Chinese Journal of Chromatography ›› 2023, Vol. 41 ›› Issue (11): 1002-1009.DOI: 10.3724/SP.J.1123.2023.07014
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ZHANG Luxing1, ZHOU Zheng2, CAO Lin2, QIAN Jiang1,*()
Received:
2023-07-15
Online:
2023-11-08
Published:
2023-11-16
Supported by:
CLC Number:
ZHANG Luxing, ZHOU Zheng, CAO Lin, QIAN Jiang. Determination of seven mycotoxins in cereals by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry based on the self-built database[J]. Chinese Journal of Chromatography, 2023, 41(11): 1002-1009.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2023.07014
t/min | φ(A)/% | φ(B)/% |
---|---|---|
0 | 90 | 10 |
2.0 | 90 | 10 |
3.0 | 80 | 20 |
7.0 | 76 | 24 |
10.5 | 70 | 30 |
13.5 | 40 | 60 |
15.0 | 30 | 70 |
18.0 | 25 | 75 |
18.1 | 5 | 95 |
21.9 | 5 | 95 |
22.0 | 90 | 10 |
Table 1 UPLC elution procedure
t/min | φ(A)/% | φ(B)/% |
---|---|---|
0 | 90 | 10 |
2.0 | 90 | 10 |
3.0 | 80 | 20 |
7.0 | 76 | 24 |
10.5 | 70 | 30 |
13.5 | 40 | 60 |
15.0 | 30 | 70 |
18.0 | 25 | 75 |
18.1 | 5 | 95 |
21.9 | 5 | 95 |
22.0 | 90 | 10 |
No. | Compound | Transitions (m/z) | Cone voltage/V | Collision energy/eV | Ion mode |
---|---|---|---|---|---|
1 | aflatoxin B1 (AFB1) | 329.068/311.053*; 329.068/243.066 | 40 | 20 | [M+H]+ |
2 | aflatoxin B2 (AFB2) | 331.080/313.067*; 331.080/285.070 | 40 | 25 | [M+H]+ |
3 | aflatoxin G1 (AFG1) | 313.070/285.072*; 313.070/270.050 | 40 | 25 | [M+H]+ |
4 | aflatoxin G2 (AFG2) | 315.085/287.090*; 315.085/259.055 | 40 | 25 | [M+H]+ |
5 | ochratoxin A (OTA) | 404.088/358.078; 404.088/239.005* | 40 | 25 | [M+H]+ |
6 | deoxynivalenol (DON) | 355.141/295.116; 355.141/265.103* | 40 | 10 | [M+CH3COO]- |
7 | zearalenone (ZEN) | 317.138/273.146; 317.138/175.036* | 40 | 25 | [M-H]- |
Table 2 MS parameters of the seven mycotoxins
No. | Compound | Transitions (m/z) | Cone voltage/V | Collision energy/eV | Ion mode |
---|---|---|---|---|---|
1 | aflatoxin B1 (AFB1) | 329.068/311.053*; 329.068/243.066 | 40 | 20 | [M+H]+ |
2 | aflatoxin B2 (AFB2) | 331.080/313.067*; 331.080/285.070 | 40 | 25 | [M+H]+ |
3 | aflatoxin G1 (AFG1) | 313.070/285.072*; 313.070/270.050 | 40 | 25 | [M+H]+ |
4 | aflatoxin G2 (AFG2) | 315.085/287.090*; 315.085/259.055 | 40 | 25 | [M+H]+ |
5 | ochratoxin A (OTA) | 404.088/358.078; 404.088/239.005* | 40 | 25 | [M+H]+ |
6 | deoxynivalenol (DON) | 355.141/295.116; 355.141/265.103* | 40 | 10 | [M+CH3COO]- |
7 | zearalenone (ZEN) | 317.138/273.146; 317.138/175.036* | 40 | 25 | [M-H]- |
Compound | GB 2761-2017 | EC No.1881/2006 | This work | |||||
---|---|---|---|---|---|---|---|---|
Rice | Wheat | Rice | Wheat | Rice | Wheat | |||
AFG1 | none | none | total: 4.0 | total: 4.0 | total: 4.0 | total: 4.0 | ||
AFG2 | none | none | ||||||
AFB1 | 10 | 5.0 | ||||||
AFB2 | none | none | ||||||
OTA | 5.0 | 5.0 | 5.0 | 5.0 | 5.0 | 5.0 | ||
DON | none | 1000 | 1250 | 1750 | 1000 | 1000 | ||
ZEN | none | 60 | 100 | 100 | 60 | 60 |
Table 3 Maximum limits for the seven mycotoxins μg/kg
Compound | GB 2761-2017 | EC No.1881/2006 | This work | |||||
---|---|---|---|---|---|---|---|---|
Rice | Wheat | Rice | Wheat | Rice | Wheat | |||
AFG1 | none | none | total: 4.0 | total: 4.0 | total: 4.0 | total: 4.0 | ||
AFG2 | none | none | ||||||
AFB1 | 10 | 5.0 | ||||||
AFB2 | none | none | ||||||
OTA | 5.0 | 5.0 | 5.0 | 5.0 | 5.0 | 5.0 | ||
DON | none | 1000 | 1250 | 1750 | 1000 | 1000 | ||
ZEN | none | 60 | 100 | 100 | 60 | 60 |
Compound | Linear range/(μg/L) | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) | |ME|/% |
---|---|---|---|---|---|---|
AFG1 | 0.25-1.25 | y=2.12×103x-3.69×102 | 0.9945 | 0.50 | 1.00 | 46.2 |
AFG2 | 0.25-1.25 | y=1.69×103x-1.48×102 | 0.9950 | 0.50 | 1.00 | 37.4 |
AFB1 | 0.25-1.25 | y=1.74×103x-0.87×102 | 0.9953 | 0.50 | 1.00 | 48.1 |
AFB2 | 0.25-1.25 | y=1.76×103x+0.46×102 | 0.9900 | 0.50 | 1.00 | 45.3 |
OTA | 1.00-5.00 | y=1.80×102x-1.11×102 | 0.9900 | 2.00 | 4.00 | 21.5 |
DON | 200-1000 | y=6.04x-6.04×102 | 0.9934 | 400 | 800 | 13.4 |
ZEN | 10.0-50.0 | y=1.12×103x-1.48×103 | 0.9974 | 2.00 | 8.00 | 0.7 |
Table 4 Linear ranges, linear equations, correlation coefficients (r), limits of detection (LODs), limits of quantification (LOQs) and matrix effects (MEs) of the seven mycotoxins in rice matrix
Compound | Linear range/(μg/L) | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) | |ME|/% |
---|---|---|---|---|---|---|
AFG1 | 0.25-1.25 | y=2.12×103x-3.69×102 | 0.9945 | 0.50 | 1.00 | 46.2 |
AFG2 | 0.25-1.25 | y=1.69×103x-1.48×102 | 0.9950 | 0.50 | 1.00 | 37.4 |
AFB1 | 0.25-1.25 | y=1.74×103x-0.87×102 | 0.9953 | 0.50 | 1.00 | 48.1 |
AFB2 | 0.25-1.25 | y=1.76×103x+0.46×102 | 0.9900 | 0.50 | 1.00 | 45.3 |
OTA | 1.00-5.00 | y=1.80×102x-1.11×102 | 0.9900 | 2.00 | 4.00 | 21.5 |
DON | 200-1000 | y=6.04x-6.04×102 | 0.9934 | 400 | 800 | 13.4 |
ZEN | 10.0-50.0 | y=1.12×103x-1.48×103 | 0.9974 | 2.00 | 8.00 | 0.7 |
Compound | Linear range/(μg/L) | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) | |ME|/% |
---|---|---|---|---|---|---|
AFG1 | 0.25-1.25 | y=3.70×103x-2.42×102 | 0.9974 | 0.50 | 1.00 | 6.3 |
AFG2 | 0.25-1.25 | y=2.23×103x+1.52×102 | 0.9934 | 0.50 | 1.00 | 17.3 |
AFB1 | 0.25-1.25 | y=3.06×103x-1.55×102 | 0.9963 | 0.50 | 1.00 | 8.6 |
AFB2 | 0.25-1.25 | y=3.52×103x-3.17×102 | 0.9972 | 0.50 | 1.00 | 10.5 |
OTA | 1.00-5.00 | y=1.72x+1.74×102 | 0.9867 | 2.00 | 4.00 | 25.2 |
DON | 200-1000 | y=5.88x-3.08×102 | 0.9961 | 200 | 800 | 15.6 |
ZEN | 10.0-50.0 | y=1.56×103x+8.08×102 | 0.9998 | 0.50 | 1.00 | 28.0 |
Table 5 Linear ranges, linear equations, r, LODs, LOQs and MEs of the seven mycotoxins in wheat matrix
Compound | Linear range/(μg/L) | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) | |ME|/% |
---|---|---|---|---|---|---|
AFG1 | 0.25-1.25 | y=3.70×103x-2.42×102 | 0.9974 | 0.50 | 1.00 | 6.3 |
AFG2 | 0.25-1.25 | y=2.23×103x+1.52×102 | 0.9934 | 0.50 | 1.00 | 17.3 |
AFB1 | 0.25-1.25 | y=3.06×103x-1.55×102 | 0.9963 | 0.50 | 1.00 | 8.6 |
AFB2 | 0.25-1.25 | y=3.52×103x-3.17×102 | 0.9972 | 0.50 | 1.00 | 10.5 |
OTA | 1.00-5.00 | y=1.72x+1.74×102 | 0.9867 | 2.00 | 4.00 | 25.2 |
DON | 200-1000 | y=5.88x-3.08×102 | 0.9961 | 200 | 800 | 15.6 |
ZEN | 10.0-50.0 | y=1.56×103x+8.08×102 | 0.9998 | 0.50 | 1.00 | 28.0 |
Compound | Spiked/ (μg/kg) | Rice | Wheat | |||
---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | |||
AFG1 | 1.00 | 111.9 | 6.4 | 119.3 | 0.8 | |
2.00 | 110.0 | 8.8 | 110.5 | 3.4 | ||
3.00 | 101.0 | 1.2 | 110.1 | 5.3 | ||
AFG2 | 1.00 | 113.4 | 1.9 | 117.0 | 7.6 | |
2.00 | 102.8 | 1.3 | 108.2 | 9.8 | ||
3.00 | 104.5 | 1.2 | 115.9 | 1.6 | ||
AFB1 | 1.00 | 123.6 | 1.6 | 122.5 | 3.4 | |
2.00 | 120.6 | 1.9 | 103.7 | 5.2 | ||
3.00 | 103.6 | 2.4 | 102.0 | 2.3 | ||
AFB2 | 1.00 | 123.5 | 5.9 | 122.0 | 4.5 | |
2.00 | 112.7 | 1.6 | 116.0 | 1.5 | ||
3.00 | 100.9 | 8.6 | 109.1 | 3.6 | ||
OTA | 4.00 | 123.9 | 10.7 | 120.0 | 9.6 | |
8.00 | 117.3 | 11.8 | 110.1 | 8.4 | ||
12.0 | 120.2 | 6.9 | 110.4 | 14.8 | ||
DON | 800 | 115.6 | 1.8 | 121.2 | 2.6 | |
1600 | 109.0 | 1.4 | 123.4 | 7.4 | ||
2400 | 118.8 | 0.2 | 115.2 | 12.5 | ||
ZEN | 40.0 | 105.5 | 9.4 | 120.9 | 7.3 | |
80.0 | 94.1 | 13.6 | 112.2 | 8.9 | ||
120 | 88.1 | 12.0 | 107.8 | 10.2 |
Table 6 Spiked recoveries and precisions of the seven mycotoxins in rice and wheat samples (n=6)
Compound | Spiked/ (μg/kg) | Rice | Wheat | |||
---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | |||
AFG1 | 1.00 | 111.9 | 6.4 | 119.3 | 0.8 | |
2.00 | 110.0 | 8.8 | 110.5 | 3.4 | ||
3.00 | 101.0 | 1.2 | 110.1 | 5.3 | ||
AFG2 | 1.00 | 113.4 | 1.9 | 117.0 | 7.6 | |
2.00 | 102.8 | 1.3 | 108.2 | 9.8 | ||
3.00 | 104.5 | 1.2 | 115.9 | 1.6 | ||
AFB1 | 1.00 | 123.6 | 1.6 | 122.5 | 3.4 | |
2.00 | 120.6 | 1.9 | 103.7 | 5.2 | ||
3.00 | 103.6 | 2.4 | 102.0 | 2.3 | ||
AFB2 | 1.00 | 123.5 | 5.9 | 122.0 | 4.5 | |
2.00 | 112.7 | 1.6 | 116.0 | 1.5 | ||
3.00 | 100.9 | 8.6 | 109.1 | 3.6 | ||
OTA | 4.00 | 123.9 | 10.7 | 120.0 | 9.6 | |
8.00 | 117.3 | 11.8 | 110.1 | 8.4 | ||
12.0 | 120.2 | 6.9 | 110.4 | 14.8 | ||
DON | 800 | 115.6 | 1.8 | 121.2 | 2.6 | |
1600 | 109.0 | 1.4 | 123.4 | 7.4 | ||
2400 | 118.8 | 0.2 | 115.2 | 12.5 | ||
ZEN | 40.0 | 105.5 | 9.4 | 120.9 | 7.3 | |
80.0 | 94.1 | 13.6 | 112.2 | 8.9 | ||
120 | 88.1 | 12.0 | 107.8 | 10.2 |
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