Abstract

In this paper, a sensitive method for the determination of 3-chloro-1,2-propanediol (3-MCPD) by high performance liquid chromatography-fluorescence detection (HPLC-FLD) was established, in which 9-(2-Hydroxypropyl) adenine (HP-Ade) was selected as the fluorescent derivatization reagent because of its good water solubility and hydrophobicity. The principle of the method lies in the origination of chloroacetaldehyde with the periodate oxidation of 3-MCPD and its' fluorescence derivatization by HP-Ade to produce a strong fluorescent substance, name as 1-N⁶-vinylidene-9-(2-hydroxypropyl)adenine (ε-HP-Ade), used for quantitative determination of 3-MCPD by HPLC-FLD. Some mobile phase conditions and incubation parameters related with the method features were studied and optimized. Under the optimal conditions, the method shows high sensitivity, good linearity (r² = 0.999) and good repeatability (RSD% between 1.04% and 2.55%), the detection limit (LOD) and quantification limit (LOQ) were 0.02 ng/mL and 0.06 ng/mL respectively. It has been successfully applied for the determination of various edible vegetable oil samples, the chromatogram shows symmetrical peak shape, perfect separation and very “clean” profiles. In comparison with gas chromatography-mass spectrum (GC-MS), the pretreatment process of the proposed method was totally operated in aqueous phase, the instrument requirements and cost are relatively lower, thus it will provide another choice for the routine analysis of 3-MCPD.

摘要

本文建立了高效液相色谱-荧光检测 (HPLC-FLD) 测定 3-氯-1,2-丙二醇 (3-MCPD) 的灵敏方法，其中 9-(2-羟丙基)腺嘌呤（HP-Ade）因其良好的水溶性和疏水性而被选作荧光衍生试剂。该方法的原理在于3-MCPD高碘酸盐氧化生成氯乙醛，HP-Ade对其进行荧光衍生产生强荧光物质，命名为1- N ⁶-vinylidene-9-(2-hydroxypropyl)adenine (ε-HP-Ade)，用于通过 HPLC-FLD 定量测定 3-MCPD。对与方法特点相关的流动相条件和孵育参数进行了研究和优化。在最佳条件下，该方法灵敏度高，线性度好（r ²= 0.999）和良好的重复性（RSD% 在 1.04% 和 2.55% 之间），检测限 (LOD) 和定量限 (LOQ) 分别为 0.02 ng/mL 和 0.06 ng/mL。它已成功应用于各种食用植物油样品的测定，色谱图显示对称的峰形、完美的分离和非常“干净”的曲线。与气相色谱-质谱（GC-MS）相比，该方法的前处理过程完全在水相中进行，仪器要求和成本相对较低，为3-3-的常规分析提供了另一种选择。 MCPD。