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方法确认-AAS标准加入法相关问题

问题1:进空白溶液、供试品溶液、供试品加标溶液后作出标准加入法最小线性二乘法标准曲线后,如果再进一针供试品溶液,能测出这针供试品溶液含有目标元素的浓度吗? 问题2:针对美国药典,标准加入法的定量限应该怎么做?不低于6份重复测定空白溶液的SD值,是吸光度的SD还是校准浓度的SD? 美国药典关于AAS的验证定量限描述: The limit of quantitation (QL) can be estimated by calculating the standard deviation of NLT six replicate measurements of a blank solution, divided by the slope of a standard curve, and multiplying by 10. If validating a procedure using the method of standard additions, the slope of standards applied to a solution of the test material is used. A measurement of a test solution prepared from a representative sample matrix spiked at the estimated QL concentration must be performed to confirm accuracy. If validating a procedure using the method of standard additions, the validation criterion applies to the final experimental result, not the spike recovery of the individual standard addition levels. Validation criteria: The analytical procedure should be capable of determining the analyte precisely and accurately at a level equivalent to 50% of the specification.
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