欢迎访问作物学报，今天是
作物学报

作物学报 ›› 2020, Vol. 46 ›› Issue (7): 1128-1133.doi: 10.3724/SP.J.1006.2020.93056

• 研究简报 • 上一篇    

玉米粉中伏马毒素FB1基体标准物质的评价

牛欣宁,王步军()   

  1. 中国农业科学院作物科学研究所 / 农业农村部谷物品质监督检验测试中心, 北京 100081
  • 收稿日期:2019-10-15 接受日期:2020-03-24 出版日期:2020-07-12 网络出版日期:2020-04-21
  • 通讯作者: 王步军
  • 作者简介:E-mail: niuxinning123@126.com
  • 基金资助:
    国家自然科学基金项目(31701704);国家粮油作物产品质量安全风险评估专项(GJFP2019001);中国农业科学院科技创新工程项目;国家重点研发计划项目(2016YFF0201803)

Evaluation of matrix reference material of Fumonisins FB1 in corn flour

NIU Xin-Ning,WANG Bu-Jun()   

  1. Institute of Crop Sciences, Chinese Academy of Agricultural Sciences / Cereal Quality Supervision and Testing Center, Ministry of Agriculture, Beijing 100081, China
  • Received:2019-10-15 Accepted:2020-03-24 Published:2020-07-12 Published online:2020-04-21
  • Contact: Bu-Jun WANG
  • Supported by:
    National Natural Science Foundation of China(31701704);National Grain and Oil Crop Product Quality and Safety Risk Assessment Special(GJFP2019001);Science and Technology Innovation Project of Chinese Academy of Agricultural Sciences;National Key Research and Development Program(2016YFF0201803)

RichHTML

8

PDF

182

摘要：

为填补我国在伏马毒素基体标准物质的空白, 本试验研制了以玉米粉为基体的伏马毒素FB1标准物质, 玉米样品经过筛、加标、冷冻干燥、磨粉、混匀、密封分装后, 用超高效液相色谱-串联质谱(UPLC-MS/MS)法检验样品的均匀性、稳定性, 并联合多家实验室对玉米粉中伏马毒素FB1含量定值, 同时分析样品的不确定度。样品均匀性经方差分析法表明F值为1.42, 小于临界值F0.05, 且伏马毒素FB1含量在规定时间6个月内无明显变化。结果表明, 均匀性与稳定性均符合标准物质的要求。样品定值为1475.56 μg kg-1, 不确定度为169.98 μg kg-1。该标准物质可替代进口标准物质, 用于伏马毒素检测过程中的仪器校准、实验室质量控制和操作人员的水平考核等。

关键词: 玉米粉, 伏马毒素FB1, 超高液相色谱-串联质谱法, 标准物质

Abstract:

To fill the gap of matrix reference material of fumonisins in our country, we developed a reference material of Fumonisins FB1 in corn flour. The homogeneity and stability of corn samples were tested by UPLC-MS/MS after screening, labeling, freeze-drying, grinding, mixing and sealing it. The content of Fumonisins FB1 in corn flour was determined by several laboratories, and the uncertainty of samples was analyzed. The homogeneity of the sample was calculated, with 1.42 of F which was less than the critical F0.05, and there was no significant change in the content of Fumonisins FB1 within the limited time for six months. The results showed that the uniformity and stability fulfill the requirements of reference material. The determined value of the sample was 1475.56 μg kg-1, and the uncertainty was 169.98 μg kg-1. The reference material can be used to calibrate the instrument, control laboratory quality and evaluate the testing quality of operators during the testing process of Fumonisins.

Key words: corn flour, Fumonisins FB1, UPLC-MS/MS, reference material

表1

玉米粉中伏马毒素FB1均匀性检验结果"

编号
No.		 测定值Estimated value 平均值
Mean
样品1 Sample 1 样品2 Sample 2 样品3 Sample 3
1 1526.94 1515.99 1548.48 1530.47
2 1475.93 1561.67 1466.99 1501.53
3 1541.65 1578.75 1586.70 1569.03
4 1642.69 1523.99 1477.12 1547.93
5 1547.76 1553.40 1320.62 1473.93
6 1550.76 1523.61 1429.61 1501.33
7 1409.22 1429.40 1519.65 1452.76
8 1564.07 1584.00 1582.17 1576.74
9 1515.83 1487.58 1465.17 1489.52
10 1550.90 1519.14 1513.76 1527.93
11 1498.30 1473.52 1516.96 1496.26
12 1425.48 1570.33 1425.64 1473.82
13 1455.89 1375.58 1479.23 1436.90
14 1461.25 1342.56 1568.66 1457.49
15 1446.23 1483.95 1393.13 1441.11
组间标准偏差的平方 S12 5915.88
组内标准偏差的平方 S22 4164.09
统计量F Statistic F 1.42
F0.05(14,30) 2.04
判断 Judgment 均匀 Inhomogeneous

表2

玉米粉中伏马毒素FB1短期稳定性检验结果"

时间
Day (d)		 测定值 Estimated value 平均值
Mean
样品1 Sample 1 样品2 Sample 2 样品3 Sample 3
0 1443.21 1527.20 1401.19 1457.20
1 1437.83 1505.11 1410.89 1451.28
4 1483.95 1512.63 1563.87 1520.15
7 1457.61 1471.37 1438.96 1455.98
14 1412.94 1400.17 1369.62 1394.24
斜率 b1 -4.79
斜率不确定度 s(b1) 3.64
临界值 t0.95, n-2×s(b1) 11.58
结论Conclusion 稳定Stabilization

图1

玉米粉中伏马毒素FB1短期稳定性趋势分析图"

表3

玉米粉中伏马毒素FB1长期稳定性检验结果"

温度
Temperature		 时间(月)
Time (month)		 测定值Estimated value 平均值
Mean		 斜率
b1		 临界值
t0.95, n-2×s(b1)		 结论
Conclusion
样品1
Sample 1		 样品2
Sample 2		 样品3
Sample 3
4℃ 0 1443.21 1527.20 1401.19 1457.20 -20.86 31.60 稳定
Stabilization
1 1481.61 1527.86 1525.53 1511.67
2 1368.36 1430.24 1428.94 1409.18
4 1442.54 1422.36 1477.85 1447.58
6 1389.45 1334.99 1283.45 1335.96
-18℃ 1 1468.15 1382.05 1450.64 1433.62 -10.27 31.40 稳定Stabilization
2 1498.44 1526.57 1531.25 1518.75
4 1407.69 1372.59 1405.98 1395.42
6 1457.35 1381.64 1398.07 1412.35

图2

玉米粉中伏马毒素FB1长期稳定性趋势分析图"

表4

各实验室联合定值测定结果"

实验室编号
Laboratory number		 测定值Estimated value
1 2 3 4 5 6
A 930 940 940 950 960 1100
B 1400 1300 1500 1500 1300 1300
C 1800 1500 1300 1600 1400 1400
D 1800 2200 1900 2200 2100 2300
E 1400 1400 1200 1300 1400 1400
F 1500 1500 1500 1600 1600 1700
平均值Mean 1475.56
[1] 杨朋飞, 王南希, 屈凌波, 伍松陵, 孙长坡. 伏马毒素消减方法研究进展. 粮油食品科技, 2015, (5):82-85.
Yang P F, Wang N X, Qu L B, Wu S L, Sun C P. Research progress in fumonisins’ degradation. Sci Technol Cereals Oils Foods, 2015, (5):82-85 (in Chinese with English abstract).
[2] Ramesh C G. Reproductive and Developmental Toxicology. NewYork: Academic Press, 2017. pp 925-943.
[3] Poersch A B, Trombetta F, Souto N S, Oliveira Lima C, Braga A C M, Dobrachinski F, Ribeiro L R, Soares F A, Fighera M R, Royes L F F, Oliveira M S, Furian A F. Fumonisin B1 facilitates seizures induced by pentylenetetrazol in mice. Neurotoxicol Teratol, 2015,51:61-67.
pmid: 26342287
[4] Pepeljnjak S, Petrinec Z, Kovaci S, Segvic M. Screening toxicity study in young carp (Cyprinus carpio L.) on feed amended with Fumonisin B1. Arch Ind Hygiene Toxicol, 2009,60:419-426.
[5] Osuchowski M F, Edwards G L, Sharma R P. Fumonisin B1 induced neurodegeneration in mice after intracerebroventricular infusion is concurrent with disruption of sphingolipid metabolism and activation of proinflammatory signaling. Neurotoxicology, 2005,26:211-221.
doi: 10.1016/j.neuro.2004.10.001 pmid: 15713342
[6] Antonissen G, Van Immerseel, Pasmans F, Ducatalle R, Janssens G P, De Baere S, Mountzouris K C, Su S, Wong E A, De Meulenaer B, Verlinden M, Devreese M, Haesebrouck F, Novak B, Dohnal I, Martel A, Groubels S. Mycotoxins deoxynivalenol and fumonisins alter the extrinsic component of intestinal barrier in broiler chickens. J Agr Food Chem, 2015,63:10846-10855.
[7] Grenier B, Loureiro-Bracarense A P, Lucioli J, Pacheco G D, Cossalter A M, Moll W D, Schatzmayr G, Oswald I P. Individual and combined effects of subclinical doses of deoxynivalenol and fumonisins in piglets. Mol Nutr Food Res, 2011,55:761-771.
doi: 10.1002/mnfr.201000402 pmid: 21259430
[8] Li Y, Fan Y, Xia B, Xian Q, Wang Q, Sun W, Zhang H, He C. The immunosuppressive characteristics of FB1 by inhibition of maturation and function of BMDCs. Int Immunopharmacol, 2017,47:206-211.
doi: 10.1016/j.intimp.2017.03.031 pmid: 28432936
[9] Mahmoodi M, Alizadeh A M, Sohanaki H, Rezaei N, Amini-Najafi F, Khosravi A R, Hosseini S K, Safari Z, Hydarnasab D, Khori V. Impact of fumonisin B1 on the production of inflammatory cytokines by gastric and colon cell lines. Iran J Allergy Asthma Immunol, 2012,11:165-173.
doi: 011.02/ijaai.165173 pmid: 22761190
[10] Keck B B, Bodine A B. The effects of fumoniisin B1 on viability and mitogenic response of avian immune cells. Poultry Sci, 2006,85:1020-1024.
[11] Singh M P, Kang S C. Endoplasmic reticulum stress-mediated autophagy activation attenuates fumonisin B1 induced hepato-toxicity in vitro and in vivo. Food Chem Toxicol, 2017,110:371-382.
doi: 10.1016/j.fct.2017.10.054 pmid: 29097114
[12] Loiseau N, Polizzi A, Dupuy A, Therville N, Rakotonirainy M, Loy J, Viadere J L, Cossalter A M, Bailly J D, Puel O, Kolf-Clauw M, Bertrand-Michel J, Levade T, Guillou H, Oswald I P. New insights into the organ-specific adverse effects of fumonisin B1: comparison between lung and liver. Arch Toxicol, 2005,89:1619-1629.
doi: 10.1007/s00204-014-1323-6 pmid: 25155190
[13] Riley R T, Voss K A. Differential sensitivity of rat kidney and liver to fumonisin toxicity: organ-specific differences in toxin accumulation and sphingoid base metabolism. Toxicol Sci, 2006,92:335-345.
doi: 10.1093/toxsci/kfj198 pmid: 16613836
[14] Bouhet S, Oswald I P. The intestine as a possible target for fumonisin toxicity. Mol Nutr Food Res, 2007,51:925-931.
doi: 10.1002/mnfr.200600266 pmid: 17642075
[15] Ewuola E O, Egbunike G N. Gonadal and extra-gonadal sperm reserves and sperm production of pubertal rabbits fed dietary fumonisin B1. Animal Reprod Sci, 2010,119:282-286.
[16] Somosk I B, Kov C M, Cseh S. Effects of T-2 and fumonisin B1 combined treatment onin vitro mouse embryo development and blastocyst quality. Toxicol Ind Health, 2018,34:353-360.
[17] Bondy G, Mehta R, Caldwell D, Coady L, Armstrong C, Savard M, Miller J D, Chomyshyn E, Bronson R, Zitomer N, Riley R T. Effects of long term exposure to the mycotoxin fumonisin B1 in p53 heterozygous and p53 homozygous transgenic mice. Food Chem Toxicol, 2012,50:3604-3613.
doi: 10.1016/j.fct.2012.07.024 pmid: 22841953
[18] KÖppen R, Bremser W, Stephan I, Klein-hartwig K, Rasenko T, Koch M. T-2 and HT-2 toxins in oat flakes: development of a certified reference material. Anal Bioanal Chem, 2015,407:2997-3007.
pmid: 25399074
[19] 刘素丽, 王宏伟, 赵梅, 曹进, 黄丙楠, 钮正睿. 食品中基体标准物质研究进展. 食品安全质量检测学报, 2019,10(1):8-13.
Liu S L, Wang H W, Zhao M, Cao J, Huang B N, Niu Z R. Research progress of matrix reference materials for food. J Food Saf Qual, 2019,10(1):8-13 (in Chinese with English abstract).
[20] 中华人民共和国国家质量监督检验检疫总局. 一级标准物质技术规范: JJF 1006-1994. 北京: 中国计量出版社, 1994.
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China. Technical Norm of Primary Reference Material: JJF 1006-1994. Beijing: Chinese Metrology Press, 1994 (in Chinese).
[21] 中华人民共和国国家质量监督检验检疫总局. 标准物质定值的通用原则及统计学原理: JJF 1343-2012. 北京: 中国标准出版社, 2012.
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China. General and Statistical Principles for Characterization of Reference Materials: JJF 1343-2012. Beijing: Standards Press of China, 2012 (in Chinese).
[22] ISO. ISO Guide 35: 2006 Reference Materials-general and Statiscal Principles for Certification. International Organization for Standardization (ISO): Geneva, 2006.
[23] 中华人民共和国国家质量监督检验检疫总局, 中国国家标准化管理委员会. 标准样品工作导则: (3)标准样品定值的一般原则和统计方法: GB/T 15000. 3-2008. 北京: 中国计量出版社, 2008.
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China. Standardization Administration of the People's Republic of China. Standard Sample Work Guidelines: (3) Reference Materials-General and Statistical Principles for Certification: GB/T 15000. 3-2008. Beijing: Chinese Metrology Press, 2008 (in Chinese).
[24] 中国实验室国家认可委员会. 化学分析中不确定度的评估指南. 北京: 中国计量出版社, 2006. pp 31-36.
China National Accreditation Board for Laboratories. Guidance on Evaluating the Uncertainty in Chemical Analysis. Beijing: Chinese Metrology Press, 2006. pp 31-36(in Chinese).
[25] 中国国家标准化管理委员会. 检测实验室中常用不确定度评定方法与表示: GB/T 27411-2012. 北京: 中国计量出版社, 2013.
Standardization Administration of the People’s Republic of China. Routine Methods for Evaluation and Expression of Measurement Uncertainty in Testing Laboratory: GB/T 27411-2012. Beijing: Chinese Metrology Press, 2013 (in Chinese).
[1] 单露英, 李俊, 李亮, 张丽, 王颢潜, 高佳琪, 吴刚, 武玉花, 张秀杰. 转基因玉米NK603基体标准物质研制[J]. 作物学报, 2022, 48(5): 1059-1070.
[2] 王渭霞, 赖凤香, 胡海燕, 何佳春, 魏琪, 万品俊, 傅强. 超低温11年保存期对转基因作物基体标准样品核酸检测的影响[J]. 作物学报, 2022, 48(1): 238-248.
[3] 李俊,李亮,李夏莹,宋贵文,沈平,张丽,翟杉杉,柳方方,吴刚,张秀杰,武玉花. 转基因玉米MIR604基体标准物质研制[J]. 作物学报, 2020, 46(4): 473-483.
[4] 陆大雷, 郭换粉, 董策, 陆卫平. 鲜食期和成熟期糯玉米粉理化特性的差异[J]. 作物学报, 2010, 36(12): 2170-2178.
Viewed
Full text


Abstract

Cited
  Shared   
  Discussed   
No Suggested Reading articles found!
京ICP备15008789号-2