固相萃取-多波长超高效液相色谱法同时测定食品中的4种甜味剂

Simultaneous determination of 4 kinds of artificial sweeteners by solid phase extraction-ultra performance liquid chromatography under different wavelength

中文关键词:  超高效液相色谱  响应面  甜味剂  安赛蜜  纽甜  阿斯巴甜  糖精钠

英文关键词:ultra performance liquid chromatography  response surface methodology  sweeteners  acesulfame-K  neotame  aspartame  saccharin sodium

中文摘要:

      目的 建立固相萃取富集净化, 超高效液相色谱-二极管阵列检测器快速测定食品中安赛蜜、纽甜、阿斯巴甜、糖精钠4种甜味剂的方法。方法 以ACQUITY UPLC? BEH C18(100 mm×2.1 mm, 1.7 μm)为色谱柱, 对流动相的组成、洗脱方式、检测波长等进行优化, 同时应用Box-Behnken中心组合法进行3因素3水平的实验设计, 考察料液比、提取时间、溶液pH对提取得率的影响。结果 最佳工艺条件为提取时间 30 min、液固比5:1(V:m)、溶液pH 6。4种甜味剂在0.05~5.00 mg/kg线性范围内线性关系良好, 线性相关系数(r2)均大于0.9951; 目标物的检出限(S/N≥3)为0.005~0.5 mg/L; 3个加标水平下的回收率为73.6%~103.2%, 相对标准偏差为1.8%~6.2%。结论 此方法简单、快速、分离效果好、分析成本低, 可用于食品中4种甜味剂的检测。

英文摘要:

      Objective To establish a method for simultaneous determination of 4 kinds of sweeteners (acesulfame-K, neotame, aspartame and saccharin sodium)in food by solid phase extraction (SPE) coupled with ultra performance liquid chromatography with diode array detection (UPLC-DAD). Methods The UPLC separation was carried out on a ACQUITY UPLC? BEH C18 column (100 mm×2.1 mm, 1.7 μm). Several parameters, including the composition and gradient elution program of the mobile phase and optimum detection wavelength of diode-array detector were optimized for improving the chromatographic performance and the sensitivity of determination. Based on single-factor tests, a 3-factor and 3-level center composite experimental design of Box-Behnken was adopted to investigate the influence of 3 main factors including liquid-solid ratio, ultrasonic treatment time and solution pH. Results The optimum conditions of ultrasonic-assisted extraction technology were as follows: ultrasonic treatment time was 30 min, liquid-solid ratio was 5:1 (V:m) and solution pH=6. The 4 kinds of sweeteners had good linear relationships in the range of 0.05-5.00 mg/kg, and the correlation coefficients were higher than 0.9951. The limits of detection (S/N≥3) of the 4 sweeteners were 0.005-0.5 mg/L. The recoveries for 4 kinds of artificial sweeteners at 3 spiked levels were 73.6%-103.2% with relative standard deviations of 1.8%-6.2%. Conclusion This method is simple, rapid and has good separation effect and low analysis cost, which can be used to detect 4 kinds of sweeteners in food.