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