Recent Advances in the Analysis of Vitamin D and Its Metabolites in Food Matrices
Abstract
:1. Introduction
2. Recent Applications of Sample Preparation
2.1. Conventional Extraction Techniques
2.2. Solid-Phase Extraction
2.3. Preparative Chromatographic Techniques
2.4. Miniaturized Techniques
3. Recent Applications of Chromatographic Techniques
3.1. Liquid Chromatography Applications
3.2. Gas Chromatography
3.3. Supercritical Fluid Chromatography
4. Conclusions and Future Remarks
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Name | Structure | Molecular Formula | Molecular Weight (g/mol) | Name | Structure | Molecular Formula | Molecular Weight (g/mol) |
---|---|---|---|---|---|---|---|
D3 | C27H44O | 384.65 | 1OH-D2 | C28H44O2 | 412.65 | ||
D2 | C28H44O | 396.66 | 24,25-(OH)2D3 | C27H44O3 | 416.64 | ||
25-OHD2 | C28H44O2 | 412.65 | 1,25-(OH)2D2 | C28H44O3 | 428.70 | ||
25-OHD3 | C27H44O2 | 400.64 | 1,25-(OH)2D3 | C27H44O3 | 416.64 | ||
1-OHD3 | C27H44O2 | 400.64 |
Analytes | Matrix (Amount) | Sample Pre-Treatment | Determination Technique | Recovery % | LOD | Comments | Reference |
---|---|---|---|---|---|---|---|
D2, D3, 25-OHD2, 3-epi-25-OHD2, 25-OHD3, 3- epi-25-OHD3 | Commercial breast milk (1 mL) | Deproteinization (40 °C, 1 h, EtOH (1 mL)); LLE 2 X (hexane/EtOAc (9/1, v/v) (2.5 mL)) | UHPSFC-(QqQ)-MS/MS | 70–107 | 0.02 μg/L a) | -APCI (+) was used as ionization source. -NH4HCOO in MeOH was used as make-up solvent. -Different columns were evaluated. -Derivatization was carried out using PTAD. -Deuterated compounds were used as ISs. -Comparison between saponification and deproteinization. -SRM was used for method validation. -SFC conditions: fluoro-phenyl column, mobile phase (MeOH/NH4HCOO/H2O/CO2), 45 °C. | [4] |
D3 | Rice (1 g) | SLE (hexane (4 mL), 5 min under N2) | HPLC-UV | - | - | -Vitamin A, E and amino acids and pesticides were also evaluated. -LC conditions: C18 column, mobile phase (ACN/H2O), 30 °C. -Occurrence: 13.8–28.6 mg/kg. | [22] |
D2, D3 | Infant formula, cereals, adult nutritionals, mixed meals (2 g) | Hydrolysis (α-amylase (50 mg): 45 °C, 30 min, papain solution (5 mL)); LLE (acidified MeOH (20 mL), BHT in isooctane (10 mL)) | UHPSFC-(QqQ)-MS/MS | 90–110 | 40 pg a) | -APCI (+) was used as ionization source. -NH4HCOO in MeOH was used as make-up solvent. -SRM was used for method validation. -Vitamin K, A and D were also evaluated. -Derivatization was carried out using PTAD. -Isotopically labelled compounds were used as surrogate ISs. -SFC conditions: 1-AA column, mobile phase (MeOH/NH4HCOO/H2O/CO2), 45 °C. | [23] |
D2, D3 | Fortified bread, bovine milk, infant formula (4 g) | Milk and infant formulas: VA-LLE (MeOH/H2O/isooctane (6.25/1.25/2.50, v/v/v), 2 min). Bread: homogeneization (EDTA (2 mL), ascorbic acid (100 mg), vortex), saponification (KOH in water, 60 °C, 30 min), LLE (MeOH/isooctane, (2/1, v/v), (30 mL)) | HPLC-(QqQ)-MS/MS | - | - | -ESI (+) was used as ionization source. -Deuterated D3 was used as surrogate IS. -Comparison of D2 and D3 supplement efficiency. -LC conditions: C18 column, mobile phase (MeOH/H2O/NH4HCOO), 40 °C. | [24] |
D3 | Finfish, shellfish (30 g) | Folch method (CHCl3/MeOH, (2/1, v/v) (450 mL)); saponification (KOH in MeOH, 30 min, refluxing): LLE (petroleum ether, (50 mL)) | HPLC-UV | - | - | -Mineral and other fat-soluble vitamins were also evaluated. -LC conditions: C18 column, mobile phase (MeOH/ACN), -. -Occurrence: 7.72–23.28 μg/kg. | [25] |
D2, D3 | Milk powder, infant formulas, nutritional formulas (1.8–21.0 g or 10 mL) | Saponification (KOH, pyrogallol, EtOH, 1 h, 70 °C); LLE (isooctane (10 mL)); washing (H2O) | UHPLC-(QqQ)-MS/MS | 96–101 | 1.2–1.6 µg/kg | -ESI (+) was used as ionization source. -Derivatization was carried out using PTAD. -AOAC Official Method 2016.05. -Deuterated standards were used as ISs. -LC conditions: C18 column, mobile phase (MeOH/H2O/FA), 40 °C. | [26] |
D3, D2, 25-OHD2, 25-OHD2, 24,25-(OH)2D2, 24,25-(OH)2D3, 1,25-(OH)2D2, 1,25-(OH)2D3 | Human, cow, mare, goat and sheep milk (4 mL) | Deproteinization (ACN (8 mL), vortex 2 min, room temperature (15 min)); LLE 2 X (hexane/DCM (1/4, v/v) (12 mL)) | HPLC-(QqQ)-MS/MS | 88–99 | 0.27–0.47 pM | -ESI (+) was used as ionization source. -Different columns were tested. -Derivatization was carried out using PTAD. -Comparison between saponification and deproteinization. -Deuterated standards were used as ISs -LC conditions: C18 column, mobile phase (MeOH/H2O/FA), -. | [39] |
D3 | Dietary supplements (-) | Dilute-and-shoot strategic (-) | HPLC-(TSQ)-MS, HPLC-(TSQ)-MS/MS, HPLC-UV | - | - | -APCI (+) was used as ionization source. -SIM and full scan modes were compared. -APCI and ESI were compared. -D2 was used as IS. -Triacylglycerols were also evaluated. -LC conditions: hydrophilic endcapping-C18 column, mobile phase (MeOH/ACN/DCM), 10 °C. | [27] |
D2, D4, pre-D2, pre-D4, tachysterol2, tachysterol4, lumisterol2, lumisterol4, ergosterol, 22,23-dihydroergosterol | Oyster mushroom (5 g) | Method 1: Saponification/hydrolysis (KOH, sodium ascorbate, NaOH, 1 h, 80 °C, refluxing); LLE (diethyl ether (50 mL); EtOH/pentane (1/5, v/v) (60 mL), pentane (50 mL and 20 mL)). Method 2: Saponification/hydrolysis (KOH, sodium ascorbate, NaOH, 20 h, 18 °C, refluxing); LLE (diethyl ether (50 mL); EtOH/pentane (1/5, v/v) (60 mL), pentane (50 mL and 20 mL)). Method 3: US-LLE X 3 (pentane (100, 100 and 50 mL), 10 min, 13 °C) | HPLC-UV, HPLC-(QqQ)-MS/MS | 97 | 0.02–0.06 mg/kg | -APCI (+) was used as ionization source. -Analysis was carried out after UV-B treatment. -D3 was used as surrogate IS. -Different extraction methods were compared. -LC conditions: hydrophilic endcapping-C18 column, mobile phase (MeOH/H2O/FA), 40 °C. | [7] |
Pre-D3, D3 | Fortified cereals, cereals-based food, milk, fruit juice, yogurt, sun flower oil, egg yolk (5–30 g) | Saponification (KOH, H2O, EtOH, 20 min, 80 °C); LLE (ciclohexane, (41 mL)) | 2D-HPLC-UV-(QqQ)-MS/MS | 96–105 | 0.5–0.8 μg/kg | -ESI (+) was used as ionization source. -Deuterated D3 was used as IS. -SRMs were used for validation. -Pre-D3, D3 were analyzed together. -LC conditions: C8 and C18 columns, mobile phase (MeOH/ACN/H2O/FA), 35 °C. | [41] |
D2, D3 | Milk, infant formula, fruit juice, vegetable beverage (20–25 g) | Saponification (KOH, EtOH, BHT, 1 h, room temperature), LLE (2× hexane (50 mL)) | HPLC-DAD | - | 0.82–1.57 ng b) | -Vitamin E was also evaluated. -C8 and C18 columns were compared. -LC conditions: C18 column, mobile phase (MeOH/ACN), -. | [28] |
D3 | Milk-based formula (0.5 g) | Dilution (H2O, 10 mL);VA-LLE (IPA (10 mL) with (NH4)2SO4); saponification (KOH, NaCl, NH3, 30 min, room temperature) | HPLC-(QqQ)-MS/MS | 93–110 | 0.84 μg/kg | -ESI (+) was used as ionization source. -SRMs were used for validation. -Comparison with official method. -LC conditions: C18 column, mobile phase (MeOH/H2O/NH4HCOO), 40 °C. | [29] |
Analytes | Matrix (Amount) | Sample Pre-Treatment | Sorbent | Elution Solvents (Volume) | Determination Technique | Recovery % | LOD | Comments | Reference |
---|---|---|---|---|---|---|---|---|---|
D2, D3 | Cereal and flour-based products (1.5 g) | Saponification (KOH, EtOH, hexane, 60 °C, 30 min); vortex, centrifugation, upper layer drying, reconstitution and filtration | C18 colum (-) | MeOH using a gradient at different flow rates | UHPLC-PDA | >70 | 0.05–0.12 mg/L | -Online SPE was carried out. -Vitamin K was also evaluated. -SRM was used for method validation. -Occurrence: 1.0–2.9 mg/kg. -LC conditions: C18 column, mobile phase (MeOH/H2O), 30 °C. | [30] |
D2, D3, 25-OHD2, 25-OHD3 | Plants, seaweeds, fruit seed (-) | Saponification (KOH, ascorbic acid in H2O, EtOH, overnight, room temperature) | Diatomaceous earth column (-) | Petroleum ether (2 × 30 mL) | HPLC-(QqQ)-MS/MS | 94–101 | 0.5 μg/kg | - ESI (+) was used as ionization source. -Deuterated compounds were used as ISs. -Derivatization was carried out using PTAD. -LC conditions: C18 column, mobile phase (MeOH/H2O), -. | [9] |
D3, 25-OHD3 | Porcine fat and liver (0.2–1 g) | Saponification (KOH, sodium ascorbate, EtOH; overnight, room temperature); LLE (20% EtOAc in heptane); drying; reconstitution (1% IPA in heptane) | Silica column (500 mg) | 6% IPA in heptane; 10% IPA in heptane | HPLC-(QqQ)-MS/MS | 72–124 | <0.1 μg/kg a) | -ESI (+) was used as ionization source. -Derivatization was carried out using PTAD. -LC conditions: C18 column, mobile phase (MeOH/H2O/FA/methyl amine), 50 °C. | [42] |
D3 | Fruit, fruit juices, dietary supplements (2 g) | SLE (MeOH); centrifugation; filtration; hydrolysis (carrez solutions) | C18 column (500 mg) | 60% MeOH in water (3 mL); MeOH (3 mL); DCM (3 mL) | HPLC-DAD | 86–95 | 5.28 mg/Lb) | -9 more vitamins were also analyzed. -Occurrence: 2.5–74 μg/kg. -LC conditions: C18 column, mobile phase (MeOH/H2O/TFA), 30 °C. | [31] |
D3 | Cod liver oil-based dietary supplements (0.2% of each capsule) | Dilution in hexane (up to 1 mL) | NH2-propyl column (200 mg) | EtOAc (1 mL) | HPLC-(QqQ)-MS/MS | - | - | -APCI (+) was used as ionization source. -Deuterated D3 was used as IS. -Occurrence: 1.31 mg/pill. -LC conditions: C18 column, mobile phase (MeOH/H2O), -. | [8] |
D3, 25-OHD3 | Pork, beef, egg, chicken, turkey, dolphinfish, salmon, tilapia (20 g) | Saponification (KOH, pyrogallol, EtOH; overnight, room temperature); LLE X 4 (petroleum ether/diethyl ether, 2/8, v/v); washing (5% KOH); drying (N2); reconstitution (0.1% IPA in ciclohexane (0.5 mL)/(DCM 0.6 mL)) | Silica colum (1000 mg) | 0.4–3.0% IPA in DCM | D3: HPLC-DAD, 25-OHD3: HPLC-(QqQ)-MS/MS | 73–88 | 0.4 µg/kg | -APCI (+) was used as ionization source. -D2 and 25-OHD2 were used as ISs. -CRM and ground pork control sample were used for method validation. -Poultry was also analyzed. -Further purification was carried out after SPE using normal phase semi-preparative HPLC. -Occurrence: D3 (1.1–9.2 μg/kg); 25OHD3 (0.9–3.6 μg/kg). -LC conditions: C18 column, mobile phase D3: (MeOH/H2O),-; 25-OHD3: (MeOH/H2O/acetic acid), -. | [10] |
Analytes | Matrix (Amount) | Sample Pre-Treatment | Column | Mobile Phase | Determination Technique | Recovery % | LOD | Comments | Reference |
---|---|---|---|---|---|---|---|---|---|
D2, D3 | Cacao, cacao-based food (-) | Saponification (KOH, -); LLE (hexane) | Silica column | - | HPLC-(QTrap)-MS/MS | - | - | -ESI (+) used as ion source. -Occurrence: 1.5–54.8 μg/kg. -Deuterated D3 and D2 were used as ISs. -Derivatization was carried out using PTAD. -LC conditions: C18 column, mobile phase (ACN/H2O/NH4HCOO/FA), -. | [32] |
D2, D3 | Yogurt, dietary supplement, margarine (-) | Homogeneization (hexane; water/EtOH (1/1, v/v)), saponification (KOH, 60 °C, 30 min); washing of hexane phase (water/EtOH (1/1, v/v)) | Silica column | 0.1% IPA in DCM | GC-(ToF)-MS | - | 50–150 pg | -EI used as ion source. -Comparison with HPLC-MS and HPLC-UV determination were carried out using different sample pre-treatments. -Online-HPLC-GC was performed reducing procedure complexity. -Deuterated D2 and D3 were used as ISs. -Determination was carried out using pyro- isomers due to the transformation reaction occuured at high temperature. | [33] |
D3 | Finfish, shellfish (5–10 g) | Saponification (KOH, EtOH, ascorbic acid, 75 °C, 30 min, refluxing); LLE (petroleum ether/diethyl ether: AOAC 992.26) | Silica column | MeOH/ACN (2/8, v/v) | HPLC-DAD; HPLC-(TSQ)-MS | - | <2.0 µg/kg a) | -APCI (+) used as ion source -D2 used as IS. -Study of the improvement of the saponification process. -SRM was used for method validation. -Occurrence: (0.5–1.8 μg/kg) -LC conditions: C18 column, mobile phase (MeOH/ACN), -. | [34] |
D3 | Fortified orange juice (30 mL) | LLE (Ethyl ether, petroleum ether, ascorbic acid) | Silica column | IPA/MTBE/ciclohexane/heptane (0.05/0.2/4.875/4.875, v/v/v/v) | HPLC-UV-(TSQ)-MS, HPLC-(IT)-MS | - | UV: 0.298 µg/kg MS: 1.175 µg/kg | -APCI (+) was used as ionization source. -Occurrence: 10.7–16.63 μg/kg. -D2 was used as IS. -LC conditions: C18 column, mobile phase (MeOH/ACN), 40 °C. | [35] |
Analytes | Matrix (Amount) | Sample Pre-Treatment | Technique | Determination Technique | Recovery % | LOD | Comments | Reference |
---|---|---|---|---|---|---|---|---|
D3 | Wheat flour, powder bread (2.0 g) | Saponification (H2O, KOH, EtOH, sodium ascorbate; -) (ultrasounds, 5 min, 25 °C); deproteinization (carrez solutions) | DLLME (dispersant: EtOH (650 μL); extractant: octanol (80 μL)) | HPLC-UV-Vis | 87–94 | 0.7 μg/kg | -LC conditions: C18 column, mobile phase (MeOH), 25 °C. | [36] |
D2, D3 | Milk (1 mL) | Dilution (phosphate buffer, 9 mL) | m-μ-dSPE (sorbent: Fe3O4@PPy (30 mg); elution solvent: ACN (1 mL)) | HPLC-UV | 72–90 | 0.02–0.05 µg/L | -Occurrence: D2: 6.5–10.2 µg/L; D3: 2.7–8.8 µg/L. -LC conditions: C18 column, mobile phase (MeOH/ACN), -. | [37] |
D2, D3 | Infant formula (50–250 g), green vegetables (0.2–2 g) | SLE (ACN, 3 mL) | DLLME (dispersant: ACN (3 mL); extractant: CCl4 (150 μL)) | HPLC-(IT)-MS | 88–103 | 3.1–4.0 μg/L | -APCI (+) was used as ionization source. -Vitamin K1, K2 and K3 were also evaluated. -CRM were used for method validation. -Different LC columns were evaluated. -DAD was also applied as detector. -LC conditions: C18 column, mobile phase (ACN/H2O/IPA), 25 °C. | [38] |
D2 | Fruit juice, milk beverage (0.1 mL) | Deproteinization (ACN, 0.9 mL) | m-μ-dSPE (sorbent: C18@Fe3O4 (30 mg); elution solvent: ACN (-)) | CLC-UV | -Other fat-soluble vitamins were also evaluated. -LC conditions: C18 column, mobile phase (ACN), -. | [39] |
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Socas-Rodríguez, B.; Sandahl, M.; Holm, C.; Turner, C. Recent Advances in the Analysis of Vitamin D and Its Metabolites in Food Matrices. Separations 2020, 7, 36. https://doi.org/10.3390/separations7020036
Socas-Rodríguez B, Sandahl M, Holm C, Turner C. Recent Advances in the Analysis of Vitamin D and Its Metabolites in Food Matrices. Separations. 2020; 7(2):36. https://doi.org/10.3390/separations7020036
Chicago/Turabian StyleSocas-Rodríguez, Bárbara, Margareta Sandahl, Cecilia Holm, and Charlotta Turner. 2020. "Recent Advances in the Analysis of Vitamin D and Its Metabolites in Food Matrices" Separations 7, no. 2: 36. https://doi.org/10.3390/separations7020036
APA StyleSocas-Rodríguez, B., Sandahl, M., Holm, C., & Turner, C. (2020). Recent Advances in the Analysis of Vitamin D and Its Metabolites in Food Matrices. Separations, 7(2), 36. https://doi.org/10.3390/separations7020036