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Purification, characterization, and identification of 3‐hydroxy‐4‐methoxy benzal acrolein–an intermediate of synthesizing advantame
Food Science & Nutrition ( IF 3.5 ) Pub Date : 2020-01-01 , DOI: 10.1002/fsn3.1307 Bo-Ru Chen 1 , Qiang Liu 1 , Huan Wang 1 , Zi-Yuan Gao 1 , Azhari Siddeeg 1 , Si-Ming Zhu 1
Food Science & Nutrition ( IF 3.5 ) Pub Date : 2020-01-01 , DOI: 10.1002/fsn3.1307 Bo-Ru Chen 1 , Qiang Liu 1 , Huan Wang 1 , Zi-Yuan Gao 1 , Azhari Siddeeg 1 , Si-Ming Zhu 1
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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 < 2%, n = 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.
中文翻译：
Advantame合成中间体3-羟基-4-甲氧基苯亚甲基丙烯醛的纯化、表征和鉴定
Advantame是一种新型甜味剂，3-羟基-4-甲氧基苯亚甲基丙烯醛是合成该甜味剂的重要中间体。本研究的目的是评估一种新的低成本方法来纯化 3-羟基-4-甲氧基苯亚甲基丙烯醛，并以中间体粗品为原料。使用C 18柱低压柱色谱法纯化中间体，使用甲醇-水（6:4，v/v），流速为6.0 ml/min，粗中间体的上样量为溶液总量为10.0mg。建立了高效液相色谱（HPLC）分析3-羟基-4-甲氧基苯亚甲基丙烯醛的方法。该方法的线性度、重复性、准确性、检测限和定量限均经过验证。通过比较信噪比，3-羟基-4-甲氧基苯亚甲基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 ( r > .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范围为 94.5% 至 106.37%。该方法已成功应用于3-羟基-4-甲氧基苯亚甲基丙烯醛的分析；因此，该方法可在中间体的工业合成和实时检测中投入实际应用。
更新日期：2020-01-01
中文翻译：
Advantame合成中间体3-羟基-4-甲氧基苯亚甲基丙烯醛的纯化、表征和鉴定
Advantame是一种新型甜味剂，3-羟基-4-甲氧基苯亚甲基丙烯醛是合成该甜味剂的重要中间体。本研究的目的是评估一种新的低成本方法来纯化 3-羟基-4-甲氧基苯亚甲基丙烯醛，并以中间体粗品为原料。使用C 18柱低压柱色谱法纯化中间体，使用甲醇-水（6:4，v/v），流速为6.0 ml/min，粗中间体的上样量为溶液总量为10.0mg。建立了高效液相色谱（HPLC）分析3-羟基-4-甲氧基苯亚甲基丙烯醛的方法。该方法的线性度、重复性、准确性、检测限和定量限均经过验证。通过比较信噪比，3-羟基-4-甲氧基苯亚甲基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 ( r > .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范围为 94.5% 至 106.37%。该方法已成功应用于3-羟基-4-甲氧基苯亚甲基丙烯醛的分析；因此，该方法可在中间体的工业合成和实时检测中投入实际应用。
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