State Key Laboratory of Pulp and Paper Engineering and ‡School of Materials Science and Engineering, South China University of Technology , Guangzhou, Guangdong 510640, People's Republic of China.
J Agric Food Chem. 2017 Aug 16;65(32):7012-7016. doi: 10.1021/acs.jafc.7b03144. Epub 2017 Aug 8.
This study reports on a headspace-based gas chromatography (HS-GC) technique for determining the degree of substitution (DS) of cationic guar gum during the synthesis process. The method is based on the determination of 2,3-epoxypropyltrimethylammonium chloride in the process medium. After a modest pretreatment procedure, the sample was added to a headspace vial containing bicarbonate solution for measurement of evolved CO by HS-GC. The results showed that the method had a good precision (relative standard deviation of <3.60%) and accuracy for the 2,3-epoxypropyltrimethylammonium chloride measurement, with recoveries in the range of 96-102%, matching with the data obtained by a reference method, and were within 12% of the values obtained by the more arduous Kjeldahl method for the calculated DS of cationic guar gum. The HS-GC method requires only a small volume of sample and, thus, is suitable for determining the DS of cationic guar gum in laboratory-scale process-related applications.
本研究报告了一种基于顶空的气相色谱(HS-GC)技术,用于在合成过程中测定阳离子瓜尔胶的取代度(DS)。该方法基于过程介质中 2,3-环氧丙基三甲基氯化铵的测定。经过适度的预处理程序后,将样品加入顶空瓶中,加入碳酸氢盐溶液以通过 HS-GC 测量释放的 CO。结果表明,该方法对 2,3-环氧丙基三甲基氯化铵的测定具有良好的精密度(<3.60%的相对标准偏差)和准确性,回收率在 96-102%范围内,与参考方法获得的数据相匹配,并且与更繁琐的凯氏定氮法测定阳离子瓜尔胶的计算 DS 的值相差不超过 12%。HS-GC 法仅需少量样品,因此适用于实验室规模的过程相关应用中测定阳离子瓜尔胶的 DS。