摘要
目的:建立盐酸右美托咪定中细菌内毒素定量检测方法,准确评估本品中的内毒素污染水平。方法:采用动态显色法,测定温度为(37±1)℃,检测波长为405 nm,预设达限值为95%,反应时间为3600 s。用细菌内毒素检查用水制备标准品或供试品系列溶液,并以内毒素检查用水作为阴性对照,分别与动态显色鲎试剂反应,通过标准曲线可靠性试验、盐酸右美托咪定干扰,确定盐酸右美托咪定的不干扰稀释倍数,并用该方法进行细菌内毒素定量检测。结果:标准曲线可靠性中回归方程为lgT=2.7936-0.3171lgC,相关系数∣r∣=0.9997,本品在选取的20000倍稀释浓度下对实验无干扰,干扰中回收率均在50%~200%之间,3批样品的内毒素含量均小于规定的限值,符合《中华人民共和国药典》2015年版要求和企业限值标准。结论:动态显色法可用于定量检测盐酸右美托咪定中的细菌内毒素含量。
Objective:To establish a quantitative method for the determination of bacterial endotoxin in dexmedetomidine hydrochloride to accurately assess endotoxin contamination level in the product.Methods:Kinetic chromogenic assay was performed at the following conditions:temperature of(37±1)℃,detection wavelength of 405 nm,preset limit value of 95%and reaction time of 3600 s.Bacterial endotoxin standard series solutions and test products were diluted with water for bacterial endotoxin test,and water for bacterial endotoxin test was used as a negative control.Then the endotoxin standard series solutions and test products groups reacted with kinetic chromogenic tachypleus amoebocyte lysate reagent,respectively.The quantitative measurement of bacterial endotoxin could be implemented by this method with the non-interfering dilution factor obtained by the reliability test of standard curve and interference test of the product.Results:In the reliability test of standard curve,the regression equation of the curve was lgT=2.7936-0.3171 lgC,the correlation coefficient of∣r∣was 0.9997.No interference was detected at dilution factor of 20,000 and the recovery values in the interference test all ranged from 50%to 200%.The endotoxin contents of three batches of samples were all below the prescribed limit,which met the requirements of Chinese Pharmacopoeia and limit criteria in industry.Conclusion:Kinetic chromogenic assay is used to quantitatively measure endotoxin in dexmedetomidine hydrochloride.
作者
谢美园
王尧尧
何跃芳
XIE Mei-yuan;WANG Yao-yao;HE Yue-fang(Yangtze River Pharmaceutical Group Co.,Ltd,Taizhou 225321,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2020年第9期1619-1623,共5页
Chinese Journal of Pharmaceutical Analysis
关键词
盐酸右美托咪定
动态显色法
内毒素污染
定量检测
干扰试验
dexmedetomidine hydrochloride
kinetic chromogenic assay
bacterial endotoxin contamination
quantitative detection
interference test
