反相离子对色谱法测定油菜籽(饼)中的硫苷

Determination of Glucosinolates in Rapeseed by Reversed-Phase Ion-Pair Liquid Chromatography

用反相离子对色谱法直接测定油菜籽(饼)中原始硫苷成分,在样品预处理中加入抗氧化剂以防止吲哚类硫苷的氧化分解。研究了主要色谱参数对硫苷组分保留值和选择性的影响,采用烯丙基硫苷或苯甲酸作内标,对硫苷的6种组分进行了定性定量的测定。

Abstract:This paper presents a method for the direct determination of intact glucosinolates in rapeseed by reversed phase ion pair liquid chromatography (RILC).The catechin,mercaptoethanol and phytic acid was adopted respectively in sample pretreatment to prevent indole glucosinolates being oxidized. Among them, the effect of mercaptoethanol was the most obvious.The effects of composition and concentration of the mobile phase, the pH of the mobile phase and the column temperature on the retention and the capacity factor of the glucosinolates were studied. The condition of this method by RILC has been set up:column,YWG C 18 H 37 (10 μm, 250 mm×4 mm i.d.); mobile phase,0.02 mol/L KH 2PO 4 buffer(pH 6) containing 4.5 mmol/L (C 4H 8) 4NBr and CH 3CN(90/10, V/V );flow rate, 1 mL/min; detector,UV 226 nm; column temperation,30 ℃. In this condition, six glucosinolates were separated completely. The relative correction factors were determined by using sinigrin or benzoic acid as the internal standard. The characteristics of glucosinolates in different kinds of Chinese rapeseed can be determined by this RILC method.