河北大学学报(自然科学版) ›› 2023, Vol. 43 ›› Issue (5): 484-491.DOI: 10.3969/j.issn.1000-1565.2023.05.006

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HPLC法测定远志中黄曲霉毒素B1含量的不确定度评定

马力辉1,2,3,崔炎1,2,3,李迅1,2,3,赵志磊1,2,3,4   

  • 收稿日期:2022-10-17 出版日期:2023-09-25 发布日期:2023-10-25
  • 通讯作者: 赵志磊(1977—)
  • 作者简介:马力辉(1967—),男,河北定州人,河北大学教授,博士,主要从事检测技术及产品创新研究.
    E-mail:malihui@aliyun.com
  • 基金资助:
    河北省重点研发计划项目(21344801D)

Evaluation of uncertainty of measurement in determination of aflatoxin B1 content in polygala tenuifolia willd by HPLC

MA Lihui1,2,3,CUI Yan1,2,3,LI Xun1,2,3,ZHAO Zhilei1,2,3,4   

  1. 1.College of Quality and Technical Supervision, Hebei University, Baoding 071002, China; 2. National& Local Joint Engineering Research Center of Metrology Instrument and System, Baoding 071002, China; 3. Hebei Key Laboratory of Energy Metering and Safety Testing Technology, Baoding 071002, China; 4.Institute of Geographical Indications, Hebei University, Baoding 071002, China
  • Received:2022-10-17 Online:2023-09-25 Published:2023-10-25

摘要: 为评定高效液相色谱法测定远志中黄曲霉毒素B1含量的不确定度,依据国家计量技术规范 JJF 1059.1—2012《测量不确定度评定与表示》,对随机选取的6 个远志样品,建立数学模型,从标准溶液稀释、样品称量、样品最终定容体积和仪器测定重复性等方面分析不确定度来源,量化不确定度分量,计算合成不确定度和扩展不确定度.实验结果表明远志中黄曲霉毒素B1测定结果合成标准不确定度为0.016 39 μg/kg,扩展不确定度0.032 78 μg/kg.不确定度评定结果表明:HPLC法对远志中黄曲霉毒素B1含量的测定数据可靠,远志中黄曲霉毒素B1含量的测量不确定度主要来源于重复性实验、标准曲线的拟合、液相色谱仪的使用.

关键词: 不确定度, 黄曲霉毒素B1, HPLC, 远志

Abstract: In order to evaluate the uncertainty of measurement in the determination of aflatoxin B1 in polygala tenuifolia willd by high performance liquid chromatography(HPLC),according to the national metrology technical specifications described in JJF1059.1—2012 “Evaluation and Expression of Uncertainty in Measurement”, six samples were randomly selected, and the mathematical model was established to analyze uncertainty sources,quantify the uncertainty components, calculate synthetic uncertainty and extend uncertainty in terms of the dilution of standard solution, the weighing of the samples, the final volume of the samples and the repeatability of instrumental measurement. The experimental results showed that the combined uncertainty of aflatoxin B1 determination in polygala7 tenuifolia- DOI:10.3969/j.issn.1000-1565.2023.05.006HPLC法测定远志中黄曲霉毒素B1含量的不确定度评定马力辉1,2,3,崔炎1,2,3,李迅1,2,3,赵志磊1,2,3,4(1.河北大学 质量技术监督学院,河北 保定 071002;2.计量仪器与系统国家地方联合工程研究中心,河北 保定 071002;3.河北省能源计量与安全检测技术重点实验室,河北 保定 071002;4.河北大学 地理标志研究院,河北 保定 071002 )摘 要:为评定高效液相色谱法测定远志中黄曲霉毒素B1含量的不确定度,依据国家计量技术规范 JJF 1059.1—2012《测量不确定度评定与表示》,对随机选取的6 个远志样品,建立数学模型,从标准溶液稀释、样品称量、样品最终定容体积和仪器测定重复性等方面分析不确定度来源,量化不确定度分量,计算合成不确定度和扩展不确定度.实验结果表明远志中黄曲霉毒素B1测定结果合成标准不确定度为0.016 39 μg/kg,扩展不确定度0.032 78 μg/kg.不确定度评定结果表明:HPLC法对远志中黄曲霉毒素B1含量的测定数据可靠,远志中黄曲霉毒素B1含量的测量不确定度主要来源于重复性实验、标准曲线的拟合、液相色谱仪的使用.关键词:不确定度;黄曲霉毒素B1;HPLC;远志 中图分类号:O657.72 文献标志码:A 文章编号:1000-1565(2023)05-0484-08Evaluation of uncertainty of measurement in determination of aflatoxin B1 content in polygala tenuifolia willd by HPLCMA Lihui1,2,3,CUI Yan1,2,3,LI Xun1,2,3,ZHAO Zhilei1,2,3,4(1.College of Quality and Technical Supervision, Hebei University, Baoding 071002, China;2. National&Local Joint Engineering Research Center of Metrology Instrument and System, Baoding 071002, China;3. Hebei Key Laboratory of Energy Metering and Safety Testing Technology, Baoding 071002, China;4.Institute of Geographical Indications,Hebei University, Baoding 071002, China)Abstract: In order to evaluate the uncertainty of measurement in the determination of aflatoxin B1 in polygala tenuifolia willd by high performance liquid chromatography(HPLC),according to the national metrology technical specifications described in JJF1059.1—2012 “Evaluation and Expression of Uncertainty in Measurement”, six samples were randomly selected, and the mathematical model was established to analyze uncertainty sources,quantify the uncertainty components, calculate synthetic uncertainty and extend uncertainty in terms of the dilution of standard solution, the weighing of the samples, the final volume of the samples and the repeatability of instrumental measurement. The experimental results showed that the combined uncertainty of aflatoxin B1 determination in polygala7 tenuifolia- 收稿日期:2022-10-17 基金项目:河北省重点研发计划项目(21344801D) 第一作者:马力辉(1967—),男,河北定州人,河北大学教授,博士,主要从事检测技术及产品创新研究.E-mail:malihui@aliyun.com 通信作者:赵志磊(1977—),男,河北辛集人,河北大学教授,博士,主要从事食品药品质量检测技术.E-mail:15930721279@163.com第5期马力辉等:HPLC法测定远志中黄曲霉毒素B1含量的不确定度评定willd was 0.016 39 μg/kg and the extended uncertainty was 0.032 78 μg/kg.The uncertainty assessment results showed that determination of aflatoxin B1 in polygala tenuifolia willd by HPLC method were reliable, and the uncertainties of measurement in the determination of aflatoxin B1 in polygala tenuifolia willd were mainly come from the repeatability, the fitting of the standard curve, and the use of HPLC.

Key words: uncertainty, aflatoxin B1, HPLC, polygala tenuifolia willd

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