原文由 quanchaoli 发表:
Dear Sir,
I studied the chromatograms (recd. from Tushar) of analysis of Shenyang Rifampicin, B.No. 20059136 and the observations are as follows.
尊敬的先生:
我分析了沈阳抗生素厂利福平批号为20059136的色谱并得出以下结论。
1) As we were getting the extra ,unseparated , duplet or splitted Peak in our analysis ( done in presence of Chinese people even with using their column and method ) these chromatograms are also exhibiting the unseparated, duplet , splited extra peak at the R.T. 2.42 and 2.54 having the equal basemarking width of only one peak compaired to other peaks of the impurities.
我们在分析时得到了额外的未分离的峰、对峰或裂峰(在中方人员面前当场试验,甚至采用中方人员提供的色谱柱和分析方法),这些色谱图同样也存在额外的未分离的峰、对峰和裂峰,与杂质的其它峰相比,在保留时间为2.42和2.54分钟时出的是底部峰宽相近的单峰。
2) All the Chromatograms ( received ) i.e Resolution solution, 3 Standards, Rifampicin Dilute test soln. , Assay solution are chromatographed at the responce of 0.18 Au but only the chromatogram of Test preparation showing impurities is chromatographed at the response 0.44 Au to hide the unseparated problematic impurity peak.
所有的色谱图(收到的),也就是分离溶液,3个标准液,利福平稀释液,分析液色谱的峰响应值为0.18 Au,但只有检测液表明杂质峰响应值为0.44 Au,隐藏了未分离的有疑问的杂质峰。
3) We can't understand why the integration parameters are changed for this particular chromatogram. The reason is that , because the peak can not be separated individually in two, acceptable baseline peaks by using the USP method they forcebly ( By manual integration ) marked it in two peaks by minimising the height visuality to show two separate peaks less than 1%
对于这个特别的谱图我们不明白积分参数为什么改变了。原因是因为色谱峰不能分成两个独立的峰,通过USP方法手动积分,以不超过1%的比例减小峰的视觉高度,强行将此峰标记为两个可接受的基线峰。
4) As per the chromatograms area Rifa Quinone is not 0.376% but it is 0.808% and problematic peak is 1.187% as considered to a single peak. If it is considered as 2 unseparated peaks the the % will be 0.353% and 0.834%
根据谱图,醌氏利福平峰面积不是0.376%,而是0.808%,如果只考虑是一个峰的话,存在问题的峰是1.187%。如果考虑是两个未分开的峰,那么百分比是0.353%和0.834%。
5) The total impurities ( O.T. Rifa Quinone) calculated upon party's chromatograms is 2.958% ( Lim = NMT 3.5% )
So if at the time of release we will pass the material less than 97% purity what will be the status of the product within expiry
period ?
根据对方的谱图,总杂质含量(O.T.醌氏利福平)为2.958%(Lim=NMT 3.5%)
因此如果在来料放行时杂质含量就是97%,那么产品在以后(有效期内)又将如何?
So again the matter remains unanswered whether to release these materials taking in to account the calculated Risks in future or Reject these to avoid the Risks of inviting the impurities in our products.
Pralhad
所以问题仍然没有得到解决,在产品放行的时候,你们是否考虑到了来料未来的预计风险,或者拒收来料来避免给我们产品带来杂质的危险。
Pralhad