酸枣仁中黄曲霉毒素B1残留测定的不确定度评定

Uncertainty Evaluation of Determination of Aflatoxin B1 in Zizyphi Spinosi Semen by HPLC

目的对高效液相色谱法测定酸枣仁中黄曲霉毒素B1残留量的不确定度进行评定。方法对HPLC测定酸枣仁中黄曲霉毒素B1残留量的全过程进行分析,同时结合酸枣仁中黄曲霉毒素B1的HPLC方法验证数据,对分析过程中称量、供试品溶液及对照品溶液制备等影响因素引起的不确定度进行评价,最后根据各分量计算出合成不确定度并进行了扩展。结果酸枣仁中黄曲霉毒素残留量B1为6.218μg.kg-1,置信概率(P)为95%时,其扩展不确定度为0.496μg.kg-1。结论该方法适用于HPLC测定酸枣仁中黄曲霉毒素B1残留量的不确定度评定,为黄曲霉毒素分析过程的不确定度评定提供了重要参考。

OBJECTIVE To establish an uncertainty analysis method for determination of aflatoxin B1 in Zizyphi Spinosi Semen by HPLC. METHODS The uncertainty arising from various factors in the whole process of analysis was evaluated. The facilitated method of evaluation was achieved by analysis of the uncertainty sources arising from the procedure of analysis and by using the valida- tion data of assay. All the standard uncertainties were then combined according to the appropriate rules to give a combined standard un- certainty and an expanded standard uncertainty. RESULTS When the residue level of aflatoxin B1 in Zizyphi Spinosi Semen was 6. 218 μg·kg-1, the expanded standard uncertainty for allatoxin B1 was 0. 496μg·kg-1 （p =95 % ）. CONCLUSION This meth- od is applicable for the uncertainty evaluation of ailatoxin B1 residue determination. It provides an important reference for the uncertain- ty evaluation for the aflatoxin B1 residue determination in Zizypbi Spinosi Semen.