沉香中沉香四醇的测量不确定度评估

目的:建立HPLC定量分析沉香药材中沉香四醇含量的测量不确定度的评定方法,找出影响不确定度的因素,为沉香药材质量控制提供科学依据。方法:用HPLC方法测定沉香四醇的含量,并根据《测量不确定度评定与表示》(JJF1059.1-2012)中的规定评估其不确定度,通过统计分析,量化不确定分量,最终确定测量结果的扩展不确定度和置信水平。结果:5批沉香药材中沉香四醇含量测定的不确定度评估结果为(2.80±0.45),(5.13±0.82),(13.86±2.21),(74.86±11.87),(125.71±19.94)g·L~(-1)。发现测量不确定度的主要影响因素有沉香样品的均匀性、称量、配制浓度及高效液相色谱仪性能4个类型,通过严格按照四分法取样沉香样品、确保称量介质保持干燥、正确或规范使用玻璃器皿和精密仪器、可有效减少样品痕量分析的误差。结论:该方法可用于HPLC法测定沉香药材中沉香四醇含量的不确定度分析,方法简便,测量结果不确定度纳入标准制定,有利于标准痕量更加合理,对沉香药材痕量分析方法的建立和质量标准的制定具有重要意义。

Evaluation of Measurement Uncertainty for Determination of Agarotetrol in Aquilariae Lignum Resinatum

Objective: To find out the impacting factors on uncertainty by establishing a HPLC method for a quantitative analysis of agarotetrol, in order to provide the evidence for quality control of traditional Chinese medicinal materials of Aquilariae Lignum Resinatum. Method: Agarotetrol in Aquilariae Lignum Resinatum was determined by HPLC, and the uncertainty was evaluated according to JJF1059.01-2012.The uncertainty components were quantified through a statistical analysis, and extended uncertainty and confidence level were finally determined. Result: The uncertainty evaluation results for the content determination of agarotetrol from five samples was (2.80±0.45), (5.13±0.82), (13.86±2.21), (74.86±11.87),(125.71±19.94)g·L^-1. Sample homogeneity, weighing, compound concentration and HPLC property were the major factors to measure the uncertainty. The error of sample trace analysis could be reduced by quartering samples, drying weighing medium and correctly or regularly using glassware and precision instruments. Conclusion: The method can be used for uncertainty analysis of content of agarotetrol in Aquilariae Lignum Resinatum, which makes the standard trace amount more rational and significant to establish uncertainty analysis methods and quality standard for Chinese medicinal materials of Aquilariae Lignum Resinatum.