Detection Method of Synephrine content in Citrus Extract
2024.07.17
[Content Detection] According to HPLC determination.
Chromatographic conditions and system applicability test: Use ODS as filler, methanol- monobasic potassium phosphate (take monobasic potassium phosphate 0.6g, Sodium dodecyl sulfonate 0.1g, glacial acetic acid 1ml, add water to dissolve and dilute to 1000ml) as mobile phase, detection wavelength length as 275nm. The number of theoretical plates should not less than 2000 according to the calculation of the peak of Synephrine.
The preparation of Reference Sample Solution: take appropriate amount of reference sample of Synephrine, measure accurately, add water to make the solution of 1ml containing 30ug of reference sample.
The preparation of the test solution: take the sample powder of 1g, weigh accurately, put in a conical flask with cover, add the methanol 50ml precisely, weigh, heat reflux for 1.5 hour, cool down, weigh again, to full the lose weight by using the methanol, shake well, filtrate. Measure 10ml of subsequent filtrate precisely, drying by distillation, add 10ml water to the residue to dissolve, pass through a polyamide column (60-90 screen mesh, 2.5g, 1.5cm inner diameter, dry column packing), add 25ml water to elute, collect the eluted solution, move to a 25ml flask, add water to the scale, shake well.
Detection method: Precisely draw 10-20ul each of the above-mentioned two reference solution and test solution, and inject it into the HPLC instrument for determination.
This item is calculated base on dry basis, and detect the Synephrine of which not less than 0.30%.
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