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【答案】应助回帖
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koalaone: 金币+1 2012-11-13 07:54:07
My experience as your reference:
1. 气相测残留溶剂的回收率: 80%-120%.
2. 原料残留溶剂的方法学验证，但测得的回收率比较高: since you are working on 原料残留溶剂, you cannot add your reference standard to placebo to measure your recovery. You only can use 原料 + 80%, 100%, 120% working standard solution (100% working standard solution is ICH limit level) to calculate recovery%. To troubleshooting 回收率比较高
1) When you measure your sample(原料), you may measure your sample n=3 or 5 to get mean value.
2) Prepare sample in a fast or correct way (我100mg定容到1ml, this is not normal way to do, the volume is too low that will be difficult to manage sample evaporation) to avoid sample evaporation.
3) Sample + matrix interaction may cause this issue too. You can try different solvent (matrix) to dissolve your sample.
4) If still cannot get right recovery%, you may try internal standard or external standard method. |
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