Analytical performance of methodologies developed for the determination of sterigmatocystin (STE) in food from 2021 to 2024
Sample | Extraction | Determination | LOD/LOQ(μg/kg or µg/L) | Recovery (%) | Concentration levels (μg/kg) (number of samples, detection rate) | Ref | ||
---|---|---|---|---|---|---|---|---|
Brown rice, wheat | 25 g sample, 100 mL ACN:water (17:3, v/v)SPE (Horiba Aflaking IAC)Dried and reconstituted | LC-MS/MSInertSustain C18 (150 mm × 2.1 mm, 3 µm)2 mM NH4Ac in water/2 mM NH4Ac in ACN | 0.02–0.03/0.05–0.09 | 86–102 | Brown rice 0.35–5.70Polished rice 0.02–0.30Wheat 0.05–2.20Bread 0.02–0.20Baked sweets 0.01–0.20Noodles 0.01–0.80 | [23] | ||
Rice, maize, soybean | 5 g sample, 25 mL MeOH:water (7:3, v/v)30 min shakingSPE (HMON@MIP)TFA + hexane derivatizationDried and reconstituted | LC-FDSymmetry C18 (250 mm × 4.6 mm, 5 µm)ACN:water (32:68, v/v) | - | 81–95 | - | [24] | ||
Chilli, pepper | 50 g sample, 10% KCl in ACNLLE (2x hexane)LLE (hexane:CHCl3, 1:1 v/v)Dried and reconstituted | GO-FAM-FRET | 24/132 | 71–89 | - | [25] | ||
Soaked rice, steamed rice, fermented rice, fermented wine | QuEChERS | LC-MS/MSAcquity 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 | 0.01–0.07/0.03–0.25 | 73–119 | - | [26] | ||
Wheat | 10 g sample, 25 mL ACN:water (9:1, v/v), 1 g MgSO4, 1 g NaCl30 min shacking20 min centrifugationMSPE (Fe3O4-MIP) elution 5 mL MeOH:TEA (9:1, v/v)20 min shakingDried and reconstituted | LC-DAD | 0.63/- | 88–97 | 3.4–4.5 | [27] | ||
Cereals, nuts, vegetables, oil, noodle, paste, seasoned food, instant food | 5 g sample, 20 mL 0.1% FA in ACN:water (1:1, v/v)30 min shaking10 min centrifugationSPE (Isolute Myco) elution 2 mL 0.1% FA in ACN + 4 mL MeOHDried and reconstituted | LC-MS/MSImtakt Cadenza C18 (100 mm × 2 mm, 3 μm)0.1% FA + 5 mM AF in water/0.1% FA + 5 mM AF in MeOH | 0.4–0.9/1.2–2.8 | 69–112 | Processed foods 0.08–1.93 (n = 522, 4.2%)Agricultural products 0.08–10.07 (n = 613, 3.9%) | [28] | ||
Black, green, and Oolong teas | QuEChERS5.0 g sample, ACN:water (75:25, v/v)30 min UAE, 1 g NaCl, 1 g MgSO45 min centrifugationdSPE (C18)5 min centrifugation | LC-MS/MSShim-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 | 0.04–0.12/0.13–0.40 | 101–118 | 0.13–0.48 (n = 126, 13.5%) | [29] | ||
Wheat | 5 g sample, 20 mL ACN:water (8:2, v/v)10 min UAE5 min centrifugationMSPE (MHNTs@MIP) elution 5.3 mL EtOH:HAc (9:1, v/v)Dried and reconstituted | LC-DADHedera ODS-2 (250 mm × 4.6 mm)MeOH:water (60:40 v/v) | 1.1/3.5 | 89–103 | - | [30] | ||
Roasted coffee bean, black pepper | 10 g sample, 40 mL MeOH:water (8:2, v/v)5 min shaking2 min centrifugationSPE (Envi-carb SPE) elution 6 mL tolueneHexane cleaningSPE (IAC) elution 2 mL ACN | LC-MS/MSAcquity CSH C18 (150 mm × 2.1 mm, 1.7 μm)0.05 M FA and AF in MeOH:water (8:2, v/v)/water | 0.03/0.10 | 92–105 | 0.08–0.87 (n = 18, 22%) | [31] | ||
Rice, wheat | 5 g sample, 10 mL ACN:water (8:2, v/v)10 min UAE5 min centrifugationDried and redissolved in 10 mL water15 min dSPE [SiO2@mPMO-IL(im)2] elution 2 mL MeOH5 min centrifugationDried and reconstituted | LC-MS/MSODS (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) | 0.9–1.5/3.0–4.5 | 92–102 | - | [32] | ||
Coix seed | 5 g sample, 20 mL 0.1% FA in ACN:water (7:3, v/v)30 min mechanically shaking5 min centrifugation | SIDA-UHPLC-MS/MS | 0.03/0.10 | 83–88 | LOQ–23 (n = 60, 83%) | [33] | ||
Mango, litchi, longan, and their products | 2 g sample, 10 mL 1% HAc in ACN:water (8:2, v/v)10 min UAE5 min centrifugationdSPE (PSA, C18)10 min vortex shaking5 min centrifugationDried and reconstituted tube | LC-MS/MSAcquity BEH C18 (100 mm × 2.1 mm, 1.7 μm)Water/0.2% FA in ACN | 0.01/0.04 | 84–116 | - | [34] | ||
Honey | 1.5 g sample, 3 mL water, 2.5 mL ACN, 1 g MgSO4, 0.25 g NaCl, 0.25 g Na3Cit, 0.125 g Na2HCit1 min hand shaking10 min centrifugation2 min dSPE (MgSO4)10 min centrifugationDried and reconstituted | LC-MS/MSEclipse Plus C18 RRHT (100 mm × 2.1 mm, 1.8 µm)0.2 M NH4HCO3 in water/0.2 M NH4HCO3 in ACN | 0.3/1.0 | 101–103 | 0.4–18.7 (n = 57, 3.5%) | [35] | ||
Pale lager beer | 25 mL sample, pH adjustment to 7.4SPE (11+Myco MS-PREP IAC) elution 2 mL MeOHDried and reconstituted | LC-MS/MSAcquity 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] | ||
Rice | 5 g sample, 10 mL ACN:water (8:2, v/v)10 min UAE5 min centrifugationDried and reconstituted in 10 mL water25 min MSPE (Fe3O4/ZIFs) elution 2 mL 10% FA in ACNDried and reconstituted | LC-DADODS column (250 mm × 4.6 mm, 5 μm)Water/0.05% H3PO4 in ACN | 0.4/1.2 | 79–95 | 1.2–2.2 (n = 56, 3.6%) | [37] | ||
Cocoa beans | 7.5 g sample, 18 mL 5% HAc in ACN:water (7:3, v/v), 3 g NaCl60 min shaking15 min freezing, –70°C10 min centrifugation | LC-MS/MSAcquity 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 | 3/10 | 97–109 | 10–11 (n = 135, 1.5%) | [38] | ||
Spice, herb | - | LC-MS/MS | - | - | 0.4–7.8 (n = 155, 4%) | [39] | ||
Rice, wheat | 5 g sample, 10 mL 10% FA in water, 10 mL ACN, 4 g MgSO4, 1 g NaCl, 1 g Na3Cit, 0.5 g Na2HCit5 min shaking5 min centrifugationSPE (Oasis Prime HLB) | LC-MS/MSAcquity 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 semen | 2 g sample, 15 mL 0.2% FA in ACN:water (84:16, v/v)10 min UAE10 min centrifugationS-µSPE (MycoSpin 400)Dried and reconstituted | LC-MS/MSAcquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 µm)0.1% FA in MeOH/2 mM AF in water | 0.3/1.0 | 94–105 | LOQ–2.2 (n = 20, 15%) | [41] | ||
Plant-based milk alternatives | No sample treatment | ELISA | 2/- (ELISA) | - | Soy (n = 7, 14%)Almond (n = 7, 0%)Oat (n = 14, 14%)Others (n = 26, 8%) | [42] | ||
10 mL sample | LLE (EtAc)Dried and reconstituted in PBSSPE (VICAM AflaTest WB SR+ IAC) elution 3 mL MeOH | LC-MS/MS | Phenomenex 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 sauce | 2 g sample, 20 mL ACN:water (8:2, v/v)10 min orbital shaking5 min centrifugationLLE (Hexane)3 min centrifugationSPE (Oasis PRiME HLB)Dried and reconstituted | LC-HRMSAccucore aQ C18 (150 mm × 2.1 mm, 2.6 μm)0.1% FA in water/0.1% FA in MeOH | 0.3/1.0 | 71–104 | Sesame oil LOQ–2.9 (n = 12, 8%) | [43] | ||
Corn, millet, rice, soybean, oats | 5 g sample, 25 mL ACN:water (8:2, v/v)30 min shakingCentrifugationSPE (COF@MIP) elution 5 mL ACNDried and reconstituted | LC-DADWaters Symmetry-C18 (250 mm × 4.6 mm, 5 µm)MeOH:water (80:20, v/v) | 2/8 | 79–98 | - | [44] | ||
Rice bran, maize | 1 g sample, 4 mL 1% FA in ACN:water (8:2, v/v)90 min vortex shaking15 min centrifugation | LC-MS/MSGemini C18 (100 mm × 4.6 mm, 5 μm)5 mM NH4Ac + 1% HAC in water/5 mM NH4Ac + 1% HAC in MeOH | 0.5/2.5 | 92–105 | Rice bran 2.8–272.3 (n = 125, 98%)Maize 0.3–17.9 (n = 125, 43%) | [45] | ||
Dry-cured meat products | QuEChERSSPE defatting (Captiva EMR-Lipid)SPE (Easi-extract sterigmatocystin IAC) | LC-MS/MSGemini (150 mm × 4.6 mm, 5 µm) | 0.02/0.06 | 114 | 0.10–3.93 (n = 250, 4%) | [46] | ||
Licorice | 2 g sample, 20 mL ACN:water (84:16, v/v)30 min UAEQuEChERS (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/MSAcquity 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 | 0.09/0.30 | 107–116 | - | [47] | ||
Long-ripened Grana cheese | 10 g sample, 50 mL ACN:water (8:2, v/v)60 min rotary shakingFiltration, 2 mL PBSSPE (R-Biopharm-Rhône IAC) elution 6 mL ACNDried and reconstituted | LC-MS/MSBetasil RP-18 (150 mm × 2.1 mm, 5 µm)0.2% FA in water/0.2% FA in ACN | 0.05/0.15 | 87–92 | LOQ–6.9 (n = 107, 94%) | [48] | ||
Pseudostellariae Radix | ACN:water (8:2, v/v)1 h shakingdSPE (PSA + C18 + MgSO4) | LC-MS/MSAcquity 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, chocolate | 5 g sample, 20 mL JSM FO 970415 min shaking5 min centrifugation | LC-MS/MS | 0.01–0.02/0.05–0.15 | 94–100 | 0.2–2.2 | [50] | ||
Cocoa | 7.5 g sample, 18 mL 0.5% HAc in ACN:water (7:3, v/v), 3 g NaCl60 min shaking15 min frozen at –70°C10 min centrifugation | LC-MS/MSTitan C18 (100 mm × 2.1 mm, 1.9 μm) | - | - | 2.4–3.3 (n = 18, 11%) | [51] | ||
Carob | 1 g sample, 10 mL water, 10 mL 1% HAc in ACN10 min UAE10 min shaking, 1 g NaCl, 4 g MgSO4Dried and reconstituted | LC-MS/MSTitan C18 (100 mm × 2.1 mm, 1.9 μm) | - | - | 0.15–0.18 (n = 22, 14%) | [51] | ||
Cheese | 2.5 g sample, 5 mL 0.1% FA in ACN, 5 mL saturated MgSO430 min shaking7 min centrifugationDefatting, 4 mL heptane5 min shakingDried and reconstituted | LC-MS/MSGemini 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 | 0.01/0.04 | 100–106 | 0.08–4.99 (n = 11, 82%) | [52] | ||
Goat, camel, and cow milk | 1 mL sample, 1 mL 1% FA in ACN, 0.4 g MgSO4, 0.1 g NaCl10 min centrifugation | LC-MS/MSAcquity 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 food | 2 g sample, 10 mL JSM FO 970415 min shaking5 min centrifugation | LC-MS/MS | 0.02/0.07 | 100 | 0.02–0.50 (n = 85, 34%) | [54] | ||
Rice, peanut, maize, sorghum | 5 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 kernels | 25 g sample, 100 mL MeOH:water (8:2, v/v), 5 g NaCl3 min extractionPBS dilutionSPE (Easi-Extract Sterigmatocystin IAC) elution 1.5 mL ACNDried and reconstituted | LC-FLDODS2 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) | 1.3/4.2 | 81–87 | 9–101 (n = 30, 5%) | [56] | ||
Herbs, herbal infusions | 1 g herb sample, 5 mL water, 30 min shaking | 5 mL 1% FA in ACN, 2 g MgSO4, 1 g NaCl1 h orbital shaking15 min centrifugationdSPE (C18, Z-sep+)Dried and reconstituted | LC-MS/MSKinetex 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) | 0.5–20/2.5–40 | 73–101 | 34–147 (n = 58, 19%) | [57] | |
1 g infusion sample, 50 mL hot water, 15 min shacking | 5 min centrifugation5 mL ACN, 2 g MgSO4, 1 g NaCl5 min centrifugationDried and reconstituted | |||||||
Malt, beer | 5 g malt sample, 2 g MgSO4, 1 g NaCl, 15 mL ACN:water (75:25, v/v) | 6 min centrifugationd-SPE (MgSO4, C18)Dried and reconstituted | LC-HRMS/MSKinetex Core-Shell F5 100 A (2.6 µm)0.1% HAc + 4 mM NH4Ac in water/0.1% HAc + 4 mM NH4Ac in ACN | 5/12 | 90–97 | LOQ (n = 47, 0%) | [58] | |
5 mL beer sample, 5 mL ACN, 2 g MgSO4, 1 g NaCl | 3 min UAE5 min centrifugationdSPE (MgSO4, C18)Dried and reconstituted | |||||||
Rice bran | 20 g sample, 80 mL MeOH:water (8:2, v/v)15 min UAE5 min centrifugationDLLME (CHCl3/water)5 min centrifugationDried and reconstituted | LC-MS/MSAccucore C18 (100 mm × 2.1 mm, 2.6 μm) | 2.5/5.0 | 99 | LOQ (n = 24, 0%) | [59] | ||
Milled rice | 5 g sample, 20 mL 1% FA in ACN:water (8:2, v/v)90 min shaking | LC-MS/MSSynergi Hydro-RP (100 mm × 3 mm, 2.5 µm)1% FA and 10 mM NH4Ac in water/MeOH | 0.03/0.09 | 80 | LOQ–7 (n = 200, 74%) | [60] | ||
Dairy products | 2 g sample, 8 mL 2% FA in ACN30 min UAE5 min centrifugationSPE (Captiva EMR-lipid)Dried and reconstituted | LC-MS/MSShiseido C18 (100 mm × 2.1 mm, 3 μm)0.1% FA in water/0.1% FA in MeOH | 0.005/0.020 | 73 | LOQ (n = 76, 0%) | [61] | ||
Milling oats | 5 g sample, 20 mL 1% HAc in ACN:water (8:2, v/v)90 min shakingS-µSPE (MycoSpin 400)Dried and reconstituted | LC-MS/MSEclipse 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 | -/1 | 95 | 1–7 (n = 281, 2.3%) | [62] | ||
Garlic | 5 g sample, 20 mL 1% HAc in ACN:water (8:2, v/v)Vortex shaking | LC-MS/MSGemini C18 (150 mm × 4.6 mm, 5 μm) | 0.05/0.14 | 90 | 3–32 (n = 36, 100%) | [63] | ||
Coix seed | 5 g sample, 20 mL 1% FA in ACN:water (7:3, v/v)20 min vortex shaking5 min centrifugation | LC-HRMSCORTECS 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 | -/1 | 76–89 | 1–51 (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