超高效液相色谱法同时测定食品中4种防腐剂和5种甜味剂

Determination of 4 kinds of preservatives and 5 kinds of artificial sweetnersin foods by ultra performance liquid chromatography

中文关键词:  超高效液相色谱法  C18固相萃取柱  二极管阵列检测器  防腐剂  甜味剂

英文关键词:ultra performance liquid chromatography  C18 solid phase extraction column  photo-diode array  preservatives  artificial sweetners.

中文摘要:

      目的 建立超高效液相色谱法(ultra performance liquid chromatography , UPLC)同时测定食品中4种防腐剂和5种甜味剂含量的分析方法。方法 样品经乙腈水溶液提取, 旋转蒸发仪浓缩后, 经C18固相萃取柱净化。以CORTECS UPLC C18色谱柱(2.0 mm×100 mm, 1.6 μm)分离, 以0.02 mol/mL乙酸铵+0.02%(V/V)乙酸(A)、乙腈(B)为流动相进行梯度洗脱。采用二极管阵列检测器(photo-diode array, PDA)进行紫外波长分析。 结果 4种防腐剂和5种甜味剂在10 min内完成分析。在0.5~50.0 mg/L浓度范围内, 各防腐剂和甜味剂的浓度与峰面积具有良好的线性关系, 相关系数r2在0.999716~0.999956之间。方法的检出限为0.1 mg/kg, 定量限为0.3 mg/kg, 在0.3、2.0、4.0 mg/kg 3个添加水平的回收率为83.5%~108.1%, 相对标准偏差(relative standard deviations, RSD)小于4.6% (n=6)。结论 本方法对食品安全国家标准中防腐剂和甜味剂的前处理方法和仪器分析过程进行优化, 可同时检测食品中多种防腐剂和甜味剂的含量, 结果准确、灵敏度更高。

英文摘要:

      Objective To establish a method for the simultaneous determination of 4 kinds of preservatives and 5 kinds of artificial sweetners in foods by ultra performance liquid chromatography (UPLC). Methods The samples were extracted by acetonitrile aqueous solution, concentrated by rotary evaporator, and purified by C18 solid phase extraction column. CORTECS UPLC C18 column (2.0 mm×100 mm, 1.6 μm) was used for separation, and 0.02 mol/mL ammonium acetate with 0.02%(V/V) acetate (A) and acetonitrile(B) were used as mobile phase for gradient elution. Photo-diode array(PDA) was used for ultraviolet wavelength analysis. Results This method completed the separation of 4 kinds of preservatives and 5 kinds of artificial sweetners in 10 min. At the range of 0.5-50.0 μg/mL, the linear relationship between peak area and concentration of target compounds was good, and the correlation coefficient r2 was 0.999716–0.999956. The limit of detection was 0.1 mg/kg, and the limit of quantitative was 0.3 mg/kg. The recovery of 4 kinds of preservatives and 5 kinds of artificial sweetners at the level of 0.3, 2.0 and 4.0 mg/kg were 83.5%–108.1%, with relative standard deviations (RSDs) less than 4.6% (n=6). Conclusion This method optimizes the pretreatment method and instrument analysis process of preservatives and artificial sweeteners in the national food safety standard. It has high accuracy and sensitivity and can simultaneously detect the content of various preservatives and sweeteners in food.