Department of Analytical Chemistry, Nutrition and Food Science, University of Alicante, Alicante, Spain.
J Sep Sci. 2012 Apr;35(8):929-36. doi: 10.1002/jssc.201101072.
In the present work, an evaporative light scattering detector was used as a high-temperature liquid chromatography detector for the determination of carbohydrates. The compounds studied were glucose, fructose, galactose, sucrose, maltose, and lactose. The effect of column temperature on the retention times and detectability of these compounds was investigated. Column heating temperatures ranged from 25 to 175°C. The optimum temperature in terms of peak resolution and detectability with pure water as mobile phase and a liquid flow rate of 1 mL/min was 150°C as it allowed the separation of glucose and the three disaccharides here considered in less than 3 min. These conditions were employed for lactose determination in milk samples. Limits of quantification were between 2 and 4.7 mg/L. On the other hand, a temperature gradient was developed for the simultaneous determination of glucose, fructose, and sucrose in orange juices, due to coelution of monosaccharides at temperatures higher than 70°C, being limits of quantifications between 8.5 and 12 mg/L. The proposed hyphenation was successfully applied to different types of milk and different varieties of oranges and mandarins. Recoveries for spiked samples were close to 100% for all the studied analytes.
在本工作中,我们使用蒸发光散射检测器作为高温液相色谱检测器,用于测定碳水化合物。所研究的化合物为葡萄糖、果糖、半乳糖、蔗糖、麦芽糖和乳糖。考察了柱温对这些化合物保留时间和检测灵敏度的影响。柱温加热范围为 25 至 175°C。以纯水为流动相、流速为 1 mL/min 时,最佳峰分辨率和检测灵敏度的温度为 150°C,因为它允许在不到 3 分钟的时间内分离葡萄糖和此处考虑的三种二糖。在这些条件下,用于测定牛奶样品中的乳糖。定量限在 2 至 4.7 mg/L 之间。另一方面,由于在高于 70°C 的温度下单糖共洗脱,我们开发了一个温度梯度,用于同时测定橙汁中的葡萄糖、果糖和蔗糖。定量限在 8.5 至 12 mg/L 之间。所提出的连接成功地应用于不同类型的牛奶和不同品种的橙子和橘子。对于所有研究的分析物,加标样品的回收率接近 100%。