From:  Analytical methodologies for the determination of sterigmatocystin in food and current concentration levels

Analytical performance of methodologies developed for the determination of sterigmatocystin (STE) in food from 2021 to 2024

SampleExtractionDeterminationLOD/LOQ
(μg/kg or µg/L)
Recovery (%)Concentration levels (μg/kg) (number of samples, detection rate)Ref
Brown rice, wheat25 g sample, 100 mL ACN:water (17:3, v/v)
SPE (Horiba Aflaking IAC)
Dried and reconstituted
LC-MS/MS
InertSustain C18 (150 mm × 2.1 mm, 3 µm)
2 mM NH4Ac in water/2 mM NH4Ac in ACN
0.02–0.03/0.05–0.0986–102Brown rice 0.35–5.70
Polished rice 0.02–0.30
Wheat 0.05–2.20
Bread 0.02–0.20
Baked sweets 0.01–0.20
Noodles 0.01–0.80
[23]
Rice, maize, soybean5 g sample, 25 mL MeOH:water (7:3, v/v)
30 min shaking
SPE (HMON@MIP)
TFA + hexane derivatization
Dried and reconstituted
LC-FD
Symmetry C18 (250 mm × 4.6 mm, 5 µm)
ACN:water (32:68, v/v)
-81–95-[24]
Chilli, pepper50 g sample, 10% KCl in ACN
LLE (2x hexane)
LLE (hexane:CHCl3, 1:1 v/v)
Dried and reconstituted
GO-FAM-FRET24/13271–89-[25]
Soaked rice, steamed rice, fermented rice, fermented wineQuEChERSLC-MS/MS
Acquity UPLC HSS T3 (100 mm × 2.1 mm, 1.8 μm)
0.1% FA + 2 mM AF in water/0.1% FA + 2 mM AF in ACN
0.01–0.07/0.03–0.2573–119-[26]
Wheat10 g sample, 25 mL ACN:water (9:1, v/v), 1 g MgSO4, 1 g NaCl
30 min shacking
20 min centrifugation
MSPE (Fe3O4-MIP) elution 5 mL MeOH:TEA (9:1, v/v)
20 min shaking
Dried and reconstituted
LC-DAD0.63/-88–973.4–4.5[27]
Cereals, nuts, vegetables, oil, noodle, paste, seasoned food, instant food5 g sample, 20 mL 0.1% FA in ACN:water (1:1, v/v)
30 min shaking
10 min centrifugation
SPE (Isolute Myco) elution 2 mL 0.1% FA in ACN + 4 mL MeOH
Dried and reconstituted
LC-MS/MS
Imtakt Cadenza C18 (100 mm × 2 mm, 3 μm)
0.1% FA + 5 mM AF in water/0.1% FA + 5 mM AF in MeOH
0.4–0.9/1.2–2.869–112Processed foods 0.08–1.93 (n = 522, 4.2%)
Agricultural products 0.08–10.07 (n = 613, 3.9%)
[28]
Black, green, and Oolong teasQuEChERS
5.0 g sample, ACN:water (75:25, v/v)
30 min UAE, 1 g NaCl, 1 g MgSO4
5 min centrifugation
dSPE (C18)
5 min centrifugation
LC-MS/MS
Shim-pack XR-ODS III (75 mm × 2.0 mm, 1.6 µm)
0.1% FA + 5 mM AF in water/0.1% FA + 5 mM AF in ACN
0.04–0.12/0.13–0.40101–1180.13–0.48 (n = 126, 13.5%)[29]
Wheat5 g sample, 20 mL ACN:water (8:2, v/v)
10 min UAE
5 min centrifugation
MSPE (MHNTs@MIP) elution 5.3 mL EtOH:HAc (9:1, v/v)
Dried and reconstituted
LC-DAD
Hedera ODS-2 (250 mm × 4.6 mm)
MeOH:water (60:40 v/v)
1.1/3.589–103-[30]
Roasted coffee bean, black pepper10 g sample, 40 mL MeOH:water (8:2, v/v)
5 min shaking
2 min centrifugation
SPE (Envi-carb SPE) elution 6 mL toluene
Hexane cleaning
SPE (IAC) elution 2 mL ACN
LC-MS/MS
Acquity CSH C18 (150 mm × 2.1 mm, 1.7 μm)
0.05 M FA and AF in MeOH:water (8:2, v/v)/water
0.03/0.1092–1050.08–0.87 (n = 18, 22%)[31]
Rice, wheat5 g sample, 10 mL ACN:water (8:2, v/v)
10 min UAE
5 min centrifugation
Dried and redissolved in 10 mL water
15 min dSPE [SiO2@mPMO-IL(im)2] elution 2 mL MeOH
5 min centrifugation
Dried and reconstituted
LC-MS/MS
ODS (250 mm × 4.6 mm, 5 μm)
ACN:MeOH:water (22:22:55, v/v/v)/ACN:MeOH:water (35:35:30, v/v/v)
0.9–1.5/3.0–4.592–102-[32]
Coix seed5 g sample, 20 mL 0.1% FA in ACN:water (7:3, v/v)
30 min mechanically shaking
5 min centrifugation
SIDA-UHPLC-MS/MS0.03/0.1083–88LOQ–23 (n = 60, 83%)[33]
Mango, litchi, longan, and their products2 g sample, 10 mL 1% HAc in ACN:water (8:2, v/v)
10 min UAE
5 min centrifugation
dSPE (PSA, C18)
10 min vortex shaking
5 min centrifugation
Dried and reconstituted tube
LC-MS/MS
Acquity BEH C18 (100 mm × 2.1 mm, 1.7 μm)
Water/0.2% FA in ACN
0.01/0.0484–116-[34]
Honey1.5 g sample, 3 mL water, 2.5 mL ACN, 1 g MgSO4, 0.25 g NaCl, 0.25 g Na3Cit, 0.125 g Na2HCit
1 min hand shaking
10 min centrifugation
2 min dSPE (MgSO4)
10 min centrifugation
Dried and reconstituted
LC-MS/MS
Eclipse Plus C18 RRHT (100 mm × 2.1 mm, 1.8 µm)
0.2 M NH4HCO3 in water/0.2 M NH4HCO3 in ACN
0.3/1.0101–1030.4–18.7 (n = 57, 3.5%)[35]
Pale lager beer25 mL sample, pH adjustment to 7.4
SPE (11+Myco MS-PREP IAC) elution 2 mL MeOH
Dried and reconstituted
LC-MS/MS
Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 µm)
1 mM NH4Ac + 0.5% HAc + 0.1% FA in water/0.5% HAc + 0.1% FA in MeOH
-27-[36]
Rice5 g sample, 10 mL ACN:water (8:2, v/v)
10 min UAE
5 min centrifugation
Dried and reconstituted in 10 mL water
25 min MSPE (Fe3O4/ZIFs) elution 2 mL 10% FA in ACN
Dried and reconstituted
LC-DAD
ODS column (250 mm × 4.6 mm, 5 μm)
Water/0.05% H3PO4 in ACN
0.4/1.279–951.2–2.2 (n = 56, 3.6%)[37]
Cocoa beans7.5 g sample, 18 mL 5% HAc in ACN:water (7:3, v/v), 3 g NaCl
60 min shaking
15 min freezing, –70°C
10 min centrifugation
LC-MS/MS
Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm)
0.1% FA + 5 mM AF + 2% MeOH in water/0.1% FA in ACN
3/1097–10910–11 (n = 135, 1.5%)[38]
Spice, herb-LC-MS/MS--0.4–7.8 (n = 155, 4%)[39]
Rice, wheat5 g sample, 10 mL 10% FA in water, 10 mL ACN, 4 g MgSO4, 1 g NaCl, 1 g Na3Cit, 0.5 g Na2HCit
5 min shaking
5 min centrifugation
SPE (Oasis Prime HLB)
LC-MS/MS
Acquity HSS T3 C18 (100 mm × 2.1 mm, 1.8 μm)
1% HAc + 5 mM NH4Ac in water/1% HAc + 5 mM NH4Ac in MeOH
2/---[40]
Arecae semen2 g sample, 15 mL 0.2% FA in ACN:water (84:16, v/v)
10 min UAE
10 min centrifugation
S-µSPE (MycoSpin 400)
Dried and reconstituted
LC-MS/MS
Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 µm)
0.1% FA in MeOH/2 mM AF in water
0.3/1.094–105LOQ–2.2 (n = 20, 15%)[41]
Plant-based milk alternativesNo sample treatmentELISA2/- (ELISA)-Soy (n = 7, 14%)
Almond (n = 7, 0%)
Oat (n = 14, 14%)
Others (n = 26, 8%)
[42]
10 mL sampleLLE (EtAc)
Dried and reconstituted in PBS
SPE (VICAM AflaTest WB SR+ IAC) elution 3 mL MeOH
LC-MS/MSPhenomenex C18 (100 mm × 3.0 mm, 5.0 µm)
0.1% FA + 300 mg/L AF in water/0.1% FA + 300 mg/L AF in MeOH
Edible oil, soy sauce, bean sauce2 g sample, 20 mL ACN:water (8:2, v/v)
10 min orbital shaking
5 min centrifugation
LLE (Hexane)
3 min centrifugation
SPE (Oasis PRiME HLB)
Dried and reconstituted
LC-HRMS
Accucore aQ C18 (150 mm × 2.1 mm, 2.6 μm)
0.1% FA in water/0.1% FA in MeOH
0.3/1.071–104Sesame oil LOQ–2.9 (n = 12, 8%)[43]
Corn, millet, rice, soybean, oats5 g sample, 25 mL ACN:water (8:2, v/v)
30 min shaking
Centrifugation
SPE (COF@MIP) elution 5 mL ACN
Dried and reconstituted
LC-DAD
Waters Symmetry-C18 (250 mm × 4.6 mm, 5 µm)
MeOH:water (80:20, v/v)
2/879–98-[44]
Rice bran, maize1 g sample, 4 mL 1% FA in ACN:water (8:2, v/v)
90 min vortex shaking
15 min centrifugation
LC-MS/MS
Gemini C18 (100 mm × 4.6 mm, 5 μm)
5 mM NH4Ac + 1% HAC in water/5 mM NH4Ac + 1% HAC in MeOH
0.5/2.592–105Rice bran 2.8–272.3 (n = 125, 98%)
Maize 0.3–17.9 (n = 125, 43%)
[45]
Dry-cured meat productsQuEChERS
SPE defatting (Captiva EMR-Lipid)
SPE (Easi-extract sterigmatocystin IAC)
LC-MS/MS
Gemini (150 mm × 4.6 mm, 5 µm)
0.02/0.061140.10–3.93 (n = 250, 4%)[46]
Licorice2 g sample, 20 mL ACN:water (84:16, v/v)
30 min UAE
QuEChERS (4 g MgSO4, 1 g NaCl, 1 g Na3Cit, 0.5 g Na2HCit)
30 min MSPE [Fe3O4@PDA/MIL-101(Cr)]
Dried and reconstituted
LC-MS/MS
Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm)
5 mM NH4Ac + 0.1% NH3 in water/5 mM NH4Ac + 0.1% NH3 in MeOH
0.09/0.30107–116-[47]
Long-ripened Grana cheese10 g sample, 50 mL ACN:water (8:2, v/v)
60 min rotary shaking
Filtration, 2 mL PBS
SPE (R-Biopharm-Rhône IAC) elution 6 mL ACN
Dried and reconstituted
LC-MS/MS
Betasil RP-18 (150 mm × 2.1 mm, 5 µm)
0.2% FA in water/0.2% FA in ACN
0.05/0.1587–92LOQ–6.9 (n = 107, 94%)[48]
Pseudostellariae RadixACN:water (8:2, v/v)
1 h shaking
dSPE (PSA + C18 + MgSO4)
LC-MS/MS
Acquity HSS T3 (100 mm × 2.1 mm, 1.8 μm)
0.1% FA in water/0.1% FA in ACN
--1.5–69.6 (n = 26, 38%)[49]
Peanut butter, hazelnut butter, chocolate5 g sample, 20 mL JSM FO 9704
15 min shaking
5 min centrifugation
LC-MS/MS0.01–0.02/0.05–0.1594–1000.2–2.2[50]
Cocoa7.5 g sample, 18 mL 0.5% HAc in ACN:water (7:3, v/v), 3 g NaCl
60 min shaking
15 min frozen at –70°C
10 min centrifugation
LC-MS/MS
Titan C18 (100 mm × 2.1 mm, 1.9 μm)
--2.4–3.3 (n = 18, 11%)[51]
Carob1 g sample, 10 mL water, 10 mL 1% HAc in ACN
10 min UAE
10 min shaking, 1 g NaCl, 4 g MgSO4
Dried and reconstituted
LC-MS/MS
Titan C18 (100 mm × 2.1 mm, 1.9 μm)
--0.15–0.18 (n = 22, 14%)[51]
Cheese2.5 g sample, 5 mL 0.1% FA in ACN, 5 mL saturated MgSO4
30 min shaking
7 min centrifugation
Defatting, 4 mL heptane
5 min shaking
Dried and reconstituted
LC-MS/MS
Gemini C18 (100 mm × 3.0 mm, 5.0 μm)
0.1% FA + 300 mg/L AF in water/0.1% FA + 300 mg/L AF in MeOH
0.01/0.04100–1060.08–4.99 (n = 11, 82%)[52]
Goat, camel, and cow milk1 mL sample, 1 mL 1% FA in ACN, 0.4 g MgSO4, 0.1 g NaCl
10 min centrifugation
LC-MS/MS
Acquity HSS T3 (100 mm × 2.1 mm, 1.8 μm)
0.1% HAc + 5 mM NH4Ac in water/0.1% HAc + 5 mM NH4Ac in MeOH
--LOQ–7.7 (n = 135, 14%)[53]
Cereal-based baby food2 g sample, 10 mL JSM FO 9704
15 min shaking
5 min centrifugation
LC-MS/MS0.02/0.071000.02–0.50 (n = 85, 34%)[54]
Rice, peanut, maize, sorghum5 g sample, 20 mL 1% HAc in ACN:water (8:2, v/v)LC-MS/MS--Peanut 0.1–30 (n = 53, 40%)
Maize 0.1–12 (n = 142, 26%)
Rice 0.1–2.2 (n = 23, 48%)
Sorghum 0.1–2.5 (n = 24, 12%)
[55]
Hazelnut kernels25 g sample, 100 mL MeOH:water (8:2, v/v), 5 g NaCl
3 min extraction
PBS dilution
SPE (Easi-Extract Sterigmatocystin IAC) elution 1.5 mL ACN
Dried and reconstituted
LC-FLD
ODS2 C18-300 (150 mm × 4.6 mm, 3 μm)
120 mg/L KBr + 350 µL/L HNO3 in ACN:MeOH:water (10:15:75, v/v)
1.3/4.281–879–101 (n = 30, 5%)[56]
Herbs, herbal infusions1 g herb sample, 5 mL water, 30 min shaking5 mL 1% FA in ACN, 2 g MgSO4, 1 g NaCl
1 h orbital shaking
15 min centrifugation
dSPE (C18, Z-sep+)
Dried and reconstituted
LC-MS/MS
Kinetex C18 (150 mm × 4.6 mm, 2.6 μm)
5 mM NH4Ac in water:MeOH:HAc (94:5:1, v/v)/water:MeOH:HAc (2:97:1, v/v)
0.5–20/2.5–4073–10134–147 (n = 58, 19%)[57]
1 g infusion sample, 50 mL hot water, 15 min shacking5 min centrifugation
5 mL ACN, 2 g MgSO4, 1 g NaCl
5 min centrifugation
Dried and reconstituted
Malt, beer5 g malt sample, 2 g MgSO4, 1 g NaCl, 15 mL ACN:water (75:25, v/v)6 min centrifugation
d-SPE (MgSO4, C18)
Dried and reconstituted
LC-HRMS/MS
Kinetex Core-Shell F5 100 A (2.6 µm)
0.1% HAc + 4 mM NH4Ac in water/0.1% HAc + 4 mM NH4Ac in ACN
5/1290–97LOQ (n = 47, 0%)[58]
5 mL beer sample, 5 mL ACN, 2 g MgSO4, 1 g NaCl3 min UAE
5 min centrifugation
dSPE (MgSO4, C18)
Dried and reconstituted
Rice bran20 g sample, 80 mL MeOH:water (8:2, v/v)
15 min UAE
5 min centrifugation
DLLME (CHCl3/water)
5 min centrifugation
Dried and reconstituted
LC-MS/MS
Accucore C18 (100 mm × 2.1 mm, 2.6 μm)
2.5/5.099LOQ (n = 24, 0%)[59]
Milled rice5 g sample, 20 mL 1% FA in ACN:water (8:2, v/v)
90 min shaking
LC-MS/MS
Synergi Hydro-RP (100 mm × 3 mm, 2.5 µm)
1% FA and 10 mM NH4Ac in water/MeOH
0.03/0.0980LOQ–7 (n = 200, 74%)[60]
Dairy products2 g sample, 8 mL 2% FA in ACN
30 min UAE
5 min centrifugation
SPE (Captiva EMR-lipid)
Dried and reconstituted
LC-MS/MS
Shiseido C18 (100 mm × 2.1 mm, 3 μm)
0.1% FA in water/0.1% FA in MeOH
0.005/0.02073LOQ (n = 76, 0%)[61]
Milling oats5 g sample, 20 mL 1% HAc in ACN:water (8:2, v/v)
90 min shaking
S-µSPE (MycoSpin 400)
Dried and reconstituted
LC-MS/MS
Eclipse Plus C18 (100 mm × 2.1 mm, 1.8 µm)
0.1% HAc + 5 mM NH4Ac in water/0.1% HAc + 5 mM NH4Ac in MeOH
-/1951–7 (n = 281, 2.3%)[62]
Garlic5 g sample, 20 mL 1% HAc in ACN:water (8:2, v/v)
Vortex shaking
LC-MS/MS
Gemini C18 (150 mm × 4.6 mm, 5 μm)
0.05/0.14903–32 (n = 36, 100%)[63]
Coix seed5 g sample, 20 mL 1% FA in ACN:water (7:3, v/v)
20 min vortex shaking
5 min centrifugation
LC-HRMS
CORTECS C18 (100 mm × 2.1 mm, 1.6 μm)
0.1% FA + 1 mM NH4Ac in water/0.1% FA + 1 mM NH4Ac in MeOH
-/176–891–51 (n = 77, 30%)[64]

-: not indicated. SPE: solid-phase extraction; LOD: limit of detection; LOQ: limit of quantification; LC: liquid chromatography; MS: mass spectrometry; HMON@MIP: hollow-structured microporous organic networks coated with molecularly imprinted polymers; FD: fluorescence; GO-FAM-FRET: graphene oxide-aptamer-FD resonance energy transfer; QuEChERS: quick, easy, cheap, effective, rugged, and safe; MSPE: magnetic SPE; DAD: diode array; UAE: ultrasound-assisted extraction; dSPE: dispersive SPE; SiO2@mPMO-IL(im)2: ionic liquid-functionalized mesoporous multipod silica; UHPLC: ultra-high-performance LC; PSA: primary secondary amine; ZIFs: zeolitic imidazolate frameworks; COF@MIP: MIPs-coated covalent organic framework nanoflowers; DLLME: dispersive liquid-liquid microextraction; HRMS: high-resolution MS; ELISA: enzyme-linked immunosorbent assay; ACN: acetonitrile; IAC: immunoaffinity column; TFA: trifluoroacetic acid; LLE: liquid-liquid extraction; FA: formic acid; AF: ammonium formiate; TEA: triethylamine; SIDA: stable isotope dilution assay; S-µSPE: spin micro SPE; PBS: phosphate buffer saline; FLD: fluorescence detector; MHNTs@MIP: magnetic halloysite nanotubes coated molecular imprinted polymer