总有机碳检测法在五味子提取清洁验证中的应用  

Application of Total Organic Carbon Method in Cleaning Validation for Extraction of Schisandra chinensis

作　　者：徐婷 陶金 岳镭 XU Ting;TAO Jin;YUE Lei(Shanghai Hutchison Pharmaceuticals)

机构地区：[1]上海和黄药业有限公司

出　　处：《中国标准化》2023年第19期224-229,共6页China Standardization

摘　　要：为了证明总有机碳(total organic carbon,TOC)检测法可用于中药材五味子提取设备的清洁验证。采用淋洗法与擦拭法取样,并验证TOC检测法的线性、精密度与准确度、检测限(LOD)与定量限(LOQ)、取样回收率与稳定性,评价总有机碳法用于中成药清洁验证的效果。结果表明,五味子浓度(x)在0.024~0.960 mg/L范围内时,其与TOC值(y)呈良好的线性关系,回归方程为y=218.8x-0.033,r 2=0.999;精密度与准确度的相对标准偏差(RSD)均不超过4%;检测限(LOD)为3.84μg/L,定量限(LOQ)为11.5μg/L;采用两种方式取样,在低、中、高浓度淋洗法平均取样回收率分别为63.91%、81.00%、81.11%,擦拭法平均取样回收率分别为87.50%、83.33%、106.94%;样品溶液分别在0、4、8、24、28、48 h进行TOC检测,RSD为5.21%;应用于生产中减压浓缩罐设备残留量计算,结果符合限度浓度要求。TOC法可用于五味子提取生产清洁验证,可广泛应用于多活性成分的中药制药生产。To prove that the total organic carbon(TOC)method can be applied in cleaning validation(CV)for extraction of Schisandra chinensis.Sampling by rinsing and swabbing methods the TOC method was verifi ed for linearity,precision and accuracy,limit of detection(LOD)and limit of quantitation(LOQ),sampling recovery rate,stability,which was used for evaluating the effectiveness of facilities cleaning of Chinese patent medicine.The Schisandra chinensis extract concentration(x)at a range of 0.024~0.960 mg/L showed good linear relationship to TOC value(y),of which the linear regression equation was y=218.8x-0.033,r 2=0.999.Both the RSDs in accuracy and precision tests were less than 4%.LOD was 3.8μg/L,LOQ was 11.5μg/L.Sampling by two methods,the average sampling recoveries of rinsing method at low,medium and high concentrations were 63.91%,81.00%and 81.11%respectively,and those of swabbing method were 87.50%,83.33%and 106.94%respectively.The test solutions were detected at 0,4,8,24,28,and 48 h respectively by TOC method,with RSD of 5.21%.When applied in the production,the residual concentration of vacuum concentration tank residues were lower than allowable level.The TOC method can be used for CV of Schisandra chinensis extract,which means that it can be widely used for CV of traditional Chinese medicine production with complex components.

关 键 词：总有机碳检测法 五味子 清洁验证 擦拭法取样 淋洗法取样 

分 类 号：R284[医药卫生—中药学]