冻干甲型肝炎减毒活疫苗三氯甲烷残留量检测方法的建立及验证  

Establishment and verification of a detecting method for residual chloroform amount in freeze-dried live attenuated hepatitis A vaccine

作　　者：宋天扬 赵王丽 罗正辉 唐军 王璇 杨欢 杨东琼 乔燕 宋杰 Song Tianyang;Zhao Wangli;Luo Zhenghui;Tang Jun;Wang Xuan;Yang Huan;Yang Dongqiong;Qiao Yan;Song Jie(Department of Quality Control,Institute of Medical Biology,Chinese Academy of Medical Sciences,Key Laboratory for Quality Control and Evaluation of Vaccines and Biological Products,National Medical Products Administration,Kunming 650018,China)

机构地区：[1]中国医学科学院医学生物学研究所质量检定室,国家药品监督管理局疫苗及生物制品质量控制与评价重点实验室,昆明650018

出　　处：《国际生物制品学杂志》2022年第2期97-101,共5页International Journal of Biologicals

摘　　要：目的建立准确可靠检测冻干甲型肝炎减毒活疫苗中三氯甲烷残留量的方法。方法采用顶空气相色谱进行三氯甲烷残留量检测,用外标法计算三氯甲烷含量。对方法的专属性、线性、范围、准确度、精密度、定量限和耐用性进行验证。结果三氯甲烷峰5次进样峰面积的相对标准偏差小于5%,且与其他峰分离度大于1.5。阳性对照溶液在相应保留时间处可见三氯甲烷峰,阴性对照溶液无三氯甲烷峰。三氯甲烷的浓度在10~1000 ng/ml范围内与峰面积成线性关系。浓度为600 ng/ml的供试品溶液回收率在91.3%~99.0%之间,含量相对标准偏差均小于4%。定量限浓度为0.022 ng/ml。结论建立的三氯甲烷残留量检测方法具有良好的专属性、线性、范围、准确度、精密度和耐用性,符合定量检测的需求。Objective To establish an accurate and reliable method to determinate residual chloroform amount in freeze-dried live attenuated hepatitis A vaccine.Methods The content of chloroform was measured by headspace gas chromatography and calculated by external standard method.The specificity,linearity and range,accuracy,precision,detection limit,quantitative limit and durability of the analytical method were verified.Results The relative standard deviation(RSD)value of chloroform peak was less than 5%and the degree of separation from other peaks was greater than 1.5.The peak of chloroform in the positive solution was observed during the corresponding retention time,and there was no chloroform peak observed in the reference solution.The concentration of chloroform in the range of 10-1000 ng/ml was linearly related to the peak area.The solution recovery rates of the tested samples were between 91.3%and 99.0%with the concentrations of 600 ng/ml,and the RSDs were all less than 4%.The quantitative limit concentration was 0.022 ng/ml.Conclusion The established method has good specificity,linearity and range,accuracy,precision and durability,and accord with requirements of quantitative measurement.

关 键 词：三氯甲烷 色谱法 气相 肝炎疫苗 甲型 疫苗 减毒 方法验证 

分 类 号：R392.7[医药卫生—免疫学]