TABLE 3.
Analytical methods for the determination of polyphenols in cladodes
| Opuntia species | Extraction method | Analysis | Compounds identified | Reference |
|---|---|---|---|---|
| Opuntia ficus‐indica (L.) Mill. | Alkaline hydrolysis: 4 N NaOH (1:10, m/v) at 40℃ for 30 min | Detection method: LC/MS‐TOF. Stationary phase: Zorbax SB‐C18, 3.0 × 100 mm, 3.5 µm. Mobile phase: A: water—formic acid, B: methanol. Mode: [M]+; 100–1500 m/z | Quercetin glucosyl‐rhamnosyl‐pentoside, isorhamnetin dihexosyl‐ rhamnoside, kaempferol rhamnosyl‐rhamnosyl‐glucoside, isorhamnetin‐glucosyl‐rhamnosyl‐rhamnoside, isorhamnetin‐glucosyl‐rhamnosyl‐pentoside, isorhamentin hexosyl‐methyl pentosyl‐pentoside, isorhamentin glucosyl‐pentoside, kaempferol‐glucosyl‐rhamnoside, isorhamentin glucosyl‐rhamnoside | Antunes‐Ricardo et al. (2014) |
| Opuntia ficus‐indica (L.) Mill. | Solvent extraction: 0.1 g of sample in 2 ml of methanol:acetone:water (5:4:1), 2.5 hr at 4℃ | Detection method: LC–MS/MS. Stationary phase: Hydro‐RP18, (150 mm × 4.6 mm × 3 mm). Mobile phase: A: acetonitrile/methanol‐formic acid, B: formic acid. Chromatograms recorded: λ = 200–600 nm | Eucomic acid, chlorogenic acid, chlorogenic acid derivative, quercetin 3‐O‐rhamnosyl‐ (1→2)‐[rhamnosyl‐(1→6)]‐glucoside, quercetin 3‐O‐xylosyl‐ rhamnosyl‐glucoside, quercetin 3‐O‐dirhamnoside, kaempferol 3‐O‐(rhamnosyl‐galactoside)−7‐O‐rhamnoside, kaempferol 3‐O‐(rhamnosyl‐glucoside)−7‐O‐rhamnoside, kaempferol 3‐O‐robinobioside‐ 7‐O‐arabinofuranoside, isorhamnetin 3‐O‐rhamnoside‐ 7‐O‐(rhamnosyl‐hexoside), quercetin 3‐O‐rutinoside, quercetin 3‐O‐glucoside, isorhamnetin 3‐O‐rutinoside, kaempferol 3‐O‐rutinoside, quercetin 3‐O‐ arabinofuranoside, kaempferol 3‐O‐glucoside, kaempferol 7‐O‐neohesperidoside, isorhamnetin 3‐O‐galactoside | Astello‐García et al. (2015) |
| Opuntia ficus‐indica (L.) Mill. | Alkaline hydrolysis: 4 N NaOH (1:10, m/v) at 40℃ for 30 min | Detection method: HPLC‐PDA. Stationary phase: Zorbax SB‐C18 (9.4 × 250 mm, 5 µm). Mobile phase: A: water—formic acid, B: methanol. Mode: [M]+;100–1500 m/z | Isorhamnetin‐glucosyl‐pentoside, isorhamnetin‐glucosyl‐rhamnoside, isorhamnetin‐glucosyl‐rhamnosyl‐rhamnoside, isorhamnetin‐glucosyl‐rhamnosyl‐pentoside | Antunes‐Ricardo et al. (2015) |
| Opuntia ficus‐indica f. inermis | Maceration: 25 g of sample, ethanol 100%, 24 hr | Detection method: LC‐HRESIMS. Stationary phase: RP Pursuit XRs ULTRA 2.8, C18, 100 mm ×2 mm. Mobile phase: A: formic acid‐water, B: formic acid‐metanol. Mode: [M]+ 100–2,000 m/z | Quercetin, quercetin 3‐O‐glucoside, kaempferol, kaempferol 3‐O‐glucoside, kaempferol 3‐O‐rutinoside, isorhamnetin, isorhamnetin 3‐O‐glucoside, isorhamnetin 3‐O‐neohesperidoside, 3,3ʹ,4ʹ,5,7‐pentahydroxy‐flavanone, p‐coumaric acid, zataroside‐A, indicaxanthin, ß‐sitosterol | Msaddak et al. (2017) |
| Opuntia ficus‐indica (L.) Mill. | Solvent extraction: 4 g of sample, methanol 50%, 2 hr | Detection method: HPLC‐DAD. Stationary phase: Kinetex C18, 5 µm RP 250 × 4.60 mm. Mobile phase: A: water—formic acid, B: acetonitrile. Chromatograms recorded: Phenolic acids: λ = 256–325 nm, flavonoids: λ = 360 nm | Quercetin, kaempferol, isorhamnetin, ferulic acid, 4‐hydroxybenzoic acid | De Santiago et al. (2018) |
| Opuntia ficus‐indica | Agitation: 4 g of sample, 0.1% formic acid in 80:20 (v/v) methanol/water, 25,000 rpm for 3 min | Detection method: UHPLC‐ESI‐QTOF‐MS; Stationary phase: Agilent Zorbax eclipse plus C18, 50 × 2.1 mm, 1.8 µm. Mobile phase: A: water, B: methanol‐formic acid‐ammonium formate. Mode:[M]+ 50–1000 m/z | Luteolin‐glu, apigenin‐glu, isoflavonoid, myricetin‐glu, quercetin‐glu, kaempferol‐Glu, isorhamnetin‐Glu, furofurans, dibenzylbutyrolactone, alkylphenols, hydroxybenzaldehydes hydroxycoumarins tyrosols, hydroxybenzoics, hydroxyphenylpropanoics, hydroxycinnamics | Rocchetti et al. (2018) |
| Opuntia ficus‐indica (L.) Mill. | Solvent extraction: 200 mg of sample, methanol acidified with formic acid, Sonicated for 25 min | Detection method: UHPLC‐ESI‐MSn. Stationary phase: XSelect HSS T3, (50 × 2.1 mm × 2.5 µm). Mobile phase: A: acetonitrile—formic acid, B: acidified acetonitrile. Mode: [M]−: noncolored phenolics, [M]+: Betalains | Protocatechuic acid hexoside, myricetin‐hexoside, ferulic acid derivative, ferulic acid hexoside, sinapic acid hexoside, quercetin‐rhamnose‐hexoside‐rhamnose, rutin‐pentoside, syrinigyl(t8‐O−4)guaiacyl, kaempferol‐di‐rhamnose‐hexoside, isorhamnetin‐ rhamnose‐rutinoside, quercetin‐hexoside‐pentoside, isorhamnetin derivative, dihydrosinapic acid hexoside, quercetin 3‐O‐rutinoside (rutin), secoisolariciresinol‐hexoside, isorhamnetin derivative, quercetin‐hexoside, kaempferol‐rutinoside, syringaresinol, naringenin‐hexoside, isorhamnetin rutinoside, isorhamnetin‐C‐hexoside, naringin | Mena et al. (2018) |
| Opuntia ficus‐indica (L.) Mill. | Maceration: 500 mg in 25 ml aqueous methanol (80%) overnight at 4℃ | Detection method: LC/MS‐TOF. Stationary phase: Agilent Extended C18 (1.8 μm, 2.1 × 50 mm). Mobile phase: A: water +0.1% formic acid, B: acetonitrile. Mode: [M]−: 50–1,700 m/z | Piscidic acid, eucomic acid, isorhamnetin rhamnosyl‐rutinoside, isorhamnetin‐glucosyl‐rhamnosyl‐pentoside, rutin, narcissin (isorhamnetin rutinoside), isorhamnetin glucoside | Blando et al. (2019) |
| Opuntia ficus‐indica | Solvent extraction: 100% methanol (3× 2L) | Detection method: HPLC‐PDA‐Ms/Ms; Stationary phase: HS F5 column (15 cm 4.6 mm ID, 5 mm; Mobile phase: A:Water +0.1% formic, B: Acetonitrile +0.1% formic; Mode:[M]+ | Quinic acid, malic acid, piscidic acid, diferuloyl‐syringsic acid, eucomic acid, dicaffeoylferulic acid, p‐coumaric acid 3‐O‐glucoside, 7‐glucosyl‐oxy−5‐methyl flavone glucoside sinapic acid 3‐O‐glucoside, sinapic acid 3‐O‐galactoside, quercetin pentosyl‐rutinoside, kaempferol rhamnosyl‐rutinoside isorhamnetin‐glucosyl‐rutinoside, rhamnetin rhamnosyl‐rutinoside, isorhamnetin rhamnosyl‐rutinoside, isorhamnetin pentosyl‐rutinoside, rutin, kaempferol pentosyl‐rutinoside, isorhamnetin pentosyl‐rutinoside, isorhamnetin pentosyl‐hexoside, isorhamnetin rutinoside, rhamnetin 3‐O‐glucoside, isorhamnetin 3‐O‐glucoside, isorhamnetin coumaroyl‐rutinoside, rhamnetin, isorhamnetin, diosmetin, tricin, hydroxyl octadecadienoic acid, eicosanoic acid, eicosanoic acid isomer heneicosanoic acid eicosanoic acid isomer behenic acid | El‐Hawary et al. (2020) |
HPLC‐PDA: high‐pressure liquid chromatograph equipped with a photodiode array detector; UHPLC‐ESI‐QTOF‐MS: ultrahigh‐performance liquid chromatography coupled with electrospray ionization‐quadrupole time‐of‐flight mass spectrometry; HPLC‐PDA‐Ms/Ms: High‐performance liquid chromatography‐photodiode array‐electrospray ionization mass spectrometry; LC/ MS‐TOF: liquid chromatography coupled to a time‐of‐flight mass spectrometer; UHPLC‐ESI‐MSn: ultrahigh‐performance liquid chromatography with electrospray ionization tandem mass spectrometry; LC–MS/MS: high‐performance liquid chromatographic and mass spectrometric; HPLC‐DAD: high‐performance liquid chromatography‐diode array detector system; LC‐HRESIMS: liquid chromatography‐high resolution electro‐spray ionization mass spectrometry.