Acta Agriculturae Zhejiangensis ›› 2022, Vol. 34 ›› Issue (12): 2728-2739.DOI: 10.3969/j.issn.1004-1524.2022.12.16
• Food Science • Previous Articles Next Articles
DENG Tao1(), YANG Hua2, XIAO Yingping2, WANG Wen2, LYU Wentao2, WANG Xiaoli2, WU Zhen1,*(
), JI Xiaofeng2,*(
)
Received:
2022-01-24
Online:
2022-12-25
Published:
2022-12-26
Contact:
WU Zhen,JI Xiaofeng
CLC Number:
DENG Tao, YANG Hua, XIAO Yingping, WANG Wen, LYU Wentao, WANG Xiaoli, WU Zhen, JI Xiaofeng. Simultaneous determination of five Alternaria toxins by QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry in fruit puree for infants[J]. Acta Agriculturae Zhejiangensis, 2022, 34(12): 2728-2739.
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URL: http://www.zjnyxb.cn/EN/10.3969/j.issn.1004-1524.2022.12.16
真菌毒素 Mycotoxin | 母离子 Precursor ion/ (m/z) | 子离子 Product ions/ (m/z) | 去簇电压 Declustering potential/eV | 碰撞能量 Collision energy/eV | ESI扫描方式 ESI Scanning way | 保留时间 Retention time/min |
---|---|---|---|---|---|---|
TeA | 196.0 | 139.0* | -50 | -28 | - | 4.01 |
112.0 | -50 | -40 | ||||
TEN | 413.3 | 271.1 | -123 | -23 | - | 6.37 |
140.8* | -126 | -27 | ||||
AME | 271.2 | 256.2* | -100 | -28 | - | 6.92 |
228.2 | -100 | -42 | ||||
AOH | 257.0 | 213.2* | -120 | -32 | - | 6.28 |
147.2 | -120 | -42 | ||||
ALT | 293.0 | 257.0* | 57 | 19 | + | 5.81 |
239.0 | 70 | 29 |
Table 1 MS-MS parameters for five Alternaria toxins
真菌毒素 Mycotoxin | 母离子 Precursor ion/ (m/z) | 子离子 Product ions/ (m/z) | 去簇电压 Declustering potential/eV | 碰撞能量 Collision energy/eV | ESI扫描方式 ESI Scanning way | 保留时间 Retention time/min |
---|---|---|---|---|---|---|
TeA | 196.0 | 139.0* | -50 | -28 | - | 4.01 |
112.0 | -50 | -40 | ||||
TEN | 413.3 | 271.1 | -123 | -23 | - | 6.37 |
140.8* | -126 | -27 | ||||
AME | 271.2 | 256.2* | -100 | -28 | - | 6.92 |
228.2 | -100 | -42 | ||||
AOH | 257.0 | 213.2* | -120 | -32 | - | 6.28 |
147.2 | -120 | -42 | ||||
ALT | 293.0 | 257.0* | 57 | 19 | + | 5.81 |
239.0 | 70 | 29 |
Fig.7 Effect of purifying agent C18 and PSA on the recoveries of five Alternaria toxins (at spiked level of 20 μg·kg-1) * indicated the significant difference (P<0.05).
真菌毒素 Mycotoxin | 线性范围 Linear range/ (μg·kg-1) | 线性方程 Linearity | 决定系数 Determination coefficient (R2) | 检测限 Limit of detection/ (μg·kg-1) | 定量限 Limit of quantification/ (μg·kg-1) |
---|---|---|---|---|---|
TeA | 0.1~200 | y=6 518.6x-4 576.6 | 0.998 8 | 0.1 | 0.3 |
TEN | 0.1~200 | y=68 726x+242 291 | 0.998 6 | 0.1 | 0.3 |
AME | 0.1~200 | y=366 699x+610 963 | 0.999 6 | 0.1 | 0.3 |
AOH | 0.1~200 | y=104 261x+95 424 | 0.999 8 | 0.1 | 0.3 |
ALT | 0.1~200 | y=87 531x-43 124 | 0.999 6 | 0.1 | 0.3 |
Table 2 Linear relationship, limit of detection, limit of quantitation of five Alternaria toxins
真菌毒素 Mycotoxin | 线性范围 Linear range/ (μg·kg-1) | 线性方程 Linearity | 决定系数 Determination coefficient (R2) | 检测限 Limit of detection/ (μg·kg-1) | 定量限 Limit of quantification/ (μg·kg-1) |
---|---|---|---|---|---|
TeA | 0.1~200 | y=6 518.6x-4 576.6 | 0.998 8 | 0.1 | 0.3 |
TEN | 0.1~200 | y=68 726x+242 291 | 0.998 6 | 0.1 | 0.3 |
AME | 0.1~200 | y=366 699x+610 963 | 0.999 6 | 0.1 | 0.3 |
AOH | 0.1~200 | y=104 261x+95 424 | 0.999 8 | 0.1 | 0.3 |
ALT | 0.1~200 | y=87 531x-43 124 | 0.999 6 | 0.1 | 0.3 |
真菌毒素 Mycotoxin | 添加浓度 Spiked concentration/ (μg·kg-1) | 精密度 Accuracy/% | 相对标准偏差RSD/% | ||
---|---|---|---|---|---|
日内/(n=6) Intra-day/(n=6) | 日间/(n=18) Inter-day/(n=18) | 日内/(n=6) Intra-day/(n=6) | 日间/(n=18) Inter-day/(n=18) | ||
TeA | 5 | 73.8±2.4 | 78.5±9.0 | 3.2 | 8.5 |
20 | 82.6±5.5 | 83.6±6.3 | 6.7 | 7.5 | |
50 | 77.3±3.2 | 81±±5.6 | 4.1 | 7.0 | |
TEN | 5 | 115.3±4.8 | 117.9±5.3 | 4.1 | 4.5 |
20 | 116.9±3.9 | 112.6±4.9 | 3.3 | 4.3 | |
50 | 117.3±2.7 | 118.0±8.2 | 2.3 | 7.0 | |
AME | 5 | 97.4±4.0 | 93.1±4.4 | 4.1 | 4.8 |
20 | 91.0±5.0 | 92.8±5.1 | 5.5 | 5.8 | |
50 | 96.3±5.6 | 95.5±4.9 | 5.8 | 6.1 | |
AOH | 5 | 107.7±2.6 | 106.3±4.8 | 2.4 | 4.5 |
20 | 105.9±2.5 | 105.5±2.5 | 2.3 | 2.4 | |
50 | 101.9±8.3 | 104.2±8.5 | 8.2 | 8.2 | |
ALT | 5 | 108.2±6.8 | 109.6±6.3 | 6.3 | 7.7 |
20 | 107.7±3.3 | 106.0±3.5 | 3.1 | 3.3 | |
50 | 112.3±3.4 | 111.9±3.3 | 3.0 | 4.3 |
Table 3 Recoveries and intra- and inter-day accuracy and precision for the determination of five Alternaria toxins
真菌毒素 Mycotoxin | 添加浓度 Spiked concentration/ (μg·kg-1) | 精密度 Accuracy/% | 相对标准偏差RSD/% | ||
---|---|---|---|---|---|
日内/(n=6) Intra-day/(n=6) | 日间/(n=18) Inter-day/(n=18) | 日内/(n=6) Intra-day/(n=6) | 日间/(n=18) Inter-day/(n=18) | ||
TeA | 5 | 73.8±2.4 | 78.5±9.0 | 3.2 | 8.5 |
20 | 82.6±5.5 | 83.6±6.3 | 6.7 | 7.5 | |
50 | 77.3±3.2 | 81±±5.6 | 4.1 | 7.0 | |
TEN | 5 | 115.3±4.8 | 117.9±5.3 | 4.1 | 4.5 |
20 | 116.9±3.9 | 112.6±4.9 | 3.3 | 4.3 | |
50 | 117.3±2.7 | 118.0±8.2 | 2.3 | 7.0 | |
AME | 5 | 97.4±4.0 | 93.1±4.4 | 4.1 | 4.8 |
20 | 91.0±5.0 | 92.8±5.1 | 5.5 | 5.8 | |
50 | 96.3±5.6 | 95.5±4.9 | 5.8 | 6.1 | |
AOH | 5 | 107.7±2.6 | 106.3±4.8 | 2.4 | 4.5 |
20 | 105.9±2.5 | 105.5±2.5 | 2.3 | 2.4 | |
50 | 101.9±8.3 | 104.2±8.5 | 8.2 | 8.2 | |
ALT | 5 | 108.2±6.8 | 109.6±6.3 | 6.3 | 7.7 |
20 | 107.7±3.3 | 106.0±3.5 | 3.1 | 3.3 | |
50 | 112.3±3.4 | 111.9±3.3 | 3.0 | 4.3 |
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