摘要
基于聚氧乙烯脱水山梨醇单油酸酯（吐温80）中聚乙氧基团与硫氰酸钻铵生成可溶于有机溶剂的蓝色复合物的显色反应，建立一种适用于药用辅料吐温80快速、准确定量的比色测定方法，为中药注射剂质量控制提供可靠技术手段。在反应动力学研究基础上，对显色反应温度、时间和萃取有机溶剂等关键条件进行优化，并以中药注射剂苦木注射液为供试品进行系统的方法学验证和适用性考察。最终确定在试样溶液中加入3mL硫氰酸钴铵溶液，于沸水浴中显色反应2h，冷却至室温后精密加入二氯甲烷5mL萃取显色产物，根据萃取溶液在623llm波长处的吸光度计算试样中吐温80含量。在优化测定条件下，吐温80在0．8-3．0mg与吸光度呈良好线性关系（Y=0．258x-0．047，r=0．9996，n=6），精密度RSD〈2．0％，平均回收率为99．66％。该方法可快速、准确测定药物制剂中吐温80的含量，适用于中药注射剂的质量控制。
Based on the fact that chromogenic reaction of blue complex, a reaction product which can be dissolved in organic sol- vents, can be realized by polyethoxy and ammonium thiocyanate in tween 80, a rapid and accurate way for the determination for twecn 80 in pharmaceutical adjuvant was established in this study, providing reliable technical means for quality control of traditional Chinese medicine injections. Based on the study of reaction kinetics, chromogenic reaction temperature and time, as well as extraction of organ- ic solvents and other key conditions were optimized, and Kumu injection was used as the test material for method validation and appli- cability investigation. It was finally determined that 3 mL ammonium thiocyanate solution was added in the sample solution, and the re- action was carried out in a boiling water bath for 2 h. After cooling to room temperature, 5 mL of dichloromethane was added to extract the chromogenic product. The absorbance value was measured at the wavelength of 623 nm to calculate the tween 80 content in the sam- ple. Under optimized conditions, tween 80 solution showed a good linear relationship with the absorbance in the range from 0.8 mg to 3.0 mg. The linear regression equation was y = 0. 258x - 0. 047. The correlation coefficient r was 0. 999 6. Under the experimental conditions, the average recovery was 99.66%, and the precision RSD was less than 2. 0%. The results showed that this method can quickly and accurately determine the content of tween 80 in Kumu injection, and it could be applicable to the quality control of tradi-tional Chinese medicine injections.
作者
杨倩文
王宁
张杰
许卉
李志勇
YANG Qian-wen;WANG Ning;ZHANG Jie;XU Hui;LI Zhi-yong(Center of Advanced Drug Delivery System and Biotech Drugs in Universities of Shandong, Key Laboratory of Molecular Pharmacology and Drug Evaluation, Ministry of Education, Yantai University, Yantai 264005, China;State Key Laboratory of State Key Laboratory of Innovative Natural Medicine and Traditional Chinese Medicine Injections, Ganzhou 341000, China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2018年第4期743-747,共5页
China Journal of Chinese Materia Medica
基金
国家“重大新药创新”科技重大专项(2017ZX09301039)
