An Overview of the Analytical Methods for the Determination of Organic Ultraviolet Filters in Cosmetic Products and Human Samples
Abstract
:1. Introduction
2. Analytical Methods for UV Filter Determination in Cosmetic Samples
2.1. Sample Preparation
2.2. Analytical Techniques
3. Analytical Methods for UV Filter Determination in Biological Samples
3.1. Sample Preparation
3.2. Analytical Techniques
3.3. Accuracy and Sensitivity
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
Abbreviations
[C6MIM][PF6]: | hexyl-3-methylimidazolium hexafluorophosphate |
2-OH-BP: | 2-hydroxybenzophenone |
3-BC: | 3-benzophenone camphor |
4-AHA: | p-aminohippuric acid |
4-AMB: | p-acetamidobenzoic acid |
4-DHB: | 4,4-dihydroxybenzophenone |
4-MBC: | 3-(4-methylbenzylidene)-camphor |
4-OCH3-AHA: | p-acetamidohippuric acid |
4-OH-BP: | 4-hydroxybenzophenone |
5cx-EPS: | 5-(((2-hydroxybenzoyl)oxy)methyl)heptanoic acid |
5-OH-EHS: | 5-hydroxy-2-ethylhexyl salicylate |
5oxo-EHS: | 2-ethyl-5-oxohexyl 2-hydroxybenzoate |
AALME: | air-assisted liquid–liquid microextraction |
Ac: | Acetone |
APCI: | atmosphere pressure chemical ionisation |
API: | atmosphere pressure ionisation |
APPI: | atmosphere pressure photoionisation |
ASE: | accelerated solvent extraction |
BMDBM: | butyl methoxydibenzoylmethane/avobenzene |
BAµE: | bar adsorptive microextraction |
BC: | benzyl cinnamate |
BDM: | butyl methoxydibenzoylmethane |
EMT: | bis-ethylhexyloxyphenol methoxyphenyl triazine |
BP: | Benzophenone |
BP-1: | 2,4-dihydroxybenzophenone |
BP-10: | 2-hydroxy-4-methoxy-4′-methylbenzophenone |
BP-12: | (2-hydroxy-4-octoxy-phenyl)-phenyl-methanone |
BP-2: | 2,2′,4,4′-tetrahydroxybenzophenone |
BP-3: | 2-hydroxy-4-methoxybenzophenone |
BP-4: | 2-hydroxy-4-methoxybenzophenone-5-sulphonic acid |
BP-6: | 2,2′-dihydroxy-4,4′-dimethoxybenzophenone |
BP-7: | 5-chloro-2- hydroxybenzophenone |
BP-8: | 2,2′-dihydroxy-4-methoxybenzophenone |
BP-OH: | Benzhydrol |
BS: | benzyl salicate |
BZT: | Benzotriazole |
C18: | Octadecyl |
CDAA: | 2-cyano-3,3-diphenyl acrylic acid |
CPE: | cloud point extraction |
DAD: | diode-array detection |
DART-MS: | direct-analysis-in-real-time mass spectrometry |
DBT: | diethylhexyl butamino triazone |
DCM: | Dichloromethane |
DEA: | Diethylaminopropyl |
DHHB: | diethyloamino hydroxybenzoyl hexyl benzoate |
DLLME: | dispersive liquid–liquid microextraction |
DMF: | n,n-dimethylformamide |
DTS: | drometrizole trisiloxane |
DS: | Densitometry |
d-SPE: | dispersive solid-phase extraction |
EA: | ethyl acetate |
ECD: | electron captur detector |
EDP: | 2-ethylhexyl 4-(n,n-dimethylamino)benzoate |
EHC: | ethylhexyl cinnamate |
EHS: | 2-ethylhexyl salicylate |
EI: | electron impact |
EMC: | ethylhexyl methoxycinnamate |
EHS: | ethylhexyl salicylate |
ESI: | electrospray ionisation |
ET: | ethylhexyl triazone |
EtOH: | Ethanol |
EtPABA: | ethyl p-aminobenzoic acid |
FL: | Fluorescence |
FPSE: | fabric phase sorptive extraction |
GC: | gas chromatography |
HFLPME: | hollow-fiber liquid-phase microextraction |
HPLC: | high-performance liquid chromatography |
HS: | salicylic acid 3,3,5-trimethcyclohexyl ester |
HTLC: | high-temperature liquid chromatographic |
IMC: | isoamyl p-methoxycinnamate |
LC: | liquid chromatography |
LD: | liquid desorption |
LLE: | liquid–liquid extraction |
LOD: | limit of detection |
log Ko/w: | log octanol/water partition coefficient |
LOQ: | limit of quantification |
LTP-MS: | low temperature plasma ionisation mass spectrometry |
MA: | menthyl anthranilate |
MAE: | microwave-assisted extraction |
MBBT: | methylene bis-benzotriazolyl tetramethyl butyl phenol |
MBC: | 4-methylbenzylidene camphor |
MBP: | methylene bis-benzotriazoyl tetramethylbutylphenol |
MeCN: | Acetonitrile |
MEKC: | micellar electrokinetic capillary chromatography |
MeOH: | Methanol |
MEPS: | microextraction by packed sorbent |
MMLLE: | microporous membrane liquid–liquid extraction |
MS/MS: | tandem mass spectrometry |
MS: | mass spectrometry |
MSPD: | matrix solid phase dispersion |
MTBE: | methyl tert-butyl ether |
NaCl: | sodium chloride |
OC: | 4-methylbenzilidene camphor/octocrylane |
ODP: | octyl dimethyl PABA |
ODPABA: | 2-ethylhexyl 4-(dimethylamino)benzoate |
OMC: | 2-ethylhexyl p-methoxycinnamate |
OS: | 2-ethylhexylsalicylate |
PABA: | p-aminobenzoic acid |
PMDSA: | 2-phenylbenzimidazole-5-sulphonic acid |
PDA: | photodiode-array detection |
PEG-25 PABA: | polyethylene glycol 25 paminobenzoic acid |
PHBA: | 4-hydroxy benzoic acid |
PLE: | pressurized liquid extraction |
pKa | acid dissociation constant |
PSA: | primary-secondary amine |
QuEChERSExtraction: | Quick, Easy, Cheap, Effective, Rugged, and Safe Extraction |
R: | Recovery |
RSD: | relative standard deviation |
SALLE: | salt-assisted liquid–liquid extraction |
SBSE: | stir bar sorptive extraction |
SDME: | single-drop microextraction |
SFC: | supercritical fluid chromatography |
SIA: | sequential injection analysis |
SI SPE: | sequential injection solid-phase extraction |
SLE: | solid–liquid extraction |
SPE: | solid-phase extraction |
SPME: | solid-phase microextraction |
SWV: | squarewave voltammetry |
TBHPBT: | 2-(5-tert-butyl-2-hydroxyphenyl)benzotriazole |
TCM: | trichloroamine |
TFA: | trifluoroacetic acid |
TFC: | turbulent flow chromatography |
THB: | 2,3,4-trihydroxybenzophenone |
TLC: | thin-layer chromatography |
UAE: | ultrasound-assisted extraction |
UHPLC: | ultra-high-performance liquid chromatography |
UHPSFC: | ultra-high performance supercritical fluid chromatography |
UPLC: | ultra-performance liquid chromatography |
USAD-SPE: | ultrasound-assisted dispersive solid phase extraction |
UV/Vis: | ultraviolet/visible spectrometry |
VADLLME: | vortex-assisted dispersive liquid–liquid microextraction |
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Chemical Name | INCI Name a | Abbreviation | CAS Number | Structure | Max. Concentration (%) | Log Ko/w a | pKa a | Solubility (g/L) a,b |
---|---|---|---|---|---|---|---|---|
Benzophenone derivatives | ||||||||
2-Hydroxy-4-methoxybenophenone/Oxybenzone | Benzophenone-3 | BP-3 | 131-57-7 | 10 | 3.79 | 7.56 | 0.21 | |
2-Hydroxy-4-benzophenone-5-sulfonic acid and its sodium salt/Sulisobenzoate | Benzophenone-4, Benzophenone-5 | BP-4, BP-5 | 4065-45-6/6628-37-1 | 5 (as acid) | 0.37 | −0.70 | 0.65 | |
Benzoic acid, 2-[4-(diethylamino)-2-hydroxybenzoyl]-hexylester | Diethylamino Hydroxybenzoyl Hexyl Benzoate | DHHB | 302776-68-7 | 10 | 6.54 | 7.29 | 9.5 · 10−4 | |
p-Aminobenzoic acid derivatives | ||||||||
Ethoxylated ethyl-4-aminobenzoate | PEG-25 PABA | PEG-25 PABA | 116242-27-4 | 10 | −0.66 | - | - | |
2-Ethylhexyl-4-(dimethylamino)benzoate/Padimate O (USAN:BAN) | Ethylhexyl Dimethyl PABA | OD-PABA | 21245-02-3 | 8 | 6.15 | 2.39 | 0.0021 | |
Salicylates | ||||||||
Benzoic acid, 2-hydroxy-3,3,5-trimethylcyclohexyl ester/Homosalate | Homosalate | HS | 118-56-9 | 10 | 6.16 | 8.09 | 0.02 | |
2-Ethylhexyl salicylate/Octisalate | Ethylhexyl Salicylate | EHS | 118-60-5 | 5 | 5.97 | 8.13 | 0.028 | |
Cinnamates | ||||||||
2-Ethylhexyl-4-methoxycinnamate/Octinoxate | Ethylhexyl Methoxycinnamate | OMC | 5466-77-3 | 10 | 5.8 | - | 0.15 | |
Isopentyl-4-methoxycinnamate/Amiloxate | Isoamyl p-Methoxycinnamate | IMC | 71617-10-2 | 10 | 4.33 | - | 0.06 | |
Benzimidazole derivatives | ||||||||
2-Phenylbenzimidazole-5-sulfonic acid and its potassium, sodium, and triethanolamine salts/Ensulizole | Phenylbenzimidazole Sulfonic Acid | PMDSA | 27503-81-7 | 8 (as acid) | −0.16 | −0.87 | 0.26 | |
Sodium salt of 2,2′-bis(1,4-phenylene)-1H-benzimidazole-4,6-disulfonic acid)/Bisdisulizole disodium (USAN) | Disodium Phenyl Dibenzimidazole Tetrasulfonate | DPDT | 180898-37-7 | 10 (as acid) | −6.79 | −0.27 | 0.5 | |
Benzotriazole derivatives | ||||||||
Phenol,2-(2H-benzotriazol-2-yl)-4-methyl-6-(2-methyl-3-(1,3,3,3-tetramethyl-1-(trimethylsilyl)oxy)-disiloxanyl)propyl) | Drometrizole Trisiloxane | DTS | 155633-54-8 | 15 | 10.38 | 1.2 | 5.5 · 10−10 | |
2,2′-Methylene-bis(6-(2H-benzotriazol-2-yl)-4-(1,1,3,3-tetramethyl-butyl)phenol)/Bisoctrizole | Methylene Bis-Benzotriazolyl Tetramethylbutylphenol | MBP | 103597-45-1 | 10 | 12.46 | 7.56 | 3 · 10−8 | |
Camphor derivatives | ||||||||
N,N,N-Trimethyl-4-(2-oxoborn-3-ylidenemethyl)anilinium methyl sulfate | Camphor Benzalkonium Methosulfate | CBM | 52793-97-2 | 6 | 0.28 | - | 0.007 | |
3,3′-(1,4-Phenylenedimethylene) bis(7,7-dimethyl-2-oxobicyclo-[2,2,1]hept-1-yl-methanesu fonic acid) and its salts/Ecamsule | Terephthalylidene Dicamphor Sulfonic Acid | PDSA | 92761-26-7, 90457-82-2 | 10 (as acid) | 3.83 | −1.05 | 0.014 | |
Alpha-(2-Oxoborn-3-ylidene)-toluene-4-sulphonic acid and its salts | Benzylidene Camphor Sulfonic Acid | BCSA | 56039-58-8 | 6 (as acid) | 2.22 | −0.7 | 0.038 | |
3-(4-Methylbenzylidene)-d1 camphor/Enzacamene | 4-Methylbenzylidene Camphor | 4-MBC | 38102-62-4/ 36861-47-9 | 4 | 4.95 | - | 0.0051 | |
Polymer of N-{(2 and 4)-[(2-oxoborn-3-ylidene)methyl-]benzyl} acrylamide | Polyacrylamidomethyl Benzylidene Camphor | PBC | 113783-61-2 | 6 | - | - | - | |
Triazine derivatives | ||||||||
Benzoic acid, 4,4-((6-((4-(((1,1-dimethylethyl)amino)carbonyl)phenyl)amino)-1,3,5-triazine-2,4-diyl)diimino)bis-, bis (2-ethylhexyl) ester/ Iscotrizinol (USAN) | Diethylhexyl Butamido Triazone | DBT | 154702-15-5 | 10 | 14.03 | 3.04 | 4.6 10−7 | |
3,3′-(1,4-Phenylene)bis(5,6-diphenyl-1,2,4-triazine) | Phenylene Bis-Diphenyl triazine | - | 55514-22-2 | 5 | - | - | - | |
2,4,6-Trianilino-(p-carbo-2′-ethylhexyl-1′-oxy)-1,3,5-triazine | Ethylhexyl Triazone | ET | 88122-99-0 | 5 | 17.05 | 3.17 | - | |
2,2′-(6-(4-Methoxyphenyl)-1,3,5-triazine-2,4-diyl)bis(5-((2-ethylhexyl)oxy)phenol)/Bemotrizinol | Bis-Ethylhexyloxyphenol Methoxyphenyl Triazine | EMT | 187393-00-6 | 10 | 8.03 | 6.37 | 4.9 ·10−8 | |
Others | ||||||||
1-(4-tert-Butylphenyl)-3-(4-methoxyphenyl)propane-1,3-dione/Avobenzene | Butyl Methoxydibenzoyl-methane | BMDBM | 70356-09-1 | 5 | 4.51 | 9.74 | 0.037 | |
2-Cyano-3,3-diphenyl acrylic acid, 2-ethylhexyl ester/Octocrilene | Octocrylene | OC | 6197-30-4 | 10 (as acid) | 6.88 | - | 2 · 10−4 | |
Dimethicodiethylbenzalmalonate | Polysilicone-15 | BMP | 207574-74-1 | 10 | - | - | - | |
2-ethoxyethyl(2Z)-2-cyano-2-[3-(3-methoxy-propylamino) cyclohex-2-en-1-ylidene]acetate | Methoxypropylamino Cyclohexenylidene Ethoxyethylcyanoacetate | - | 1419401-88-9 | 3 | - | - | - |
UV Filters | Matrix | Analytical Technique | Analytical Performance a | Ref. |
---|---|---|---|---|
BP-3, IMC, MBC, DHHB, OC, EDP, BDM, EMC, EHS, HS, DBT, ET, DTS, MBP, EMT | Sunscreens, facial creams, lip balms, aftershave creams | LC-UV/Vis; type of column: C18; column temperature: 60 °C; mobile phase: ethanol/formic acid (aq) mobile phase modifier: hydroxypropyl-β-cyclodextrin (HP-β-CD) | LOD: 0.02–0.22 µg mL−1 LOQ: 0.07–0.74 µg mL−1 R: 98–104% RSD: 0.9–7.1% | [10] |
PMDSA, BP-4, BP-3, MBC, DHHB, EMC, OC, MBP, EMT, ET, BDM | Emulsion, oil | HPLC-UV/Vis; type of column: C8 or C18 or C16; column temp.: 35 °C; mobile phase: gradient acetonitrile/perchloric acid (aq) or isocratic methanol/acetonitrile or isocratic methanol/perchloric acid | LOD: 0.1–1.2 µg mL−1 LOQ: no data R: 93.9–103.4% RSD: 0.2–1% | [13] |
BP-1, BP-2, BP-3 | Emulsion | MEKC-UV/Vis; type of capillary: a 51 cm uncoated fused-silica; surfactant: sodium tetraborate containing sodium dodecyl sulfate | 10−8–3.9010−7 mol/L LOQ: no data R: 89.5–102.5% RSD: 1.14–8.09% | [14] |
PMDSA, PABA, BP-4, BP-3, IMC, MBC, OC, EMC, HS, EHS, MBBT | Creams, lotions, foundation, loose powder, lipstick | HPLC-UV/Vis; type of column: C18; column temp.: 30 °C; mobile phase: gradient methanol/tetrahydrofuran/perchloric acid (aq) | LOD: 200–500 ng mL−1 LOQ: 700–6700 ng mL−1 R: 98.5–102.2% RSD: 0.51–1.72% | [15] |
PMDSA, BP-3, IMC, DHHB, OC, EMC, EHS, BDM, DBT, ET, MBP, EMT | Emulsion, sticks, powder | HPLC-UV/Vis; type of column: C18; column temp.: 40 °C; mobile phase: gradient ethanol/ 1% phosphoric acid (aq) | LOD: 0.04–1.66 µg mL−1 LOQ: 0.13–5.52 µg mL−1 R: 97–101.4% RSD: 0.38–2.42% | [16] |
HS, EDP, EHC, EHS, MBC, BDM, BP-3, OC, PHBA, BC | Cream, milk, lotion, oil, lipstick | DART-MS (ESI+) | LOD: 2.5–460 µg g−1 LOQ: no data R: 71–120% RSD: 4–30% | [17] |
EMC, IMC, EHS, MBC, BP-3, EDP, OC, BDM | Cream, lotion, spray | HPLC-UV/Vis; type of column: C18; column temp.: 30 °C; mobile phase: gradient acetonitrile/acetic acid (aq) | LOD: 0.03–1.5 mg L−1 LOQ: 0.08–4.6 mg L−1 R: 98–102% RSD: 0.97–6.1% | [18] |
BP-4, BP-3, ODP, OMC, EHS | Cream, lotion, lipstick, foundation | HPLC-UV/Vis; type of column: C18; column temp.: 40 °C; mobile phase: gradient methanol/pure water (80:20; v/v) | LOD: 1–100 ng L−1 LOQ: 4–340 ng L−1 R: 98–102% RSD: 4–5.2% | [19] |
OC | Emulsion | SWV/mercury electrode; a mixture of Britton–Robinson (BR) buffer and ethanol (7:3; v/v) as the supporting electrolyte | LOD: no data LOQ: no data R: 9.7–106% RSD: 1–3.42% | [20] |
EMC, BP-3, EHS, OC | Emulsion | LC-UV/Vis; type of column: C18; mobile phase: methanol/water (85:15; v/v) | LOD: no data LOQ: no data R: 99.67–101% RSD: 0.044–1.5% | [21] |
BDM, BP-3, EMC | Cream | HPTLC-DS.; type of column: C18 or silica gel; mobile phase: acetonitrile/water (18:2) or cyclohexane/diethyl ether/n-hexane/acetone (14:2:1:2) | LOD: no data LOQ: no data R: 92.7–102.4% RSD: no data | [22] |
PABA, PMDSA, BP-3, MBC, BP-4, OC, EDP, EMC, BDM, HS, EHS, DBT, ET, DTS | Cream | HPLC-UV/Vis; type of column: C18; mobile phase: gradient ethanol/phosphate buffer | LOD: 0.01–1.99 mg L−1 LOQ: 0.02–6.02 mg L−1 R: 90.91–109.98% RSD: 0.16–12.69% | [23] |
BP-3, BP-4 | Shampoo, gel, perfume, cream | MEKC-UV/Vis; type of capillary: a 64.5 cm uncoated fused-silica; surfactant: sodium dodecyl sulphate | LOD: 0.91–2.26 µg mL−1 LOQ: 2.72–6.79 µg mL−1 R: 90.4–107.4% RSD: 5.7–12% | [24] |
BP-1, BP-2, BP-3, BP-4, BP-6, BP-8, OC, EMC, PABA | Lotion, cream | MEKC-UV/Vis; type of capillary: a 30.2 cm uncoated fused-silica; surfactant: sodium dodecyl sulfate/γ-cyclodextrin | LOD: no data LOQ: no data R: 95.08–104.57% RSD: no data | [25] |
PABA, BP-3, IMC, MBC, OC, EDP, EMC, BDM, EHS, HS | Cream | HPLC-UV/Vis; type of column: C18; column temp.: 35 °C; mobile phase: isocratic ethanol/acetic acid (aq) (70:30; v/v) | LOD: 0.1–2 µg mL−1 LOQ: 0.5–5µg mL−1 R: no data RSD: no data | [26] |
BP, BP-3, BP-1, HBP | Cream | MEKC-UV/Vis; type of capillary: a 60 cm uncoated fused-silica; surfactant: sodium dodecyl sulfate | LOD: 3.9–6.7 ng mL−1 LOQ: 13–22.3 ng mL−1 R: 80.2–117.7% RSD: no data | [27] |
BP-3, EMC, OC, EHS, MBC, EDP | Cream, lipstick, blemish balm cream | LTP-MS | LOD: no data LOQ: no data R: no data RSD: 0.8–28.6% | [28] |
PMDSA, BP-2, BP-1, BP-8, BP, BP-6, BP-3, EHS, BP-10, HS, IMC, MBC, DHHB, BDM, BP-12 | Lotion, cream, lipstick | HPLC-MS/MS (ESI); type of column: C18; column temp.: 30 °C; mobile phase: gradient methanol/0.1% ammonium hydroxide (aq) | LOD: 2–20 mg kg−1 LOQ: 5–50 mg kg−1 R: 86.9–103.5% RSD: 1–6.8% | [29] |
EHS, EMC, BP-3, OC, EMT, BDM, DHHB, ET, DBT | Cream | UHPSFC-PDA; type of column: Torus 2-PIC; column temp.: 40 °C; mobile phase: gradient CO2/methanol/water/ammonium acetate | LOD: 0.2–1.7 mg kg−1 LOQ: 1–10.8 mg kg−1 R: 97.5–103.2% RSD: 0.7–1.6% | [30] |
BP-1, BP-2, BP-3, BP-8, HBP | Toothpaste, shampoo, face cleansers, sunscreens, body lotions, gels, hair gels,lotions, mask, hand sanitizer | HPLC-MS/MS (ESI-); type of column: C18; column temp.: 40 °C; mobile phase: gradient methanol/acetonitrile/water | LOD: 0.002–0.197 ng mL−1 LOQ: 0.001–0.059 ng mL−1 R: 61.9–116% RSD: no data | [31] |
BP-1 | Nail product | GC-MS/MS (EI+); type of column: ZB-SemiVolatiles; oven temp.: 40 °C/2 min—5 °C/1 min to 65 °C—50 °C/1 min to 300 °C/5 min | LOD: 18.3–2370 µg g−1 LOQ: no data R: 101–105% RSD: 0.69–1.13% | [32] |
BDM, EMT, OMC, OC, ET | Lotion | HPLC-UV/Vis; type of column: C18; mobile phase: acetonitrile/0.25% formic acid (aq) | LOD: 15 ng mL−1 LOQ: no data R: 88.1–104.7% RSD: 0.8–5.4% | [33] |
BDM | Emulsion | LC-UV/Vis; type of column: C18; column temp.: 42 °C; mobile phase: acetonitrile/0.5% phosphoric acid (aq) | LOD: 0.05796 µg mL−1 LOQ: 0.19322 µg mL−1 R: no data RSD: 0.46–2.83% | [34] |
EMC, MBC, BP-1, BP-2, BP-6, BP-4, OC, PABA, EDP, EHS, HS, IMC, BP-3, BP-8, BS, MA | Cream, nail polish, lipstick, hair gel | GC-MS/MS (EI+); type of column: SLB-5 ms; oven temp.: 100 °C/1 min—25 °C/1 min—290 °C/5 min | LOD: 0.0027–0.56 µg g−1 LOQ: 0.009–1.9 µg g−1 R: 37.4–110.5% RSD: 3.9–9.1% | [35] |
ET | Cream, lotion | TLC-DS.; type of layer: silica gel; mobile phase: cyclohexanediethyl ether (1:1) | LOD: 0.03 μg spot−1 LOQ: 0.1 μg spot−1 R: 95–105% RSD: 4.5–5% | [36] |
PMDSA, BDM, OC, EHS | Cream | HTLC; type of column: C18; column temp.: 150–200 °C; mobile phase: isocratic methanol/water | LOD: no data LOQ: no data R: 90.3–113.2% RSD: 2.8–5% | [37] |
EMC, MBC, BP-1, BP-2, BP-6, BDM, BP-4, PMDSA, MA, OC, EDP, IMC, BP-3, BP-8, | Lipsticks, hair gel, cream, nail polish | HPLC-MS/MS; type of column: C18; oven temp.: 30 °C; mobile phase: gradient methanol/0.1% formic acid/ammonia (aq) | LOD: 0.00039–0.031 µg g−1 LOQ: 0.0013–0.1 µg g−1 R: 81.7–102% RSD: 4.5–13% | [38] |
BDM, BP-3, EMC, EMT | Emulsion | HPLC-UV/Vis; type of column: C18; column temp.: 25 °C; mobile phase: gradient tetrahydfofuran/acetonitrile/acetic acid (aq) | LOD: no data LOQ: no data R: 99.2–104.8% RSD: no data | [40] |
BP-4 | Shampoo | TLC-UV/Vis; type of layer: silica gel 60 plates; mobile phase: acetate/ethanol/water/phosphate buffer (15:7:5:1; v/v/v/v) | LOD: 0.03 μg spot−1 LOQ: 0.1 μg spot−1 R: 100–103% RSD: 0.58–1.99% | [41] |
EHS, EMC, BP-3, OC, BDM, DHHB, ET, DBT | Cream | SFC-UV/Vis; type of column: 2-ethyl pyridine; column temp.: 30 °C; mobile phase: gradient CO2/methanol/ethanol (97:1.5:1.5) | LOD: no data LOQ: no data R: no data RSD: 0.6–2% | [42] |
UV Filters | Extraction Technique | Analytical Technique | Analytical Performance | Comments | Ref. |
---|---|---|---|---|---|
BP-3 | SPE (C8) | HPLC-UV/Vis; type of column: C18; mobile phase: isocratic methanol/water (70:30) | No data | Total content | [44] |
BP-3 | SPE (Bond Elut Certify LRC) | UPLC-MS/MS (ESI-); type of column: Kinetex Phenyl-Hexyl; column temp.: 35 °C; mobile phase: water/acetonitrile/acetic acid (aq) | LOD: 0.3 ng mL−1 LOQ: 0.61–200 ng mL−1 R: 75.8–80.3% RSD: 0.3–8% | Total and free forms content | [46] |
BP-3 | Online SPE (RP18) | HPLC-MS/MS (APCI−); type of column: RP18; mobile phase: gradient methanol/water | LOD: 0.3–0.5 ng mL−1 LOQ: no data R: 97–105% RSD: 1.7–20% | Total and forms content | [47,48,49] |
BP-3 | SPE (C18) | HPLC-MS (APCI); type of column: C18-PFP; mobile phase: methanol/water | LOD: 0.2 ng mL−1 LOQ: no data R: 96% RSD: 9.03–11.7% | Total content | [50] |
BP-1, BP-2, BP-8, 4-OH-BP | LLE (solvent: ethyl acetate) | HPLC-MS/MS (ESI+/ ESI−); type of column: C18; mobile phase: methanol/water (90:10; v/v) | LOD: no data LOQ: 0.7–2.0 ng mL−1 R: 84–112% RSD: no data | Total content | [51] |
BP-3 | SDME (acceptor phase:[C6MIM][PF6]; 25 min; 900 rpm) | LC-UV; type of column: RP18; mobile phase: ethanol/1% acetic acid aq (60:40; v/v) | LOD: 1.3 ng mL−1 LOQ: no data R: no data RSD: 6% | Free forms | [52] |
BP, BP-OH, 2-OH-BP, BP-3, BP-10 | SBSE (PDMS; 60 min; 500 rpm) | GC-MS; type of column: DB-5 ms; oven temp.: 40 °C/1 min—5 °C/1 min to 190 °C—15 °C/1 min to 280 °C/3 min | LOD: 0.05–0.1 ng mL−1 LOQ: 0.2–0.5 ng mL−1 R: 98.7–101.7% RSD: 1.5–4.8% | Free forms | [53] |
BP, BP-OH, 2-OH-BP, BP-3, BP-10 | HFLPME (toluene; 15 min; 500 rpm) | GC-MS (EI); type of column: DB-5 ms; oven temp.: 40 °C/ 1 min—5 °C/ 1 min to 190 °C—15 °C/1 min to 280 °C/ 4 min | LOD: 5–10 pg mL−1 LOQ: 20–50 pg mL−1 R: 89.3–100.2% RSD: 2.5–9.3% | Total content | [54] |
BP-1, BP-3, BP-8, BP-2, 4-OH-BP | LLE (solvent; 50% MTBE/ethyl acetate) | HPLC-MS/MS (ESI−); type of column: C18; mobile phase: gradient methanol/water | LOD: 0.08–0.28 mg mL−1 LOQ: 0.28–0.9 mg mL−1 R: 85.2–99.6% RSD: 2.8–4.5% | Total content | [55] |
BP-1, BP-3, BP-8, THB | SPE (C18) | LC-MS/MS (ESI+); type of column: Mediterranean SEA 18; mobile phase: gradient methanol/water/0.1% formic acid aq | LOD: 1 ng mL−1 LOQ: 2–4 ng mL−1 R: 84–111% RSD: no data | Total content | [56] |
BP-1, BP-2, BP-3, BP-8, 4-OH-BP | LLE (solvent; 50% MTBE/ethyl acetate) | HPLC-MS/MS (ESI); type of column: C18; mobile phase: gradient methanol/water | LOD: 0.013–0.28 ng mL−1 LOQ: no data R: 85.2–99.6% RSD: 1.4–4.5% | Total content | [57] |
BP-1, BP-2, BP-3, BP-7, 4-OH-BP, 4-MBP, 4-MBC, 3-BC | LLE | On-line TurboFlow-LC–MS/MS; type of column: TurboFlow Cyclone P and Hypersil Gold aQ | LOD: 0.2–1.0 ng mL−1 LOQ: no data R: 77.1–108% RSD: 5.7–15.1% | Total and free form content | [58] |
EDP | Automated SPE (C18 HD) | LC-MS/MS (ESI+); type of column: Mediterranean SEA C18; mobile phase: gradient methanol/ acetonitryle/water/0.2% formic acid | LOD: 0.3–1.1 ng mL−1 LOQ: 0.9–3.5 ng mL−1 R: 91–107% RSD: no data | Total and free forms content | [59] |
BP-3, OMC, OS, HS | LLE (solvent: acetonitrile) | HPLC-DAD; type of column: C18; mobile phase: gradient methanol/water (75:25; v/v) | LOD: 0.03–0.2 µg mL−1 LOQ: 0.1–0.4 µg mL−1 R: 86.8–92.2% RSD: 3.0–4.4% | Total content | [60] |
BP-1, BP-2, BP-3, BP-8, 4-OH-BP | DLLME (disperser solvent: acetone; extraction solvent: trichloromethane) | UHPLC-MS/MS | LOD: 0.1–0.2 ng mL−1 LOQ: 0.3–0.6 ng mL−1 R: 88–104% RSD: 0.5–22.5% | Total and free forms content | [61] |
BP-3, 4-MBC, HS, OC | ASE & SPE | GC-MS/MS | LOD: 0.47–0.59 pg mL−1 LOQ: no data R: 70.5–110.7% RSD: <5.04% | Total and free forms content | [62] |
BMDBM, CDAA, EHS, 5-OH-EHS, OC | LLE (solvent: actonitrile) | LC-LC-MS/MS (ESI); type of column: RP-18 ADS; | LOD: 0.1–1.5 µg L−1 LOQ: 0.2–4.1 µg L−1 R: 94.2–113.6% RSD: 2.6–16.5% | Total content | [63] |
5OH-EHS, 5oxo-EHS, 5cx-EPS | Online SPE (TurboFlow Phenyl) | HPLC-MS/MS (ESI); type of column: C18; mobile phase: gradient acetonitryle/water/0.05% acetic acid | LOD: no data LOQ: 0.01–0.15 µg L−1 R: 96–106% RSD: 1.2–2.4% | Total and free forms content | [64] |
BP-3 | Online SPE (RP18) | HPLC-MS/MS (ESI); type of column: XDB-C18; mobile phase: gradient methanol/water | LOD: 0.16 µg L−1 LOQ: no data R: 101% RSD: 5% | Total and free forms content | [65] |
BP-1, BP-2, BP-3, BP-8, 4-OH-BP | LLE (solvent: ethyl tert-butyl ether/ethyl acetate (5:1; v:v)) | UHPLC-TQMS (ESI−); type of column: C18; column temp.: 30 °C; mobile phase: water/acetonitrile | LOD: 0.01–0.2 ng mL−1 LOQ: no data R: 90.7–110.1% RSD: 6.9–14.2% | Total and free forms content | [66] |
BP-1, BP-2, BP-3, BP-8, 4-OH-BP | VADLLME (disperser solvent: 2-propanol; extraction solvent: dichloromethane) | LC-MS/MS; type of column: C18; column temp.: 23 °C; mobile phase: water/methanol | LOD: 0.02–0.03 ng mL−1 LOQ: 0.05–0.4 ng mL−1 R: no data RSD: 1.2–12% | Total content | [67] |
BP-1, BP-2, BP-3, BP-8, 4-OH-BP | AALLME (extraction solvent: 1,2-dichloroethane) | LC-MS/MS (ESI); type of column: C18; column temp.: 40 °C; mobile phase: water/methanol | LOD: 0.02–0.06 ng mL−1 LOQ: 0.05–0.20 ng mL−1 R: no data RSD: <15% | Total content | [68] |
PABA, 4-AHA, 4-AMB, 4-OCH3-AHA | LLE & SPE (solvent: ethyl acetate; C18) | HPLC-ECD; type of column: C18; mobile phase: methanol/phosphate buffer (pH 5.5) (20:80; v/v) | LOD: no data LOQ: 0.04–0.18 ng mL−1 R: 96–99% RSD: 0.2–3.8% | Total content | [69] |
BP-1, BP-3 | SPE (C8) | HPLC-UV; type of column: C18; mobile phase: acetonitryle/water | LOD: 2–40 ng mL−1 LOQ: no data R: no data RSD: 6.6–13% | Total and free form content | [70] |
PMDSA | Online SPE | SIA-FL | LOD: 12 ng mL−1 LOQ: no data R: no data RSD: 2–13% | Free forms | [71] |
PEG-25 PABA | SPE (C18) | LC-FL; mobile phase: dimethylfuran | LOD: 2.6 ng mL−1 LOQ: no data R: 91–100% RSD: 3–10% | Total content | [72] |
BP-4, 4-DHB, BP-2, BP-1, BP-8, BZ | FPSE | HPLC-PDA; type of column: C18; mobile phase: methanol/phosphate buffer (pH 3) (45:55; v/v) | LOD: 0.03 µg mL−1 LOQ: 0.1 µg mL−1 R: no data RSD: 2.3–14.4% | Total content | [73] |
EDP | In-vial MMLLE (hydrophobic PTFE membranes) | GC-MS; type of column: SPB-5; oven temp.: 60 °C/1.5 min—30 °C/1 min to 275 °C/20 min | LOD: no data LOQ: 0.11 µg L−1 R: no data RSD: 7.4% | Total content | [74] |
BP-3, BP-4 | SI SPE (C18 and diethylaminopropyl) | LC/UV; type of column: RP18; mobile phase: ethanol/acetate buffer/1% acetic acid | LOD: 30–60 ng mL−1 LOQ: no data R: no data RSD: 6–13% | Free forms | [75] |
BP-1, BP-2, BP-8, 4-OH-BP | MEPS (C18) | LC-MS/MS; mobile phase: water/methanol | LOD: 0.005–0.03 ng mL−1 LOQ: 0.02–0.10 ng mL−1 R: 18–118% RSD: 1–16% | Total and free forms content | [78] |
BP-1, BP-3, BP-8 | SPME (Carbowax/DVB) | GC-MS; type of column: DB5-MS; Oven temp.: 50 °C/0.1 min—30 °C/1 min to 150 °C—18 °C/1 min to 250 °C/12 min | LOD: 5–10 ng mL−1 LOQ: no data R: no data RSD: 5–8% | Total content | [79] |
BP, BP-1, BP-3, 4-OH-BP | BAµE | HPLC–DAD; type of column: Sea-18; mobile phase: methanol/water (75:25; v/v) | LOD(P2): <1.0 µg L−1 LOQ(P2): <0.3 µg L−1 LOD(AC4): <1.3 µg L−1 LOQ(AC4): <0.4 µg L−1 | Total content | [76] |
OMC, BP-3, OC, OS, HS | DLLME (disperser solvent: carbon tetrachloride; extraction solvent: acetonitrile) | HPLC-DAD; type of column: C18; mobile phase: isocratic water/methanol/acetonitrile (8:42:50; v/v/v) | LOD: no data LOQ: 3–45 ng mL−1 R: 86.9–97.3% RSD: 0.1–6.4% | Total content | [77] |
BP-1, BP-2, BP-3, BP-8, 4-OH-BP | Microextraction using a monolithic stirring extraction unit (150 min; 1100 rpm) | UPLC-DAD; mobile phase: acetonitrile/water | LOD: 1–10 µg L−1 LOQ: 5–20 µg L−1 R: 71–114 % RSD: 5.6–9.1% | Total content | [80] |
UV Filters | Matrix | Extraction Technique | Analytical Technique | Analytical Performance | Comments | Ref. |
---|---|---|---|---|---|---|
BP-3, BP-1, BP-8 | Serum | DLLME (disperser solvent: acetone: extraction solvent: chloroform) | LC-MS/MS (ESI+); type of column: C18; mobile phase: gradient methanol/water/0.1% formic acid | LOD: 7–8 µg L−1 LOQ: 22–28 µg L−1 R: 77–104% RSD: 8–9% | Total content | [45] |
BP-3, OMC, OS, HS | Plasma | LLE (solvent: acetonitrile) | HPLC-DAD; type of column: C18; mobile phase: gradient methanol/water (75:25; v/v) | LOD: 0.03–0.2 µg mL−1 LOQ: 0.1–0.4 µg mL−1 R: 90.8–103.8% RSD: 2.1–4.4% | Total content | [60] |
BP-3, OMC, OS, HS | Bovine serum albumin | LLE (solvent; acetonitrile) | HPLC-DAD; type of column: C18; mobile phase: gradient methanol/ water (75:25; v/v) | LOD: 0.03–0.2 µg mL−1 LOQ: 0.1–0.4 µg mL−1 R: 97.9–102.3% RSD: 1.2–3.3% | Total content | [60] |
BP-1, BP-2, BP-3, BP-6, BP-8, 4-OH-BP | Menstrual blood | DLLME (disperser solvent: acetone; extraction solvent: trichloromethane) | UHPLC-MS/MS (ESI); type of column: C18; | LOD: 0.2–0.3 ng mL−1 LOQ: no data R: no data RSD: 0.28–1.59% | Total and free forms content | [82] |
BP-1, BP-2, BP-3, BP-6, BP-8, 4-OH-BP | Serum | DLLME (disperser solvent: acetone; extraction solvent: trichloromethane) | UPLC-MS/MS (ESI+); type of column: C18; mobile phase: gradient 0.1% ammoniacal aq/0.1% ammonia in methanol | LOD: 0.1–0.3 ng mL−1 LOQ: 0.4–0.9 ng mL−1 R: 97–106% RSD: 1.9–13.7% | Total and free forms content | [83] |
BP-3 | Serum | Online SPE | HPLC-MS/MS (APPI-) | LOD: 0.5 ng mL−1 LOQ: no data R: 96% RSD: 7.7–8.7% | Total content | [84,85] |
OC, BMDBM, CDAA | Plasma | LLE (solvent: acetonitrile) | LC-LC-MS/MS (ESI); type of column: C18; mobile phase: methanol/water | LOD: 1.1–6.5 µg L−1 LOQ: 3.5–20.7 µg L−1 R: 89.0–112.8% RSD: 3.0–4.9% | Total content | [63] |
BP-3 | Plasma | LLE (solvent: acetonitrile) | UHPLC-DAD; type of column: C18; mobile phase: acetonitrile/water | LOD: no data LOQ: no data R: 94–99% RSD: 2.3–4.6% | Total content | [86] |
BP-4, 4-DHB, BP-2, BP-1, BP-8, BZ | Whole blood | FPSE | HPLC-PDA; type of column: C18; mobile phase: methanol/phosphate buffer (pH 3) (45:55; v/v) | LOD: 0.03 µg mL−1 LOQ: 0.1 µg mL−1 R: no data RSD: 0.4–10.8% | Total content | [73] |
BP-4, 4-DHB, BP-2, BP-1, BP-8, BZ | Plasma | FPSE | HPLC-PDA; type of column: C18; mobile phase: methanol/phosphate buffer (pH 3) (45:55; v/v) | LOD: 0.03 µg mL−1 LOQ: 0.1 µg mL−1 R: no data RSD: 3.6–11.1% | Total content | [73] |
BP-3, BP-1, 4-OH-BP, BP-8, 4-DHB, BP-2, BP-4, BMDBM | Umbilical cord blood | LLE (solvent: MTBE) | LC-MS/MS (ESI+; ESI−); type of column: R18; mobile phase: methanol/water | LOD: 0.05–0.42 ng mL−1 LOQ: 0.18–1.39 ng mL−1 R: 14.3–146.4% RSD: 0.5–33.8% | Total content | [81] |
BP, 4-MBP | Plasma | LLE-SPE (solvent: MTBE; Oasis Prime-HLB) | HPLC-MS/MS (ESI); type of column: C18; mobile phase: 0.1% formic acid in water/0.1% formic acid in methanol | LOD: 0.8–2 pg mL1 LOQ: 3.5–7 pg mL−1 R: 87–97% RSD: 3.1–9.1% | Total content | [87] |
UV Filters | Matrix | Extraction Technique | Analytical Technique | Analytical Performance | Comments | Ref. |
---|---|---|---|---|---|---|
BP-1, BP-3, BP-8, THB | Semen | SPE (C18) | LC-MS/MS (ESI+); type of column: Mediterranean SEA 18; mobile phase: gradient mobile phase: 0.1% formic acid in water/0.1% formic acid in methanol | LOD: 0.03–0.04 ng mL−1 LOQ: 0.08–0.13 ng mL−1 R: 98–115% RSD: no data | Total content | [56] |
BP-3, OMC, OS, HS | Epidermal membranes | LLE (solvent: acetonitrile) | HPLC-DAD; type of column: C18; mobile phase: gradient methanol/water (75:25; v/v) | LOD: 0.03–0.2 µg mL−1 LOQ: 0.1–0.4 µg mL−1 R: 98.5–99.5% RSD: 1.8–3.2% | Total content | [60] |
OC, 3-BC, 4MBC, OMC, EDP, BP-1, BP-3, BP-6, BP-8, 4-OH-BP | Milk | QuEChERS Extraction; SALLE & d-SPE (sorbent: polysecondary amine and magnesium sulphate) | UHPLC-MS/MS (API); type of column: C18; mobile phase: gradient acetonirile/water/0.1% formic acid | LOD: 0.1–0.2 ng mL1 LOQ: 0.4–0.6 ng mL−1 R: 87–112% RSD: 8–14% | Total content | [88] |
BP-3 | Breast milk | Online SPE (RP18) | HPLC-MS/MS (APCI-); type of column: RP18; mobile phase: gradient methanol/water | LOD: 0.51 ng mL−1 LOQ: no data R: 94.7% RSD: 12.7–18% | Total and free forms content | [89] |
BP-1, BP-3, 4-OH-BP, 4DHB, 4MBC, ODPABA, EtPABA, TBHPBT | Breast milk | Online TFC | HPLC-MS/MS (ESI); type of column: Cyclone and C18; mobile phase: gradient methanol/water/0.1% formic acid | LOD: 0.1–1.5 ng g−1 LOQ: 0.3–5.1 ng g−1 R: no data RSD: 1–12% | Total content | [90] |
BP-3 | Milk | Online SPE (RP18) | HPLC-MS/MS (APCI−); type of column: RP18; mobile phase: methanol/water | LOD: 0.4 ng mL−1 LOQ: no data R: 102% RSD: 8.8–12% | Total and free forms content | [91] |
BP-1, BP-3, BP-6, BP-8, 4-OH-BP | Breast milk | USAD-SPE (15 min of sonification; sorbents: C18, polysecondary amine and magnesium sulphate) | UHPLC-MS/MS (ESI+); type of column: C18; mobile phase: gradient aqueous ammonium formate solution (pH 9)/0.025% ammonia in MeOH | LOD: 0.1–0.2 ng mL−1 LOQ: 0.3–0.6 ng mL−1 R: 90.9–109.5% RSD: 2.0–12.3% | Total content | [92] |
BP-1, BP-2, BP-3, BP-6, BP-8, 4-OH-BP, THB, AVB | Nail | MAE (20 min, 1000 W of power) | UHPLC-MS/MS (ESI+); type of column: C18; mobile phase: gradient methanol/water/0.1% formic acid | LOD: 0.2–1.5 ng g−1 LOQ: 1.0–5.0 ng g−1 R: 90.2–112.2% RSD: 0.8–12.3% | Total content | [93] |
BP-1, BP-2, BP-3, BP-6, BP-8, 4-OH-BP | Placental tissue | MSPD (solvent: ethyl acetate) | UHPLC-MS/MS (ESI); type of column: C18; mobile phase: gradient 0.1% ammoniacal aq solution/0.1% ammonia in methanol | LOD: 0.1 ng g−1 LOQ: 0.2–0.4 ng g−1 R: 95–106% RSD: 4.5–11.8% | Free forms | [94] |
BP-1, BP-2, BP-3, BP-4, 4-OH-BP | Placental tissue | SLE (solvent: ethyl acetate) | LC-MS/MS (ESI−); type of column: RP18; mobile phase: gradient methanol/water | LOD: 0.02–0.36 ng mL−1 LOQ: 0.05–1.20 ng mL−1 R: 72–110% RSD: 4–40% | Total content | [95] |
BP-1, BP-2, BP-3, BP-8, 4-OH-BP | Saliva | DLLME (disperser solvent: acetone; extraction solvent: trichloromethane) | LC-MS/MS; type of column: C18; mobile phase: gradient methanol/water | LOD: 0.01–0.15 ng mL−1 LOQ: 0.05–0.40 ng mL−1 R: no data RSD: 1–19% | Total content | [96] |
EDP, 3-BC, MBC, OMC, OC, BP-1, BP-3, BP-6, BP-8, 4-OH-BP | Placenta tissue | UAE (disperser solvent: methanol; extraction solvent: anisole; 3 min of sonification) | UHPLC-MS/MS; type of column: C18; mobile phase: gradient acetonitrile/0.25% formic acid aq | LOD: 0.05–0.2 µg kg−1 LOQ: 0.15–0.5 µg kg−1 R: 90–112% RSD: 3–15% | Total content | [97] |
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Narloch, I.; Wejnerowska, G. An Overview of the Analytical Methods for the Determination of Organic Ultraviolet Filters in Cosmetic Products and Human Samples. Molecules 2021, 26, 4780. https://doi.org/10.3390/molecules26164780
Narloch I, Wejnerowska G. An Overview of the Analytical Methods for the Determination of Organic Ultraviolet Filters in Cosmetic Products and Human Samples. Molecules. 2021; 26(16):4780. https://doi.org/10.3390/molecules26164780
Chicago/Turabian StyleNarloch, Izabela, and Grażyna Wejnerowska. 2021. "An Overview of the Analytical Methods for the Determination of Organic Ultraviolet Filters in Cosmetic Products and Human Samples" Molecules 26, no. 16: 4780. https://doi.org/10.3390/molecules26164780