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Alkaloids in Citrus Fruit Juice
Phenethylamine alkaloids (adrenergic amines, biogenic amines) in tangerine juice. Fast, sensitive and
reproducible
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printable Application Sheet
Figure A: TIC – (total Ion Chromatogram) of the juice squeezing
Figure B: EIC – (extracted ion chromatogram) of selected compounds:
1. Tyramine 138.09134 m/z (M+H)+
2. N-methyltyramine 152.10699 m/z (M+H)+
3. Synephrine 168.10191 m/z (M+H)+
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Notes: The problems normally associated with the HPLC separation of adrenergic amines, such as peak tailing, low retention
and low resolution, are solved with this method and is robust and reliable enough to be considered suitable for the quality
control of Citrus plant material and many commercial citrus based products. Traditionally with ordinary HPLC methods,
extensive sample preparation is required, as well as, derivatization of many compounds or ion exchange resins must be used
for sufficient retention.
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Method Conditions
| Column |
Cogent Diamond Hydride™, 4µm, 100A |
| Catalog No. |
70000-15P-2 |
| Dimensions |
2.1 x 150 mm |
| Solvents |
A: DI water + 0.1% formic acid
B: acetonitrile + 0.1% formic acid |
| Mobile Phase |
Inverse Gradient t0 = 1.44 min
| Time |
%B |
Time |
%B |
| 0.0 |
90 |
12.0 |
30 |
| 2.5 |
90 |
13.0 |
30 |
| 6.0 |
70 |
13.1 |
90 |
| 7.0 |
70 |
15.0 |
90 |
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| Flow Rate |
0.4 mL/min. |
| Sample |
Juice, Squeezed from a Tangerine
Sample preparation: Juice was centrifuged and supernatant was diluted with acetonitrile + 0.1% formic acid (1 portion of
juice and 1 portion of acetonitrile). Sample was centrifuged again and 1 mL of the supernatant was injected. |
| Detection |
ESI – pos - Agilent 6210 MSD TOF mass spectrometer |
Discussion
This method, developed for the analysis of adrenergic amines in tangerine juice is sensitive, fast, simple and reproducible when
using Cogent Diamond Hydride™ HPLC column and an Agilent MS TOF instrument. The resulting sample and diluent, after
centrifugation is fully compatible with the ANP mobile phase (shown above), which allows direct injection of the sample with no
further prep time required. Total time of the analysis (including sample preparation and equilibration of the column) is merely
30 minutes.
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