王益超,薛琦,姜廷福,等.盐析辅助分散液液微萃取毛细管电泳测定口服液中甜味剂和防腐剂[J].中国海洋药物,2022,41(4):67-72.
盐析辅助分散液液微萃取毛细管电泳测定口服液中甜味剂和防腐剂
Determination of sweeteners and preservatives in oral liquid by salting out-assisted dispersive liquid-liquid microextraction combined with capillary electrophoresis
投稿时间:2021-04-09  修订日期:2021-05-19
DOI:
中文关键词:  分散液液微萃取  毛细管电泳  甜味剂  防腐剂
English Keywords:dispersive liquid-liquid microextraction  capillary electrophoresis  sweeteners  preservatives
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作者单位E-mail
王益超* 中国海洋大学 2504988033@qq.com 
薛琦 中国海洋大学 xueqi@ouc.edu.cn 
姜廷福 中国海洋大学 jiangtingfu@ouc.edu.cn 
吕志华 中国海洋大学 lvzhihua@ouc.edu.cn 
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中文摘要:
      目的 采用盐析辅助分散液液微萃取(SADLLME)-大体积样品堆积(LVSS)-毛细管电泳(CE)法测定阿斯巴甜、糖精、安赛蜜三种甜味剂以及苯甲酸、山梨酸两种防腐剂。方法 将待测溶液进行盐析液液微萃取处理后进行CE分析测定,设定电泳条件为:进样压力50 mbar,进样时间为 120 s,正常极性下分离电压为 20 kv,检测波长为 214 nm,分离温度为 25 °C。 结果 该方法在0.05~1.00 μg/mL范围内线性关系良好,最低检测限为2.5 ng/mL~10 ng/mL。萃取重现性良好(RSD小于10 %,n=5)。待测组分富集倍数达到657~1674,富集效果良好。把该方法应用于不同种类口服液进行食品添加剂含量的测定,均获得了满意的结果。结论 实验表明使用微萃取与在线富集结合的手段更为高效、快速,能获得更高的富集倍数,成为提高毛细管电泳灵敏度的一种可靠方法。
English Summary:
      Objective To determine aspartame, saccharin and acesamel and benzoic acid and sorbic acid as preservatives by salt-out assisted dispersive liquid-liquid microextraction (SADLLME) -mass sample stair (LVSS) -capillary electrophoresis (CE). Methods The solution was treated by salting-out liquid-liquid microextraction and CE analysis. The electrophoresis conditions were set as follows: injection pressure 50 mbar, injection time 120 s, separation voltage 20 kV under normal polarity, detection wavelength 214 nm, temperature 25 °C. Results The linear range of the method was 0.05-1.00 μg/mL, and the minimum detection limit was 2.5 ng /mL~10 ng/mL. The extraction reproducibility was good (RSD < 10%, n=5). The online enrichment ratio of the components to be measured was 657~1674 with the combination of online and offline, indicating a good enrichment effect. The method has been applied to the determination of food additives in different kinds of oral liquids and satisfactory results have been obtained. Conclusion The experiments show that the combination of microextraction and on-line enrichment is more efficient and rapid, and can obtain higher enrichment ratio, which is a reliable method to improve the sensitivity of capillary electrophoresis.
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