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
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。
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.
标题：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
英文标题：Simultaneous determination of 4 kinds of artificial sweeteners by solid phase extraction-ultra performance liquid chromatography under different wavelength
作者：
陈其钊 广东省生物工程研究所广州甘蔗糖业研究所国家糖业质量监督检验中心广东广州510316
陈嘉敏 广东省生物工程研究所广州甘蔗糖业研究所国家糖业质量监督检验中心广东广州510316
陈红香 广东省生物工程研究所广州甘蔗糖业研究所国家糖业质量监督检验中心广东广州510316
王桂华 广东省生物工程研究所广州甘蔗糖业研究所国家糖业质量监督检验中心广东广州510316
李家威 广东省生物工程研究所广州甘蔗糖业研究所国家糖业质量监督检验中心广东广州510316
郭剑雄 广东省生物工程研究所广州甘蔗糖业研究所国家糖业质量监督检验中心广东广州510316
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,
发表日期：2018-06-21
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