中国药典2010年版细菌内毒素检查凝胶法干扰试验判断模式研究

Research on judgment standard of interfering factors test of gel-clot technique for bacterial endotoxin test in Chinese Pharmacopoeia 2010 edition

目的：研究中国药典2010年版细菌内毒素检查凝胶法干扰试验判断模式的合理性,为中国药典2015年版细菌内毒素检查法的修订提供依据。方法：通过对1748批干扰试验结果统计分析,评价中国药典2010年版凝胶法干扰试验判断模式的合理性。结果：1748批试验结果中,试验结论为＂无法判断＂的批次共计132批,占7.55%,总结归纳产生＂无法判断＂结果的模式共有20种。凝胶法干扰实验为药典中收载的检测实验方法,为药品检验中的法定方法,不应出现对实验结果无法判断的情况,因此需完善。结论：建议中国药典2015年版细菌内毒素检查法凝胶法干扰试验判断模式参照美国药典36,欧洲药典7.0,日本药局方2011将凝胶法干扰试验结果判断模式修订为：＂按下式计算系列溶液B的反应终点浓度的几何平均值（Et）。Et=antilg（∑Xt/4）。式中Xt为系列溶液B的反应终点浓度的常用对数值。当Et在0.5λ～2λ（包括0.5λ和2λ）时,认为供试品在该浓度下无干扰作用。其他情况则认为供试品在该浓度下存在干扰作用。＂

Objective： To provide a basis for amendment of the current bacterial endotoxin test mentioned in Chinese Pharmacopoeia,and to investigate the scientific rationality of the judgment standard for interfering factors test of gel- clot technique for bacterial endotoxin test. Methods： The judgment standard for interfering factors test of gel- clot technique for bacterial endotoxin test recorded in Chinese Pharmacopoeia（ 2010 edition） was statistically analyzed by 1748 batches of results of interfering factors test. Results： A total of 132 out of 1748 batches were concluded as ＂ unable to determine＂,accounting for 7. 55%,and there were 20 types of models leading to ＂ unable to determine＂ results. Since the judgment standard of bacterial endotoxin interfering factors test in Chinese Pharmacopoeia（ 2010 edition） is the official method for drug test,experimental results that are ＂ unable to determine＂ should not occur. Therefore,the standard still requires improvement. Conclusion： It is suggested that the judgment standard of bacterial endotoxin interfering factors test in Chinese Pharmacopoeia（ 2015 edition） should refer to United States Pharmacopoeia 36,European Pharmacopoeia 7. 0,Japanese Pharmacopoeia 2011 and be revised into ＂ Determine the geometric mean endpoint（ Et） of Solution B by calculating the mean of the logarithms of the Solution B endpoint concentrations of the four replicate series and then taking the antilogarithm of the mean value,as indicated in the following formula： Et= antilg（ ∑Xt/4）. If the sensitivity of lysate determined in the presence of Solution B is not less than 0. 5λ and not greater than 2λ,the Sample Solution does not contain factors that interfere under the experimental conditions used. Otherwise,the Sample Solution to be examined interferes with the test. ＂