Chen Bo-Ru, Liu Qiang, Wang Huan, Gao Zi-Yuan, Siddeeg Azhari, Zhu Si-Ming
School of Food Science and Engineering South China University of Technology Guangzhou China.
Food Sci Nutr. 2020 Jan 1;8(2):744-753. doi: 10.1002/fsn3.1307. eCollection 2020 Feb.
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 C 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 ( > .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 < 2%, = 6), and the recoveries calculated using mixed sample previously quantified ranged from 94.5% to 106.37%. As long as, this method has been successfully applied to the analysis of 3-hydroxy-4-methoxy benzal acrolein; therefore, the method can be put into practical use during the industrial synthesis and real-time detection of the intermediate.
阿凡塔甜是一种新型甜味剂，3-羟基-4-甲氧基苯丙烯醛是合成该甜味剂的重要中间体。本研究旨在评估一种新的低成本方法来纯化3-羟基-4-甲氧基苯丙烯醛，以粗中间体为原料。采用C柱低压柱色谱法纯化中间体，以甲醇-水（6:4，v/v）为流动相，流速为6.0 ml/min，溶液中粗中间体的上样量总计为10.0 mg。建立了一种用高效液相色谱法（HPLC）分析3-羟基-4-甲氧基苯丙烯醛的方法。该方法在线性、重复性、准确性、检测限和定量限方面进行了验证。通过比较信噪比，3-羟基-4-甲氧基苯丙烯醛的校准曲线在0.005 - 0.08 mg/ml的宽浓度范围内呈线性（>0.999），检测限为5.0 ng/ml，定量限为15.0 ng/ml。获得了良好的重复性（RSD < 2%，n = 6），使用先前定量的混合样品计算的回收率在94.5%至106.37%之间。只要该方法已成功应用于3-羟基-4-甲氧基苯丙烯醛的分析；因此，该方法可在中间体的工业合成和实时检测中实际应用。
