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  • Fast high-performance liquid chromatography analysis of phenethylamine alkaloids in Citrus natural products on a pentafluorophenylpropyl stationary phase.

Fast high-performance liquid chromatography analysis of phenethylamine alkaloids in Citrus natural products on a pentafluorophenylpropyl stationary phase.

Journal of chromatography. A (2007-08-07)
Federica Pellati, Stefania Benvenuti
ABSTRACT

In this study, the chromatographic performance of a pentafluorophenylpropyl (PFPP) stationary phase was evaluated for the rapid separation of phenethylamine alkaloids (i.e. (+/-)-octopamine, (+/-)-synephrine, tyramine, N-methyltyramine and hordenine) in Citrus aurantium plant material (fruits and peel), various Citrus species, extracts and dietary supplements claiming to contain C. aurantium. The problems of phenethylamine alkaloid separation, such as peak tailing, low retention and low resolution, were successfully solved with this stationary phase. The parameters used for the method optimization included the mobile phase counter ion concentration and column temperature. A Discovery HS F5 column (150 mm x 4.6 mm i.d., 5 microm) was used, with an isocratic mobile phase composed of 10 mM ammonium acetate in 90:10 ACN-H(2)O (v/v), at a flow rate of 1.0 mL/min. The column temperature was set at 20 degrees C. The photodiode array detector monitored the eluent at 225 nm. The total analysis time was 10 min. The validation parameters, such as linearity, sensitivity, accuracy, precision and specificity, were found to be highly satisfactory. With a simple sample preparation procedure, different matrices were successfully analyzed for their alkaloid content. The results indicated that the products on sale, labeled as dietary supplements, vary widely in the quantitative composition of the active constituents: the amount of (+/-)-synephrine, the major alkaloid, in such products ranged from 0.65 to 27.41 mg/g. The other compounds were either not detected or were present at low levels. The developed method can be considered suitable for the quality control of Citrus plant material and commercial products.

MATERIALS
Product Number
Brand
Product Description

Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 3 mm, pkg of 1 ea
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 4 mm, pkg of 1 kit
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 10 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 21.2 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm, pkg of 1 kit
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm, pkg of 1 kit
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm