Determination of synephrine in weight-loss products using high performance liquid chromatography with acidic potassium permanganate chemiluminescence detection

Slezak, Teo; Francis, Paul S.; Anastos, Nicole; Barnett, Neil W.

doi:10.1016/j.aca.2007.04.038

Cited by 29 publications

(30 citation statements)

References 23 publications

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“…Octopamine and tyramine are natural constituents of C. aurantium, but are present at lower concentrations than synephrine (8). We previously reported that octopamine produces a similar amount of light to synephrine when treated with acidic potassium permanganate (15). Tyramine produced an emission with up to two-fold greater intensity, depending on the pH of the reagent.…”

Section: Selection Of Phenolic Compoundsmentioning

confidence: 93%

“…Where possible, we replicated the instrument manifolds and chemical conditions described in the previously proposed chemiluminescence methods for the determination of synephrine (13)(14)(15). In the first (13), an alkaline luminol solution was merged with a solution of hexacyanoferrate(III) and then with a water carrier stream containing the injected sample (Fig.…”

Section: Instrument Manifolds and Limits Of Detectionmentioning

confidence: 99%

“…2) were either commonly found in the types of samples analysed in the proposed methods for the determination of synephrine (13)(14)(15) or previously shown to give a significant response with one of more of the four chemiluminescence reagent systems. Octopamine and tyramine are natural constituents of C. aurantium, but are present at lower concentrations than synephrine (8).…”

Section: Selection Of Phenolic Compoundsmentioning

confidence: 99%

“…Although synephrine has been promoted by some supplement manufacturers as a safe alternative to ephedrine, there are concerns that it may also have potential to cause harm (3,4). Numerous new methods for the determination of synephrine have recently been reported (5)(6)(7)(8)(9)(10)(11)(12), including three based on chemiluminescence detection (13)(14)(15).…”

Section: Introductionmentioning

confidence: 99%

“…We reported the determination of synephrine based on the chemiluminescence reaction with potassium permanganate in acidic solution (15). Initial investigations were conducted using FIA, but when this method of detection was applied to quantify synephrine in C. aurantium extracts and dietary supplements, chromatographic separation was used to isolate the target analyte from interferences.…”

Section: Introductionmentioning

confidence: 99%

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Selectivity and potential interference from phenolic compounds in chemiluminescence methods for the determination of synephrine

et al. 2008

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Three recently reported chemiluminescence methods (based on reactions with alkaline luminol and hexacyanoferrate(III); acidic cerium(IV) and rhodamine B; and acidic permanganate with polyphosphates) for the determination of synephrine were re-evaluated in terms of their selectivity towards this analyte in comparison to other phenolic compounds. A fourth reagent system, acidic soluble manganese(IV) and formaldehyde, was also examined. Each set of reagents was sensitive towards synephrine (limits of detection were 3 × 10 -9 , 5 × 10 -8 , 1 × 10 -8 and 1 × 10 -8 mol/L, respectively) but also responded with numerous other phenolic compounds, including some that are present in citrus fruit extracts, dietary supplements and/or biological fluids. It is therefore recommended that the determination of synephrine in these matrices should incorporate physical separation of sample components (e.g. chromatography or electrophoresis). In more general terms, this study illustrates that accurate percentage recoveries for an analyte in spiked samples (without validation against another analytical method) are insufficient to confirm the analytical utility of new flow-injection analysis (FIA) procedures.

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Section: Selection Of Phenolic Compoundsmentioning

confidence: 93%

Section: Instrument Manifolds and Limits Of Detectionmentioning

confidence: 99%

Section: Selection Of Phenolic Compoundsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Selectivity and potential interference from phenolic compounds in chemiluminescence methods for the determination of synephrine

et al. 2008

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First Electroanalytical Methodology for the Determination of Hordenine in Dietary Supplements using a Boron‐doped Diamond Electrode

et al. 2019

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The present work describes the first electrochemical investigation and a simple, rapid and modification‐free electroanalytical methodology for quantification of hordenine (a potent phenylethylamine alkaloid) using a boron‐doped diamond electrode. At optimized square‐wave voltammetric parameters, the observed oxidation peak current in 0.1 M HClO4 at +1.33 V (vs. Ag/AgCl) increased linearly from 5.0 to 100 μg mL−1 (3.0×10−5–6.1×10−4 M), with detection limit of 1.3 μg mL−1 (7.8×10−6 M). The applicability of the developed method was tested with the determination of hordenine in the commercial dietary supplement formulations.

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Fast CE analysis of adrenergic amines in different parts of Citrus aurantium fruit and dietary supplements

Mercolini

Mandrioli

Trerè

et al. 2010

J of Separation Science

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A CE method has been developed for the simultaneous analysis of the adrenergic amines synephrine, octopamine and tyramine in Citrus aurantium (bitter orange) fruit extracts and in dietary supplements. The analytes were separated on a fused silica capillary (50 microm id, 40.0 cm effective length, 48.5 cm total length) using a BGE composed of phosphate buffer (pH 2.5, 50 mM) and applying a 30 kV potential. The samples were injected hydrodynamically at 50 mbar for 25 s. The use of photodiode array detection (lambda=195 nm) allowed the quantification of the analytes and the control of peak purity. The method has been fully validated, obtaining satisfactory values of precision and extraction yield. The analytes are extracted with water from the dried whole fruits or fruit parts (endocarp, mesocarp and exocarp) or from the commercial formulations and directly injected into the CE apparatus. The results obtained were satisfactory in terms of precision (RSD < 5.7%) and accuracy (recovery > 89%). Thus, the method has demonstrated to be suitable for the qualitative and quantitative determination of synephrine, octopamine and tyramine in C. aurantium extracts, for dietary supplement quality control and for food adulteration identification.

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Determination of synephrine in weight-loss products using high performance liquid chromatography with acidic potassium permanganate chemiluminescence detection

Cited by 29 publications

References 23 publications

Selectivity and potential interference from phenolic compounds in chemiluminescence methods for the determination of synephrine

Selectivity and potential interference from phenolic compounds in chemiluminescence methods for the determination of synephrine

First Electroanalytical Methodology for the Determination of Hordenine in Dietary Supplements using a Boron‐doped Diamond Electrode

Fast CE analysis of adrenergic amines in different parts of Citrus aurantium fruit and dietary supplements

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