气相色谱/电子捕获检测法测定键合态糖苷的研究

该文建立了GC/ECD法测定键合态糖苷的分析方法,采用N-甲基-双(三氟乙酰胺)(MBTFA)对目标物进行衍生,并优化了反应温度和时间.结果表明在60℃下反应50 min时,衍生效果最好.该衍生反应在产物中引入氟元素,可用GC/JECD法进行测定.以苯氧基葡萄糖苷为典型目标物进行线性研究,方法在0.05～200 mg/...

Study on Determination of Glucoside by Gas Chromatography with Electron Capture Detector

A GC/ECD method was developed for the determination of glucosides.The target compound(phenyl β-D-glucopyranoside) was derivatized with N-methyl bis(trifluoroacetamide)(MBTFA).The derivatization temperature and time were optimized.The result indicated that the best derivatization conditions were achieved at 60 ℃ for 50 min.Fluorine was introduced to the product molecule after derivatization to provide the fundamental element for the detection of GC/ECD.Linear study was conducted by using phenyl β-D-glucopyranoside as a typical compound,and a correlation coefficient(r2) of 0.999 6 was obtained in the range of 0.05-200 mg·L-1.Six glucosides could be accurately identified by GC/ECD after MBTFA derivatization.Repeatability experiment showed that this derivatization combined with GC/ECD determination had a good performance,the relative standard deviation for the corresponding peak area was lower than 3% in 72 h.This method was also compared with the GC-MS method,and the limit of detection of GC/ECD method was greatly lowered.The proposed method is applicable in the determination of trace amount of glucosides in real sample.