GC测定甘草中5种有机氯农药残留量的不确定度评价

Evaluation of Measurement Uncertainty for Determination of Five Organochlorine Pesticide Residues in Glycyrrhizae Radix Et Rhizoma by GC

目的对GC测定甘草中α-BHC、β-BHC、γ-BHC、δ-BHC、五氯硝基苯5种有机氯农药残留量进行测量不确定度评价。方法通过统计学方法,量化不确定度分量,计算合成不确定度和扩展不确定度,并对测定中的各影响因素进行考察。结果α-BHC、β-BHC、γ-BHC、δ-BHC、五氯硝基苯的检测结果可表示为(0.085 0±0.008 4),(0.079 7±0.008 2),(0.055 8±0.005 6),(0.031 5±0.006 0),(0.039 4±0.005 7)μg·kg-1。对α-BHC、β-BHC检测结果影响最大的是供试液与对照液峰面积的进样重复性,而对γ-BHC、δ-BHC、五氯硝基苯检测结果影响最大的是供试液峰面积的测定重复性。结论测量不确定度评定方法的确立对于中药质量标准的研究具有重要意义。

OBJECTIVE To evaluate the measurement uncertainty for determination of the residues of α-BHC, β-BHC, γ-BHC, δ-BHC, and pentachloronitrobenzene in Glycyrrhizae Radix et Rhizoma. METHODS All the standard uncertainties were combined according to the appropriate rules to give combined standard uncertainty and an expanded standard uncertainty, and the factors influenced upon the measuration were analyzed. RESULTS The result of content determination was （0.085 0± 0.008 4）, （0.079 7±0.008 2）, （0.055 8±0.005 6）, （0.031 5±0.006 0）, （0.039 4±0.005 7）μg·kg^-1. The repeatability of area in standard and sample was the primary factor for determination of α-BHC and β-BHC; and the repeatability of area in sample was the primary factor for determination of γ-BHC, δ-BHC and pentachloronitrobenzene. CONCLUSION The establishment of the methodology for the evaluation of measurement uncertainty is important for the studies of Chinese materia medica standards.