Determination of Bitter Orange alkaloids in dietary supplements standard reference materials by liquid chromatography with ultraviolet absorbance and fluorescence detection

Putzbach, Karsten; Rimmer, Catherine A.; Sharpless, Katherine E.; Sander, Lane C.

doi:10.1016/j.chroma.2006.12.027

Cited by 34 publications

(26 citation statements)

References 15 publications

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“…Most published methods for the analysis of adrenergic amines in Citrus fruits and dietary supplements are based on HPLC with spectrophotometric 8–12, spectrofluorimetric 9, 13 or mass spectrometric 14, 15 detection. Most of these methods require particular conditions, such as specific kinds of columns ( e.g.…”

Section: Introductionmentioning

confidence: 99%

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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Section: Introductionmentioning

confidence: 99%

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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show abstract

“…In the pilot exercise, participants measured caffeine in SRM 3260 Bitter Orange-Containing Solid Oral Dosage Form as the unknown and SRM 3243 Ephedra-Containing Solid Oral Dosage Form as the control (37, 67, 68). The consensus of the reported data included the target value for both the unknown and the control, with few outliers.…”

Section: Resultsmentioning

confidence: 99%

“…Participants measured synephrine in SRM 3258 Bitter Orange Fruit as the unknown and in SRM 3259 Bitter Orange Extract as the control (68, 69). The level of synephrine was approximately 10 times greater in the control than in the unknown.…”

Section: Resultsmentioning

confidence: 99%

Dietary Supplement Laboratory Quality Assurance Program:

Phillips¹,

Rimmer²,

Wood³

et al. 2012

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The National Institute of Standards and Technology (NIST) has established a Dietary Supplement Laboratory Quality Assurance Program (DSQAP) in collaboration with the National Institutes of Health Office of Dietary Supplements. Program participants measure concentrations of active and/or marker compounds as well as nutritional and toxic elements in food and dietary supplements distributed by NIST. Data are compiled at NIST, where they are analyzed for accuracy relative to reference values and concordance among the participants. Performance reports and certificates of completion are provided to participants, which can be used to demonstrate compliance with current Good Manufacturing Practices as promulgated by the U.S. Food and Drug Administration. The DSQAP has conducted five exercises to date, with total participation including more than 75 different laboratories and many more individual analysts.

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“…The sensitive determination of NE, synephrine, and isoproterenol is very important in biological fluids such as urine, plasma, and serum. Recently, HPLC, flow injection analysis (FIA), and CE have been used in the determination of synephrine [24,25] or NE [26 -29], or/ and isoproterenol [30 -32]. In CE, the detection modes used mainly include ED [24,30], LIF [26], CL [27,31], and UV -Vis [32].…”

Section: Introductionmentioning

confidence: 99%

Sensitive determination of norepinephrine, synephrine, and isoproterenol by capillary electrophoresis with indirect electrochemiluminescence detection

Liu¹,

Cao

Zheng

et al. 2008

J of Separation Science

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A new and sensitive method for the determination of norepinephrine (NE), synephrine, and isoproterenol was developed by CE separation and indirect electrochemiluminescence detection (ECL) based on their quenching effects on the tris(2,2'-bipyridyl)-ruthenium(II)/tripropylamine (TPA) system. The conditions for CE separation and ECL detection were investigated in detail. Under the optimum conditions, the three analytes were well separated within 9 min. The LODs (S/N = 3) in standard solution are 2.6 x 10(-8) mol/L for NE, 6.6 x 10(-9) mol/L for synephrine and 8.4 x 10(-8) mol/L for isoproterenol, respectively. The precisions of intraday and interday are less than 4.4 and 6.1%, respectively. The LOQs (S/N = 10) in real human urine samples are 2.6 x 10(-7) mol/L for NE, 8.8 x 10(-8 ) mol/L for synephrine, and 8.8 x 10(-7) mol/L for isoproterenol, respectively. The applicability of the proposed method was illustrated in the determination of 20 human urine samples from diabetic patients and healthy persons. The results obtained indicated that the level of NE in patients (mean value 0.41 micromol/L) was higher than that in healthy persons (mean value 0.24 micromol/L).

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Determination of Bitter Orange alkaloids in dietary supplements standard reference materials by liquid chromatography with ultraviolet absorbance and fluorescence detection

Cited by 34 publications

References 15 publications

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

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

Dietary Supplement Laboratory Quality Assurance Program:

Sensitive determination of norepinephrine, synephrine, and isoproterenol by capillary electrophoresis with indirect electrochemiluminescence detection

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