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伏马毒素B1纯度标准物质的研制

郭文博 孟佳佳 牛雪珂 王欣艺 聂冬霞 赵志辉 韩铮

郭文博,孟佳佳,牛雪珂,等. 伏马毒素B1纯度标准物质的研制[J]. 计量科学与技术,2023, 67(10): 46-53 doi: 10.12338/j.issn.2096-9015.2023.0284
引用本文: 郭文博,孟佳佳,牛雪珂,等. 伏马毒素B1纯度标准物质的研制[J]. 计量科学与技术,2023, 67(10): 46-53 doi: 10.12338/j.issn.2096-9015.2023.0284
GUO Wenbo, MENG Jiajia, NIU Xueke, WANG Xinyi, NIE Dongxia, ZHAO Zhihui, HAN Zheng. Development of a Certified Reference Material for Fumonisin B1 Purity[J]. Metrology Science and Technology, 2023, 67(10): 46-53. doi: 10.12338/j.issn.2096-9015.2023.0284
Citation: GUO Wenbo, MENG Jiajia, NIU Xueke, WANG Xinyi, NIE Dongxia, ZHAO Zhihui, HAN Zheng. Development of a Certified Reference Material for Fumonisin B1 Purity[J]. Metrology Science and Technology, 2023, 67(10): 46-53. doi: 10.12338/j.issn.2096-9015.2023.0284

伏马毒素B1纯度标准物质的研制

doi: 10.12338/j.issn.2096-9015.2023.0284
基金项目: 上海市科技兴农技术创新项目(沪农科创字(2012)第3-2号);上海市“科技创新行动计划”启明星项目(21QB1403300)。
详细信息
    作者简介:

    郭文博(1988-),上海市农业科学院助理研究员,研究方向:真菌毒素标准物质研制与应用,邮箱:guo1103bo@126.com

    通讯作者:

    韩铮(1983-),上海市农业科学院研究员,研究方向:农产品质量安全,邮箱:hanzheng@saas.sh.cn

  • 中图分类号: TB99

Development of a Certified Reference Material for Fumonisin B1 Purity

  • 摘要: 为更好的满足农产品质量安全检测需求,保证检测结果的准确性、可靠性和可溯源性,研制了伏马毒素B1(FB1)纯度标准物质。以实验室自主分离纯化获得的FB1为候选物,通过质谱、红外光谱、核磁共振谱等对其进行定性鉴定。采用质量平衡法和定量核磁法两种不同原理的方法对候选物的纯度进行定值,其中质量平衡法中采用面积归一化法、卡尔费休法、气相色谱串联质谱法和电感耦合等离子体质谱法,分别对候选物中主成分(FB1)、水分、挥发性杂质和非挥发性杂质含量进行测定。此外,开展了均匀性检验、稳定性考察,并对研制过程中产生的不确定度进行了系统的评定。结果表明:FB1纯度标准物质量值为99.1%,扩展不确定度为0.3%(k=2),均匀性良好,且满足12个月的稳定性要求。研制的FB1纯度标准物质获得国家二级标准物质证书,编号为GBW(E)100550,能够用于农产品中FB1的定性和定量检测、方法评价以及FB1量值溯源体系的建立。
  • 图  1  FB1标准物质候选物的红外光谱图

    Figure  1.  Infrared spectroscopy of FB1 certified reference material candidate

    图  2  FB1标准物质候选物的高分辨质谱图

    Figure  2.  Time-of-flight mass spectrometry (TOF/MS-MS) of the FB1 certified reference material candidate

    图  3  FB1标准物质候选物的UHPLC-CAD色谱图

    Figure  3.  Ultra-high performance liquid chromatography with charged aerosol detection (UHPLC-CAD) chromatograms of the FB1 certified reference material candidate

    图  4  FB1标准物质候选物和苯甲酸混合样品在氘代甲醇中的1H-NMR 谱图

    Figure  4.  Proton nuclear magnetic resonance (1H-NMR) spectra of mixed samples of FB1 certified reference material candidate and benzoic acid in deuterated methanol

    表  1  FB1标准物质候选物的质量平衡法定值结果

    Table  1.   Quantitative determination of the FB1 certified reference material candidate using the mass balance method (%)

    项目结果平均值标准偏差
    主成分纯度99.3199.310.031
    99.29
    99.32
    99.31
    99.29
    99.31
    水分含量0.1430.1390.003
    0.136
    0.134
    0.141
    0.143
    0.137
    无机离子杂质0.0430.0500.005
    0.057
    0.051
    0.044
    0.055
    0.050
    纯度99.12
    下载: 导出CSV

    表  2  FB1物质候选物均匀性数据与检验结果

    Table  2.   Data analysis and homogeneity testing (F-test) of the FB1 certified reference material candidate (%)

    瓶号 1 2 3
    1 99.35 99.34 99.31
    2 99.35 99.33 99.34
    3 99.29 99.29 99.32
    4 99.34 99.28 99.31
    5 99.32 99.27 99.31
    6 99.30 99.32 99.29
    7 99.26 99.32 99.34
    8 99.28 99.31 99.32
    9 99.29 99.32 99.33
    10 99.30 99.29 99.25
    11 99.34 99.29 99.31
    12 99.34 99.28 99.37
    13 99.34 99.29 99.31
    14 99.29 99.31 99.32
    15 99.32 99.31 99.28
    平均值 99.31
    组间方差(Mbetween 0.000671
    组内方差(Mwithin 0.000667
    F (Mbetween/Mwithin) 1.01
    F0.05(14, 30) 2.04
    下载: 导出CSV

    表  3  FB1物质候选物稳定性数据与检验结果

    Table  3.   Analysis of short-term and long-term stability (t-test) of the FB1 certified reference material candidate (%)

    时间(天) 短期稳定性 时间(月) 长期稳定性
    −20 ℃ 4 ℃ 60 ℃ −20 ℃
    0 99.34 99.31 99.29 0 99.32
    2 99.31 99.29 99.31 1 99.29
    4 99.32 99.33 99.32 3 99.31
    6 99.29 99.30 99.31 6 99.33
    8 99.31 99.31 99.30 12 99.29
    β1 −0.0040 0.0005 0.0010 β1 −0.0010
    β0 99.330 99.306 99.302 β0 99.313
    s 0.0151 0.0170 0.0126 s 0.0198
    s(β1) 0.0024 0.0027 0.0020 s(β1) 0.0021
    t0.95, 3 3.18 3.18 3.18 t0.95, 3 3.18
    s(β1t0.95,3 0.0076 0.0086 0.0064 s(β1t0.95, 3 0.0065
    下载: 导出CSV

    表  4  FB1标准物质候选物不确定度评定结果

    Table  4.   Evaluation of uncertainties associated with the developed FB1 certified reference material candidate

    来源 公式 不确定度/%
    均匀性(ubb $ {{u}}_{{{\mathrm{bb}}}}{=}\sqrt{\dfrac{{{M}}_{{{\mathrm{between}}}}{-}{{M}}_{{{\mathrm{within}}}}}{{n}}} $ 0.0012
    长期稳定性(ulst $ {{u}}_{{{\mathrm{lts}}}}={s(}{{\beta }}_{{1}}{)}\times {t} $ 0.0247
    短期稳定性(usts $ {{u}}_{{{\mathrm{sts}}}}={s(}{{\beta }}_{{1}}{)}\times {t} $ 0.0215
    质量平衡法(uMB $ {{u}}_{{{\mathrm{MB}}}}{}{=}{P}_{{{\mathrm{MB}}}}\times \sqrt{{\left[\dfrac{{u}\left({{P}}_{{0}}\right)}{{{P}}_{{0}}}\right]}^{{2}}{+}\dfrac{{{[}{u}{(}{{X}}_{{{\mathrm{W}}}}{)]}}^{{2}}{+}{{[}{u}{(}{{X}}_{{{\mathrm{NV}}}}{)]}}^{{2}}}{{{(1-}{{X}}_{{{\mathrm{W}}}}{-}{{X}}_{{{\mathrm{NV}}}}{)}}^{{2}}}} $ 0.0513
    定量核磁法(uqNMR $ {{u}}_{{ {\mathrm{}}}}={{P}}_{{{\mathrm{FB1}}}}\sqrt{{\left[\dfrac{{u}{(}{{I}}_{{{\mathrm{FB1}}}}/{{I}}_{{{\mathrm{std}}}}{)}}{{{I}}_{{{\mathrm{FB1}}}}{/}{{I}}_{{{\mathrm{std}}}}}\right]}^{{2}}{+}{\left[\dfrac{{u}{(}{{M}}_{{{\mathrm{FB1}}}}{)}}{{{M}}_{{{\mathrm{FB1}}}}}\right]}^{{2}}{+}{\left[\dfrac{{u}{(}{{M}}_{{{\mathrm{std}}}}{)}}{{{M}}_{{{\mathrm{std}}}}}\right]}^{{2}}{+}{\left[\dfrac{{u}{(}{{m}}_{{{\mathrm{std}}}}{)}}{{{m}}_{{{\mathrm{std}}}}}\right]}^{{2}}{+}{\left[\dfrac{{u}{(}{{m}}_{{{\mathrm{FB1}}}}{)}}{{{m}}_{{{\mathrm{FB1}}}}}\right]}^{{2}}{+}{\left[\dfrac{{u}{(}{{P}}_{{{\mathrm{std}}}}{)}}{{{P}}_{{{\mathrm{std}}}}}\right]}^{{2}}} $ 0.2821
    定值合成不确定度(uchar $ {{u}}_{{{\mathrm{char}}}}{=}\dfrac{\sqrt{{{u}}_{{{\mathrm{MB}}}}^{{2}}{+}{{u}}_{{{\mathrm{qNMR}}}}^{{2}}}}{{2}} $ 0.1434
    合成不确定度(uCRM $ {{u}}_{{{\mathrm{CRM}}}}{=}\sqrt{{{u}}_{{{\mathrm{char}}}}^{{2}}{+}{{u}}_{{{\mathrm{bb}}}}^{{2}}{+}{{u}}_{{{\mathrm{sts}}}}^{{2}}{+}{{u}}_{{{\mathrm{lst}}}}^{{2}}} $ 0.1471
    扩展不确定度(U U=k×uCRM, k=2 0.3
    下载: 导出CSV
  • [1] KAMLE M, MAHATO D K, DEVI S, et al. Fumonisins: Impact on agriculture, food, and human health and their management strategies[J]. Toxins, 2019, 11(6): 328. doi: 10.3390/toxins11060328
    [2] 郭志青, 张霞, 刁立功, 等. 镰刀菌及其伏马毒素的危害和防控[J]. 山东农业科学, 2022, 54(1): 157-164.
    [3] PONCE-GARCíA N, SERNA-SALDIVAR S O, GARCIA-LARA S. Fumonisins and their analogues in contaminated corn and its processed foods – a review [J]. Food Additives & Contaminants: Part A, 2018: 2183-2203.
    [4] CHEN J, WEI Z, WANG Y, et al. Fumonisin B1 : mechanisms of toxicity and biological detoxification progress in animals [J]. Food and Chemical Toxicology, 2021, 149(3): 111977.
    [5] DEEPTHI B V, SOMASHEKARAIAH R, POORNACHANDRA R K, et al. Lactobacillus plantarum MYS6 ameliorates fumonisin B1-induced hepatorenal damage in broilers[J]. Frontiers in Microbiology, 2017, 8: 2317. doi: 10.3389/fmicb.2017.02317
    [6] SORIANO J M, GONZáLEZ L, CATALá A I. Mechanism of action of sphingolipids and their metabolites in the toxicity of fumonisin B1[J]. Progress in Lipid Research, 2005, 44(6): 345-56. doi: 10.1016/j.plipres.2005.09.001
    [7] OSTRY V, MALIR F, TOMAN J, et al. Mycotoxins as human carcinogens-the IARC Monographs classification[J]. Mycotoxin research, 2017, 33: 65-73. doi: 10.1007/s12550-016-0265-7
    [8] U. S. Food and Drug Administration. guidance for industry: fumonisin levels in human foods and animal feeds, final guidance[EB/OL].https://www.fda.gov/regulatory-information/search-fda-guidance-documents/guidance-industry-fumonisin-levels-human-foods-and-animal-feeds.
    [9] The codex committee on food additives and contaminants. general standard for contaminants and toxins in food and feed : CODEX STAN 193-1995 [S]. Washington DC: FAO, 1995.
    [10] The Commission of the European Communities. setting maximum levels for certain contaminants in food stuffs : EC No 1881/2006 [S]. Brussel: official journal of the European Union, 2006.
    [11] 国家质量监督检验检疫总局, 中国国家标准化管理委员会. 饲料卫生标准: GB 13078-2017[S]. 北京: 中国标准出版社, 2017.
    [12] 谢刚, 王松雪. 粮油真菌毒素检测技术及标准物质研究进展[C]. 北京: 国家真菌毒素防控科技创新联盟成立大会暨第一届中国真菌毒素大会论文集, 2016.
    [13] 韩铮, 郭文博, 范楷, 等. 真菌毒素检测及相关标准物质制备技术研究 [C]. 北京: 国家真菌毒素防控科技创新联盟成立大会暨第一届中国真菌毒素大会论文集, 2016.
    [14] 卢晓华, 薄梦, 吴雪, 等. 标准物质领域发展现状及趋势[J]. 化学试剂, 2022, 44(10): 1403-1410.
    [15] GUO Z, LI X, LI H. Certified reference materials and metrological traceability for mycotoxin analysis [M]. Oxford University Press, 2019: 1695-707.
    [16] TANGNI E K, DEBONGNIE P, HUYBRECHTS B, et al. Towards the development of innovative multi-mycotoxin reference materials as promising metrological tool for emerging and regulated mycotoxin analyses[J]. Mycotoxin Research, 2016, 33(1): 1-10.
    [17] OLIVARES I R B, SOUZA G B, NOGUEIRA A R A, et al. Trends in developments of certified reference materials for chemical analysis-focus on food, water, soil, and sediment matrices[J]. TrAC Trends in Analytical Chemistry, 2018, 100: 53-64. doi: 10.1016/j.trac.2017.12.013
    [18] 郑子繁, 刘卫晓, 金芜军, 等. 质量平衡法及其在标准物质定值中的应用进展[J]. 生物技术进展, 2020, 10(6): 623-629.
    [19] 杨梦瑞, 简凌波, 王敏, 等. 盐酸沙拉沙星纯度定值方法研究及标准物质研制[J]. 农产品质量与安全, 2020(6): 35-44.
    [20] 张思遥, 李晓敏, 王海峰, 等. 差示扫描量热法测定4-正辛基酚, 炔雌醇等5种化合物的纯度 [J]. 计量科学与技术, 2022, (66)7: 22-27.
    [21] 韦棋, 苏福海. 甲卡西酮纯度标准物质的研制[J]. 计量科学与技术, 2020(11): 10-16.
    [22] 李硕, 张楠, 刘喆, 等. α-熊果苷纯度标准物质的研制[J]. 计量科学与技术, 2022, 66(8): 7-12.
    [23] GUO W B, HAN Z, YANG J H, et al. Simultaneous preparation and characterization of three high-purity type B fumonisins from maize culture[J]. Analytical Methods, 2016, 8: 2737. doi: 10.1039/C5AY03307A
    [24] 国家市场监督管理总局. 标准物质的定值及均匀性、 稳定性评估: JJF 1343-2022 [S]. 北京: 中国质检出版社, 2022.
    [25] Bezuidenhout S C, Gelderblom W C A, Gorst-Allman C P, et al. Structure elucidation of the fumonisins, mycotoxins from Fusarium moniliforme[J]. Journal of the Chemical Society, Chemical Communications, 1988(11): 743-745. doi: 10.1039/c39880000743
    [26] 李莉, 李硕. QuEChERS-超高效液相色谱-串联质谱法测定玉米油中伏马毒素B1, B2, B3[J]. 食品安全质量检测学报, 2020, 11(19): 7006-7011.
    [27] HAN Z, REN Y, LIU X, et al. A reliable isotope dilution method for simultaneous determination of fumonisins B1, B2 and B3 in traditional Chinese medicines by ultra‐high‐performance liquid chromatography‐tandem mass spectrometry[J]. Journal of Separation Science, 2010, 33(17-18): 2723-2733. doi: 10.1002/jssc.201000423
    [28] SZEKERES A, LORANTFY L, BENCSIK O, et al. Rapid purification method for fumonisin B1 using centrifugal partition chromatography[J]. Food Additives & Contaminants, 2013, 30(1): 147-155.
    [29] MARIA, MÅNSSON, MARIE, et al. Isolation and NMR Characterization of Fumonisin B2 and a New Fumonisin B6from Aspergillus niger[J]. Journal of Agricultural & Food Chemistry, 2010, 58: 949-953.
    [30] 马康, 苏福海, 王海峰, 等. 有机纯度标准物质定值技术研究进展[J]. 分析测试学报, 2013, 32(7): 901-908.
    [31] WESTWOOD S, TAICHIHUANG, TINGGARRIDO, et al. Development and validation of a suite of standards for the purity assignment of organic compounds by quantitative NMR spectroscopy[J]. Metrologia, 2019, 56: 064001. doi: 10.1088/1681-7575/ab45cb
    [32] 国家市场监督管理总局. 纯度标准物质定值计量技术规范 有机物纯度标准物质: JJF 1855-2020 [S]. 北京: 中国质检出版社, 2020.
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出版历程
  • 收稿日期:  2023-11-17
  • 录用日期:  2023-11-20
  • 修回日期:  2023-11-29
  • 网络出版日期:  2023-12-06
  • 刊出日期:  2023-10-18

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