Multiwalled Carbon Nanotube for One-Step Cleanup of 21 Mycotoxins in Corn and Wheat Prior to Ultraperformance Liquid Chromatography–Tandem Mass Spectrometry Analysis
Abstract
:1. Introduction
2. Results and Discussion
2.1. UPLC–MS/MS
2.2. Optimization of the SPE Cartridge
2.2.1. Types of MWCNT
2.2.2. Different Combinations of Sorbents
2.2.3. Amounts of MWCNT–COOH
2.3. Evaluation of the Homemade One-Step Cleanup Method
2.4. Method Validation
2.5. Method Application
3. Conclusions
4. Material and Methods
4.1. Reagents
4.2. Standards
4.3. Samples
4.4. Preparation of SPE Cartridges
4.5. Extraction
4.6. UPLC–MS/MS Conditions
4.7. Method Validation
4.8. Statistical Analysis
Supplementary Materials
Author Contributions
Funding
Conflicts of Interest
Abbreviations
15-AcDON | 15-acetyldeoxynivalenol |
3-AcDON | 3-acetyldeoxynivalenol |
AFB1 | aflatoxin B1 |
AFB2 | aflatoxin B2 |
AFG1 | aflatoxin G1 |
AFG2 | aflatoxin G2 |
DAS | diacetoxyscirpenol |
DON | deoxynivalenol |
ESI− | negative mode of electrospray ionization |
ESI+ | positive mode of electrospray ionization |
FUS-X | fusarenon X |
HLB | hydrophilic–lipophilic balanced |
HPLC–MS/MS | high-performance liquid chromatography–tandem mass spectrometry |
IAC | immunoaffinity chromatography |
LOQ | limit of quantification |
MCX | mixed-mode cationic exchange |
MFC | multifunction cleanup columns |
MRM | multiple-reaction monitoring |
MWCNT | multiwalled carbon nanotube |
MWCNT–COOH | carboxylic MWCNT |
MWCNT–OH | hydroxyl MWCNT |
NEO | neosolaniol |
NH2 | amino-propyl |
NH4Ac | ammonium acetate |
NIV | nivalenol |
OTA | ochratoxin A |
OTB | ochratoxin B |
QuEChERS | quick, easy, cheap, effective, rugged, safe |
RSD | relative standard deviation |
SPE | solid-phase extraction |
SPSS | Statistical Package for Social Science |
UPLC–MS/MS | ultraperformance liquid chromatography–tandem mass spectrometry |
ZAN | zearalanone |
ZEN | zearalenone |
α-ZAL | α-zearalanol |
α-ZOL | α-zearalenol |
β-ZAL | β-zearalanol |
β-ZOL | β-zearalenol |
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Mycotoxins | LOQ (μg L−1) | Spiked Levels | Corn | Wheat | ||||
---|---|---|---|---|---|---|---|---|
Recovery (%) | Intraday RSD (%) | Interday RSD (%) | Recovery (%) | Intraday RSD (%) | Interday RSD (%) | |||
DON | 10 | LOQ | 93.4 | 8.2 | 9.6 | 94.7 | 4.1 | 6.3 |
2LOQ | 103.6 | 2.7 | 3.2 | 96.5 | 1.3 | 3.1 | ||
10LOQ | 101.9 | 4.1 | 6.4 | 98.3 | 0.8 | 2.2 | ||
NIV | 25 | LOQ | 90.7 | 5.4 | 6.8 | 92.3 | 2.9 | 4.3 |
2LOQ | 99.4 | 4.8 | 5.4 | 99.3 | 4.4 | 4.8 | ||
10LOQ | 90.7 | 1.1 | 2.5 | 97.2 | 2.7 | 3.5 | ||
AFB1 | 0.5 | LOQ | 78.5 | 3.9 | 5.6 | 85.1 | 2.6 | 4.2 |
2LOQ | 80.5 | 1.7 | 3.4 | 82.4 | 4.4 | 6.5 | ||
10LOQ | 85.6 | 4.1 | 5.4 | 86.9 | 2.9 | 4.9 | ||
AFB2 | 0.5 | LOQ | 82.8 | 2.9 | 4.8 | 78.0 | 5.1 | 10.7 |
2LOQ | 87.5 | 1.8 | 3.6 | 80.3 | 4.6 | 9.2 | ||
10LOQ | 92.8 | 2.2 | 4.9 | 81.9 | 7.2 | 8.2 | ||
AFG1 | 0.5 | LOQ | 90.9 | 3.5 | 5.6 | 97.0 | 3.9 | 8.1 |
2LOQ | 87.8 | 7.1 | 9.8 | 87.8 | 4.2 | 6.5 | ||
10LOQ | 92.7 | 3.7 | 6.7 | 94.8 | 5.4 | 6.9 | ||
AFG2 | 0.5 | LOQ | 90.8 | 3.1 | 4.2 | 95.9 | 3.3 | 4.2 |
2LOQ | 103.6 | 2.8 | 3.5 | 90.5 | 4.0 | 4.8 | ||
10LOQ | 99.7 | 2.4 | 3.7 | 100.9 | 5.0 | 6.1 | ||
15-AcDON | 10 | LOQ | 91.8 | 2.8 | 4.3 | 100.1 | 2.0 | 3.1 |
2LOQ | 103.3 | 3.8 | 4.8 | 95.3 | 2.3 | 3.3 | ||
10LOQ | 98.9 | 4.8 | 5.7 | 97.9 | 0.8 | 2.1 | ||
3-AcDON | 10 | LOQ | 89.2 | 3.7 | 4.8 | 100.0 | 2.0 | 3.2 |
2LOQ | 105.1 | 5.8 | 7.1 | 106.8 | 3.6 | 4.5 | ||
10LOQ | 93.8 | 3.9 | 5.1 | 100.4 | 0.4 | 1.8 | ||
FUS-X | 10 | LOQ | 97.1 | 5.8 | 7.2 | 92.8 | 2.9 | 4.3 |
2LOQ | 96.8 | 2.3 | 3.4 | 86.6 | 3.9 | 5.8 | ||
10LOQ | 84.1 | 3.2 | 4.0 | 101.5 | 1.1 | 3.7 | ||
DAS | 10 | LOQ | 100.5 | 3.5 | 4.2 | 75.6 | 7.8 | 10.4 |
2LOQ | 84.6 | 2.3 | 4.3 | 93.3 | 2.0 | 4.7 | ||
10LOQ | 86.8 | 6.0 | 8.7 | 93.2 | 3.1 | 6.5 | ||
T-2 | 0.5 | LOQ | 79.8 | 4.4 | 9.6 | 80.8 | 4.7 | 9.4 |
2LOQ | 104.3 | 6.0 | 6.6 | 104.8 | 3.3 | 4.3 | ||
10LOQ | 84.9 | 4.9 | 7.3 | 98.8 | 4.6 | 5.8 | ||
HT-2 | 10 | LOQ | 81.4 | 6.8 | 8.9 | 82.2 | 3.3 | 5.7 |
2LOQ | 99.4 | 6.3 | 7.5 | 99.3 | 2.9 | 5.3 | ||
10LOQ | 89.2 | 3.2 | 6.7 | 96.2 | 3.7 | 6.8 | ||
NEO | 25 | LOQ | 88.0 | 7.2 | 8.9 | 97.6 | 4.7 | 5.9 |
2LOQ | 101.0 | 1.9 | 2.5 | 97.9 | 6.0 | 7.6 | ||
10LOQ | 92.3 | 2.9 | 4.1 | 97.9 | 2.2 | 3.6 | ||
OTA | 0.5 | LOQ | 83.2 | 2.9 | 5.4 | 105.5 | 3.0 | 4.2 |
2LOQ | 110.3 | 4.4 | 4.8 | 108.3 | 4.9 | 5.4 | ||
10LOQ | 82.0 | 4.9 | 6.3 | 92.0 | 5.6 | 6.4 | ||
OTB | 0.5 | LOQ | 100.7 | 2.7 | 3.9 | 99.6 | 3.4 | 4.8 |
2LOQ | 101.9 | 3.6 | 4.7 | 100.5 | 3.5 | 3.8 | ||
10LOQ | 92.2 | 3.9 | 5.1 | 93.5 | 3.6 | 4.1 | ||
ZEN | 0.5 | LOQ | 96.5 | 2.2 | 3.2 | 93.1 | 3.0 | 4.1 |
2LOQ | 98.5 | 3.6 | 4.8 | 102.0 | 3.6 | 4.5 | ||
10LOQ | 95.3 | 3.8 | 4.6 | 96.7 | 2.0 | 2.8 | ||
ZAN | 10 | LOQ | 108.1 | 5.0 | 5.6 | 99.6 | 4.6 | 6.2 |
2LOQ | 106.6 | 4.1 | 4.9 | 103.8 | 3.2 | 5.4 | ||
10LOQ | 105.4 | 2.9 | 3.5 | 95.7 | 3.9 | 4.8 | ||
β-ZOL | 10 | LOQ | 102.2 | 2.8 | 4.1 | 99.0 | 3.1 | 3.8 |
2LOQ | 103.0 | 3.4 | 4.9 | 94.0 | 0.3 | 1.8 | ||
10LOQ | 101.7 | 1.9 | 3.5 | 92.5 | 3.2 | 4.1 | ||
α-ZOL | 10 | LOQ | 93.8 | 3.1 | 5.3 | 81.2 | 6.1 | 9.5 |
2LOQ | 96.8 | 1.8 | 2.4 | 88.0 | 4.5 | 6.3 | ||
10LOQ | 96.5 | 2.0 | 3.1 | 89.7 | 3.5 | 5.2 | ||
α-ZAL | 10 | LOQ | 91.8 | 2.6 | 4.2 | 89.5 | 5.2 | 7.8 |
2LOQ | 93.8 | 1.6 | 3.2 | 96.2 | 6.3 | 8.2 | ||
10LOQ | 104.6 | 8.0 | 7.6 | 91.8 | 1.5 | 4.3 | ||
β-ZAL | 10 | LOQ | 91.0 | 7.9 | 9.2 | 94.3 | 3.1 | 6.2 |
2LOQ | 99.1 | 5.2 | 7.5 | 84.6 | 8.1 | 9.8 | ||
10LOQ | 106.3 | 3.0 | 5.4 | 95.8 | 3.4 | 5.2 |
Sample (n) | Mycotoxin | Positives (n) | Occurrence (%) | Mean (μg kg−1) | Range (μg kg−1) |
---|---|---|---|---|---|
Corn (59) | AFB1 | 19 | 32.2 | 2.18 | 0.5–26 |
ZEN | 59 | 100 | 69.3 | 27.5–525 | |
DON | 7 | 11.9 | 410.1 | 65.4–5100 | |
Wheat (53) | ZEN | 13 | 24.5 | 50.7 | 26.8–602 |
DON | 27 | 50.9 | 557.5 | 19.0–4050 | |
3-AcDON | 11 | 20.8 | 68.3 | 13.3–270 | |
15-AcDON | 12 | 22.6 | 49.2 | 10.1–141 |
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Jiang, D.; Wei, D.; Wang, L.; Ma, S.; Du, Y.; Wang, M. Multiwalled Carbon Nanotube for One-Step Cleanup of 21 Mycotoxins in Corn and Wheat Prior to Ultraperformance Liquid Chromatography–Tandem Mass Spectrometry Analysis. Toxins 2018, 10, 409. https://doi.org/10.3390/toxins10100409
Jiang D, Wei D, Wang L, Ma S, Du Y, Wang M. Multiwalled Carbon Nanotube for One-Step Cleanup of 21 Mycotoxins in Corn and Wheat Prior to Ultraperformance Liquid Chromatography–Tandem Mass Spectrometry Analysis. Toxins. 2018; 10(10):409. https://doi.org/10.3390/toxins10100409
Chicago/Turabian StyleJiang, Dongmei, Dizhe Wei, Liuqing Wang, Shuai Ma, Yuanfang Du, and Meng Wang. 2018. "Multiwalled Carbon Nanotube for One-Step Cleanup of 21 Mycotoxins in Corn and Wheat Prior to Ultraperformance Liquid Chromatography–Tandem Mass Spectrometry Analysis" Toxins 10, no. 10: 409. https://doi.org/10.3390/toxins10100409