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固相萃取-离子色谱法测定甘蔗废蜜及废蜜酒精废液中的非氮有机酸和无机阴离子

[Determination of nonnitrogenous organic acids and inorganic anions in sugarcane molasses and molasses alcohol waste by ion chromatography with solid-phase extraction].

作者信息

Cao Jiaxing, Hang Yiping, Lu Jianping, Tong Zhangfa

机构信息

College of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China.

出版信息

Se Pu. 2010 Sep;28(9):893-7.

Abstract

A method was established for the determination of main nonnitrogenous organic acids (including acetic, lactic, succinic, maleic, tartaric, oxalic, fumaric, citric, and aconitic acids) and three inorganic anions (Cl-, SO4(2-) and PO4(3-)) in sugarcane molasses and molasses alcohol waste by ion chromatography with solid-phase extraction. The diluted sample solution was purified by strong anion exchange (SAX) solid-phase extraction (SPE) in a small packed column to remove most of sugar, pigment and other interfering matrices. The eluate obtained from the column was rinsed with diluted KOH solution and filtered through a 0.45 microm inorganic membrane, finally separated on an anion column of IonPac AS15 with the gradient elution of KOH solution and determined with a suppressed conductivity detector. The pretreatment and procedures of SPE for separating organic acids and inorganic anions from their matrix were investigated. The detection limits wee d less than 0.20 mg/L. The relative standard derivations were less than 6.7%. The organic acids and inorganic anions in three real samples (two sugarcane molasses samples and an alcohol waste sample) were determined, the recovery ranges were from 94% to 109%. The method shows good precision and linearity.

摘要

建立了一种采用离子色谱-固相萃取法测定甘蔗废蜜和废蜜酒精中主要非氮有机酸(包括乙酸、乳酸、琥珀酸、马来酸、酒石酸、草酸、富马酸、柠檬酸和乌头酸)及三种无机阴离子(Cl-、SO4(2-)和PO4(3-))的方法。稀释后的样品溶液通过小填充柱中的强阴离子交换(SAX)固相萃取(SPE)进行纯化,以去除大部分糖、色素和其他干扰基质。从柱中获得的洗脱液用稀释的KOH溶液冲洗,并通过0.45μm无机膜过滤,最后在IonPac AS15阴离子柱上用KOH溶液梯度洗脱进行分离,并用抑制电导检测器进行测定。研究了从基质中分离有机酸和无机阴离子的SPE预处理和程序。检测限小于0.20mg/L。相对标准偏差小于6.7%。测定了三个实际样品(两个甘蔗废蜜样品和一个酒精废样品)中的有机酸和无机阴离子,回收率范围为94%至109%。该方法具有良好的精密度和线性。

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