Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi'an 710069, China; National Engineering Research Center for Miniaturized Detection Systems, Xi'an 710069, China.
College of Food Engineering and Nutritional Science, Shaanxi Normal University, Xi'an 710062, China.
Anal Chim Acta. 2017 Jun 15;972:46-53. doi: 10.1016/j.aca.2017.04.032. Epub 2017 Apr 26.
A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r = 0.9998) over the concentration range of 1-500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%-4.3%.
建立了一种用于测定食品中环己基氨基磺酸钠的新方法。在该方法中，将注射器装入样品、KMnO4 粉末和硅胶分散剂的均匀混合物，用作基质固相分散（MSPD）反应器。当反应器中渗透少量浓 HCl 时，环已基氨基磺酸钠在 5 分钟内迅速有效地转化为 2-氯环己酮，并通过在 310nm 波长处使用反相柱进行高效液相色谱法（HPLC）进行检测。与传统的溶液衍生化相比，MSPD 的柱上衍生化提供了更好的净化效果，节省了大量的时间、劳动力和费用。结果表明，在 1-500mg/L 的浓度范围内，线性良好（r=0.9998）。环已基氨基磺酸钠的检出限（LOD）和定量限（LOQ）分别为 0.3mg/L 和 1mg/L。回收率在 91.6%至 101.3%之间，相对标准偏差（RSD）在 2.5%-4.3%范围内。
