摘要
目的 :为建立注射用盐酸大观霉素细菌内毒素定量方法提供参考。方法 :建立动态浊度法测定细菌内毒素标准曲线,验证可靠性,考察样品对细菌内毒素检查的干扰情况,确定样品的最大无干扰浓度,验证方法的精密性和准确性,并进行初步应用。结果 :标准曲线可靠性验证中,相关系数r>0.99,标准曲线可靠。供试品用苯甲醇注射液溶解后稀释并添加内毒素标准品,制成供试品终浓度3.92 mg/m L及内毒素终浓度为0.25 Eu/m L的溶液,测得其回收率接近100%,供试品该浓度对内毒素测定的干扰较小。方法的精密度验证中,标准曲线各浓度点3次测量结果的变异系数均<10%,供试品加入标准曲线各浓度点的内毒素标准品后测定3次,结果的变异系数均<10%。准确率验证中,供试品中加入内毒素标准品终浓度为1.25,0.25,0.05 Eu/m L时回收率在91%~107%,加入内毒素终浓度为0.01 Eu/m L时回收率为73%和86%。另外,日常检测3批供试品的内毒素含量均小于限值,回收率在101%~103%。结论 :动态浊度法可用于定量检测注射用盐酸大观霉素的细菌内毒素。
Objective:To provide a reference for developing a method for determination of bacterial endotoxin content in spectinomycin hydrochloride for injection.Methods:The standard curve for determination of bacterial endotoxin by kinetic turbidimetric assay was plotted and verfieid for reliability.The interference of samples to determination of bacterial endotoxin was investigated to determine the maximum sample concentration without interference.The method was verified for precision and accuracy,and preliminarily applied.Results:In the reliability experiment of standard curve,all the r values of the curve were more than 0.99,indicating the validity of the standard curve.However,in the interference experiment,the samples were dissolved and diluted with benzil alcohol injection,added with standard endotoxin to prepare a solution at a final sample concentration of 3.92 mg/m L and a final endotoxin concentration of 0.25 Eu/m L.The recovery rate of endotoxin was nearly 100%,and the samples at the said concentration showed little interference to the determination of endotoxin.The coefficients of variation of determination results of standard endotoxin at various concentrations in three tests as well as the test samples added with standard endotoxin at varoius concentrations in three tests were less than 10%.In verification for accuracy,the recovery rates of test samples added with standard endotoxin to final concentrations of 1.25,0.25 and 0.05 Eu/m L were 91%~107%,while those at final endotoxin concentration of 0.01 Eu/m L were 73%and 86%.In addition,all the endotoxin contents in three batches of samples were less than the limited value by routine test,with recovery rates of 101%~103%.Conclusion:Kinetic turbidimetric assay is applicable to the quantitative determination of bacterial endotoxin in spectinomycin hydrochloride for injection.
作者
陈莉
张啸
刘永革
冯凤娇
Chen Li;Zhang Xiao;Liu Yong-ge;Feng Feng-jiao(Suzhou Institute for Drug Control,Jiangsu Suzhou 215104,China;Shandong Lukang Pharmaceutical Co.,Ltd.,Shangdong Jining,China;China Pharmaceutical University,Jiangsu Nanjing 211198,China)
出处
《中国执业药师》
CAS
2017年第6期45-48,共4页
China Licensed Pharmacist
关键词
动态浊度法
注射用盐酸大观霉素
内毒素
定量
Kinetic Turbidimetric Assay
Spectinomycin Hydrochloride for Injection
Endotoxin
Quantitative Determination
