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高效液相色谱光化学衍生法测定 延胡索中黄曲霉毒素的不确定度评定

宁知贵1,洪家顺1,曾慧婷2,李道成1,彭思思1,王裕成1*

(1 江西省道地药材质量评价研究中心,江西  赣江新区  330029;

2 江西省中医药研究院,江西  南昌  330000)

摘要:采用《中国药典》2020 年版四部黄曲霉毒素测定法中液相色谱法对延胡索中黄曲霉毒素G2(Aflatoxin G2,AFG2)、黄曲霉毒素G1(Aflatoxin G1,AFG1)、黄曲霉毒素B2(Aflatoxin B2,AFB2)、黄曲霉毒素B1(Aflatoxin B1,AFB1)进行不确定度评估。参照《化学分析中不确定度的评估指南》(CNAS-GL006—2019)、《测量不确定度评定和表示》(GB/T 27418—2017)以及《测量不确定度评定和表示》(JJF1059.1—2012)的有关规定,对测定延胡索中黄曲霉毒素的不确定度来源进行分析。通过对不确定进行量化和合成,k 为2 时,得出延胡索中AFB1、AFB2、AFG1、AFG2扩展不确定度分别为0.77、0.22、0.76、0.24mg/kg。结果表明,通过比较各分量不确定度,发现样品称量引入的不确定度分量可以忽略不计,而分析仪器引入的不确定度分量最大,占比为47%(AFG2)、44%(AFG1)、53%(AFB2)、52%(AFB1)。此外,加标回收率、被测物浓度以及样品处理过程中引入的不确定度分量也应引起注意。

关键词:延胡索;黄曲霉毒素;不确定度

Evaluation of the Uncertainty in Corydalis Yanhusuo Aflatoxin Determinationby HPLCPhotochemical Derivative Method

NING Zhi-gui1,HONG Jia-shun1,ZENG Hui-ting2,LI Dao-cheng1,PENG Si-si1,WANG Yu-cheng1*

(1 Jiangxi Province evaluation and research center of daodi herbs,Ganjiang New Area 330029,China;

2 Jiangxi Provincial Institute of TCM.,Nanchang 330000,China)

Abstract: The uncertainty evaluation of AFG2,AFG1,AFB2,and AFB1 in Corydalis yanhusuo was conducted usingliquid chromatography method for the determination of aflatoxins in Part Four of the 2020 edition of the ChinesePharmacopoeia. According to the relevant provisions of CNAS- GL006:2019“Guidelines for the Evaluation ofUncertainty in Chemical Analysis”,GB/T 27418—2017,and JJF1059.1—2012“Evaluation and Expression ofMeasurement Uncertainty”,the sources of uncertainty in the determination of aflatoxin in Corydalis yanhusuo wereanalyzed. By quantifying and synthesizing uncertainties,when k=2,the extended uncertainties of AFB1,AFB2,AFG1,and AFG2 in Corydalis yanhusuo were found to be 0.77g/kg,0.22g/kg,0.76g/kg,and 0.24g/kg,respectively.The results showed that by comparing the uncertainties of each component,it was found that the uncertainty causedby sample weighing could be ignored,while the uncertainty caused by the analytical instrument was the largest,accounting for 47%(AFG2),44%(AFG1),53%(AFB2),and 52%(AFB1). In addition,attention should also bepaid to the spiked recovery rate,the concentration of the analyte,and the uncertainty components from sampleprocessing.

Key words: corydalis yanhusuo;aflatoxins;uncertainty assessment

中图分类号:TS207.3            文献标志码:A                       文章编号:1007-7871(2024)06-0011-07

2024,Vol.27,No.6

 

 

 

 

 

 

 

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