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Acta Agronomica Sinica ›› 2020, Vol. 46 ›› Issue (7): 1128-1133.doi: 10.3724/SP.J.1006.2020.93056

• RESEARCH NOTES • Previous Articles    

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)

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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

Table 1

Test results of homogeneity of Fumzonisins FB1 in corn flour (μg kg-1)"

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

Table 2

Short-term stability test results of Fumonisins FB1 in corn flour (μg kg-1)"

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

Fig. 1

Analysis chart of short-term stability trend of Fumonisins FB1 in corn flour"

Table 3

Long-term stability test results of Fumonisins FB1 in corn flour (μg kg-1)"

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

Fig. 2

Analysis chart of long-term stability trend of Fumonisins FB1 in corn flour"

Table 4

Results of joint determination of fixed value by various laboratories (μg kg-1)"

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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