Mu Li, Liu Yuhang, Luo Huihong, Liu Qianqian, Zhang Li, Xu Ying, Li Gang, Tong Qi
College of Food Science and Engineering of ChangChun University, Changchun, Jilin, China.
Jilin Province Product Quality Supervision and Inspection Institute, Changchun, Jilin, China.
PLoS One. 2024 Aug 8;19(8):e0308220. doi: 10.1371/journal.pone.0308220. eCollection 2024.
The oil used to fry food is often used multiple times to reduce costs. However, when foods containing sweeteners are processed in this way, the sweeteners may produce substances harmful to the body as a result of repeated frying at high temperatures. This article investigated the stability of sodium cyclamate during deep-frying by HPLC using a pre-column derivatization method. The results showed that cyclohexylamine was a decomposition product of a standard sample of sodium cyclamate when deep-fried at 200°C for 25 min. A pre-column derivatization/HPLC method was established to determine cyclohexylamine, a decomposition product of sodium cyclamate, under these conditions. Dansyl chloride was used as the derivatization reagent, the derivatization temperature was 60°C, the derivatization time was 20 min, the pH of sodium bicarbonate buffer solution was 11, and the concentration of dansyl chloride was 2.0 mg/mL. Detection was carried out by using an Agilent 1260 high-performance liquid chromatograph coupled with an ultraviolet detector. The ultraviolet detection wavelength was 254 nm, and the mobile phase was acetonitrile-1.0 g/L potassium dihydrogen phosphate solution at a flow rate of 1.0 mL/min. Gradient elution was adopted, the peak of the cyclohexylamine derivative appeared at a retention time of 17.75 min, and the peak area response value was the largest. The methodological validation analysis showed that the detection limit of cyclohexylamine was 0.5 mg/kg, the quantification limit was 2.0 mg/kg, and the spiked recoveries were in the range of 99.37-110.16%. The relative standard deviations (RSDs) were in the range of 0.17-1.26%. Four samples were tested and analyzed by the established method, and cyclohexylamine was not detected.
用于油炸食品的油通常会多次使用以降低成本。然而，当以这种方式加工含有甜味剂的食品时，由于在高温下反复油炸，甜味剂可能会产生对身体有害的物质。本文采用柱前衍生化高效液相色谱法研究了甜蜜素在油炸过程中的稳定性。结果表明，甜蜜素标准样品在200℃油炸25分钟时，环己胺是其分解产物。建立了柱前衍生化/高效液相色谱法，用于测定在这些条件下甜蜜素的分解产物环己胺。使用丹磺酰氯作为衍生化试剂，衍生化温度为60℃，衍生化时间为20分钟，碳酸氢钠缓冲溶液的pH值为11，丹磺酰氯的浓度为2.0mg/mL。采用安捷伦1260高效液相色谱仪与紫外检测器联用进行检测。紫外检测波长为254nm，流动相为乙腈-1.0g/L磷酸二氢钾溶液，流速为1.0mL/min。采用梯度洗脱，环己胺衍生物的峰出现在保留时间17.75分钟处，峰面积响应值最大。方法学验证分析表明，环己胺的检出限为0.5mg/kg，定量限为2.0mg/kg，加标回收率在99.37-110.16%范围内。相对标准偏差（RSD）在0.17-1.26%范围内。采用所建立的方法对4个样品进行了测试分析，未检测到环己胺。
