate,highly sensitive and good repeatable,which can be used for the quality control of As 2 S 2 in Erhuang suppository.

关 键 词：二黄栓 二硫化二砷 雄黄 G1-熵权法 正交实验 碘量法 原子吸收分光光度法 

分 类 号：R286[医药卫生—中药学] R924.1[医药卫生—中医学]