气相色谱法测定婴幼儿配方食品中肌醇的衍生方法的比较

Comparison of derivative methods for inositol in infant formula foods by gas chromatography

中文关键词:  肌醇  气相色谱法  硅烷化  糖腈化

英文关键词:myo-inositol  gas chromatography  silylation  glycosylation

中文摘要:

      目的 对气相色谱中2种不同的衍生方法所测定的婴幼儿配方食品中肌醇含量的结果进行比较。 方法 采用硅烷化衍生法和糖腈化衍生法测定婴幼儿配方食品中的肌醇含量。结果 气相色谱-质谱法分别对2种衍生物的其特征离子和分子结构进行检测, 结果表明2种衍生物成分单一, 无杂质峰干扰色谱分析。通过对肌醇的糖腈化衍生物与硅烷化衍生物的气相色谱性能比较研究表明, 肌醇含量0.02~4.0 mg范围内, 2种衍生物的线性相关系数r2=0.999, 定量测定结果的相对标准偏差均小于8%, 加标回收率均为85%~100%。测定结果的准确度和重现性均较好, 均能得到满意的定量测定结果。相同色谱条件下, 衍生物的检测灵敏度相近, 检测限基本相同, 为1.0 mg/100 g。肌醇硅烷化衍生物的色谱峰形较好, 但是不稳定, 易水解。肌醇糖腈化衍生物较稳定, 不易水解。结论 从衍生试剂的环保性、衍生反应的安全性及衍生物的稳定性、对气相色谱仪的污染等方面考虑, 糖腈化衍生法更优于硅烷化衍生法。

英文摘要:

      Objective To compare the results of determination of inositol in infant formula by two different derivative methods using gas chromatography (GC) Methods The content of inositol in infant formula food was determined by the silylation derivation method and glycosylation derivative method. Results The characteristic ions and molecular structure of the 2 derivatives were detected by gas chromatography-mass spectrometry. The results showed that the 2 derivatives were single and had no impurity peak interference chromatographic analysis. The comparison of gas chromatographic performance of glyconitrile derivatives and silane derivatives of inositol showed that at the myo-inositol content range from 0.02 mg to 4.0 mg, the linear correlation coefficients r2 of the 2 derivatives were 0.999, the relative standard deviations of the determination of quantitative results were less than 8%, and the recovery rates were 95%-100%. The accuracy and reproducibility of the results were good and satisfactory quantitative results could be obtained. Under the same chromatographic conditions, the detection sensitivity of the derivatives was similar, and the detection limit was basically the same, which was 1.0 mg/100 g. The chromatographic peaks of inositol silane derivatives were better, but unstable and easy to hydrolyze. The derivatives of inositol nitrile were stable and difficult to hydrolyze. Conclusion Considering environmental protection of derivative reagent, safety of derivative reaction and stability of derivative and pollution to gas chromatograph, glycosylation derivative method is better than silylated derivative method.