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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 发布日期:2020-04-21
  • 通讯作者: 王步军 E-mail:wangbujun@caas.cn
  • 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 Online:2020-07-12 Published:2020-04-21
  • Contact: Bu-Jun WANG E-mail:wangbujun@caas.cn
  • 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)

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
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