1. Purification, characterization, and identification of 3‐hydroxy‐4‐methoxy benzal acrolein–an intermediate of synthesizing advantame
- Author
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Siming Zhu, Azhari Siddeeg, Zi-Yuan Gao, Huan Wang Huan Wang, Bo-Ru Chen, and Qiang Liu
- Subjects
Detection limit ,low‐pressure column chromatography ,Chromatography ,purification ,Chemistry ,Calibration curve ,Acrolein ,lcsh:TX341-641 ,Repeatability ,Raw material ,High-performance liquid chromatography ,3‐hydroxy‐4‐methoxy benzal acrolein ,HPLC ,Advantame ,chemistry.chemical_compound ,Column chromatography ,lcsh:Nutrition. Foods and food supply ,Original Research ,Food Science - Abstract
Advantame is a novel sweetener, and 3‐hydroxy‐4‐methoxy benzal acrolein is an important intermediate to synthesize the sweetener. The aim of this study was to evaluate a new low‐cost method to purify 3‐hydroxy‐4‐methoxy benzal acrolein, and the crude intermediate was used as raw material. The intermediate was purified using a low‐pressure column chromatography with a C18 column, using a methanol‐water (6:4, v/v) at a flow rate of 6.0 ml/min, and the loading amount of the crude intermediate in solution was 10.0 mg in total. A method for the analysis of 3‐hydroxy‐4‐methoxy benzal acrolein was established using high‐performance liquid chromatography (HPLC). This method was validated in terms of its linearity, repeatability, accuracy, detection limit, and quantitation limit. The calibration curves of 3‐hydroxy‐4‐methoxy benzal acrolein were linear (r > .999) over a wide concentration range of 0.005–0.08 mg/ml, by comparing the ratio of signal to noise, and the detection limit was 5.0 ng/ml and the quantification limit was 15.0 ng/ml. Good repeatability was obtained (RSD, In this study, a new low‐cost method for the preparation and purification of a sweetner intermediate named 3‐hydroxy‐4‐methoxy benzal acrolein was described. The purifying method and analysis method could be a reference to develop other sweetener intermediates.
- Published
- 2020
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