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| Matrix | Sample amount | Extraction process | Chromatographic conditions | Instrumental analysis | Linear range | LOD/LOQ | References |
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| Dioscorea species and related medicinal plants (Smilax and Heterosmilax species) | 0.5 g | 15 mL of methanol at room temperature for 0.5 h
Hydrolysis with HCl 10% under vacuum at 60°C
LLE (10 mL of chloroform)
| Mobile phase: 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) using an isocratic elution of 82% (B) in 0–10 min. Flow rate at 0.3 mL/min Column temperature: 40°C
Stationary phase: Waters BEH C18 column (2.1 × 100 mm, 1.7 μm) | HPLC-DAD at 203 nm
UPLC-MicroToFQ (ESI+) | 1–500 μg mL−1 | 0.3/0.8 ng mL−1 | [117] |
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| Root extracts and polyherbal formulations containing Smilax China | 10 g | SPE (Soxhlet apparatus with petroleum ether, chloroform, and methanol) | HPTLC
Mobile phase:
toluene : ethyl acetate (7 : 3% v/v)
HPLC
Mobile phase:
acetonitrile : water 90 : 10 (% v/v) | HPTLC and HPLC with densitometry: 425 nm
| 2.0–10 μg mL−1 | 0.7/2 μg mL−1 | [118] |
|
| Berries extracts and formulations containing Solanum nigrum | 20 g | LLE with 20% of H2SO4 in 70% IPA and hexane for 8 h | Mobile phase: acetonitrile : water 92 : 08 (% v/v). Flow rate at 1.0 mL/min Column temperature: 25°C
Stationary phase: C18 Thermo Hypersil column (250 mm × 4.6 mm, 5 μm) | HPLC-DAD at 203 nm | 1.0–60 μg mL−1 | 0.33/1.0 μg mL−1 | [119] |
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| Cultured cells of Dioscorea zingiberensis | 0.1 g | 20 mL of 95% ethanol, for 2 h. Hydrolysis with 20 mL H2SO4 1 M at 121°C for 2 h. LLE with petroleum ether. The combined petroleum and NaOH 1 M.
| Mobile phase: acetonitrile : water 90 : 10 (% v/v) Flow rate at 1.0 mL/min Column temperature: 30°C
Stationary phase: reversed-phase Agilent TC-C18 column (250 × 4.6 mm, 5 μm)
| HPLC-DAD at 203 and 410 nm | 0.0625–1.000 μg | 0.0372/0.1127 μg | [93] |
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| Cosmeceutical formulations | 2.5 g | LLE with 10 mL of methanol mixed with 50% of tetrahydrofuran | Mobile phase: water : acetonitrile 15 : 85 (% v/v)
Column temperature: room temperature
Stationary phase: Phenomenex Luna-C18 column (150 × 4.6 mm, 5 μm) | HPLC-DAD at 210 nm | 50–1000 μg mL−1 | 10/30 μg mL−1 | [120] |
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| Seed extract of Trigonella foenum graecum | 1 g | SPE (Soxhlet with water and ethanol mixture (1 : 1) for 72 h at 70°C). 80 mL of HCl 3 N for 1 h at 100°C. LLE with diethyl ether | Mobile phase: acetonitrile : water (10 : 90 v/v) gradient mode. Flow rate at 1.0 mL/min. Column temperature: 30°C
Stationary phase: reversed-phase Symmetry C8 column (250 × 4.6 mm, 5 μm) | HPTLC and HPLC-DAD at 205 nm | — | — | [100] |
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| Pharmaceutical forms containing Trigonella foenum graecum | 0.01 g | 25 mL of methanol for 15 min | Mobile phase: acetonitrile : water 90 : 10 (% v/v). Flow rate of 1.0 mL/min
Column temperature: room temperature.
Stationary phase: Phenomenex RP-C18 column (150 × 4.6 mm, 5 μm) | HPLC-UV at 203 nm | 2.0–10.0 μg mL−1 | 0.520/1.577 μg mL−1 | [121] |
|
| Polyherbal formulation containing Tribulus terrestres Linn.extract | 1 g | 90 mL HCl 3 N
for 1 h 30 at 100°C
LLE with 75 mL diethyl
ether 75 mL
| Mobile phase: methanol : water 15 : 85 (% v/v), gradient mode. Flow rate at 1.0 mL/min Column temperature: 30°C
Stationary phase: Symmetry RP-C18 column (250 × 4.6 mm, 5 μm)
| HPLC-DAD at 205 nm | 25.0–75.0 μg mL−1 | — | [122] |
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| Rhizomes or tubers of various Dioscorea species and dietary supplements | 0.5 g for solids and 1 mL for liquids | 9 to 25 mL of methanol | Mobile phase: acetonitrile : water 75 : 25 (v/v%) containing 0.05% formic acid. Flow rate at 0.27 mL/min.
Column temperature: 40°C
Stationary phase:
Acquity UPLC™ BEH Shield RP18 (100 × 2.1 mm, 1.7 μm) | UHPLC-ELSD and DAD | 15.0–550 μg mL−1 | 5.0–12/10-25 μg mL−1 | [123] |
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