中药化学成分定量分析方法学验证中精密度和准确度的探讨

目的：研究精密度、准确度和范围的具体考察方法。方法：采用RP—HPLC法，以厚朴药材为例，对该药中厚朴酚、和厚朴酚含量进行测定，在方法学验证过程中，重复性和回收率试验分别设计不同范围和不同考察方法。结果：重复性试验结果表明厚朴酚、和厚朴酚含量的RSD分别为2．5％～5．8％，2．5％～5．7％；平均回收率厚朴酚为95．1％～97．7％（RSD：2．2％～4．3％）；和厚朴酚为94．8％～97．7％（RSD=2．0％～7．5％）。结论：重复性RSD值随考察范围增大而增大，且同一浓度6份供试品溶液的测定结果与低、中、高浓度9份供试品溶液的测定结果方差非齐性。回收率RSD值亦随考察范围增大而增大。当药材取样量不同，根据被测成分含量按1：1添加对照品时，误差影响相对较小。而确定相同取样量，通过改变对照品加入量考察回收率时，9份样品测定结果RSD明显增大。

Study on Precision and Accuracy in Method Validation for Quantitative Analysis of Components in Traditional Chinese Medicine

Objective： To study the specific investigation method of precision, accuracy and range. Methods ： For determination of the contents of magnolol and honokilo in cortex magnoliae offieinalis by RP-HPLC, in different range, the repeatability and accuracy were evaluated by different methods. Results： For magnolol and honokilo, RSDs of the repeatability were 2. 5-5.8% and 2. 5-5.7%. The range within ten times. The average recoveries were 95. 1-97.7% ,with RSDs of 2. 2-4. 3% and 94. 8-97. 7% ,with RSDs of 2. 0-7.5% Conclusions： RSDs of the repeatability are increased as the range enlarged, and the variance is non-homogeneous between 6 and 9 determined results. RSDs of the recoveries are increased as the range enlarged. When the ratio of added and original amount is 1 ： 1, the error is little relatively But if recoveries are investigated by changing added amount of reference substance, RSD of the 9 sample results is obviously increased.