Geng Lijuan, Huang Junrong, Feng Feng, Jiang Pingping, Chu Xiaogang, Zhang Feng, Ling Yun
Se Pu. 2014 Dec;32(12):1380-4. doi: 10.3724/sp.j.1123.2014.07052.
Fructooligosaccharides (FOS) are usually added in milk powder as a kind of prebiotic. Thus, quantitative analysis of the FOS is very important for the quality control of milk powder. In this study, a simple method for the simultaneous determination of three FOS components with degrees of polymerization (DP) 3-5 in milk powder was developed by high performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). The samples were extracted with 50% (v/v) ethanol aqueous solution and defatted by an On Guard RP pretreatment column. The separation was performed on a CarboPac PA200 column by gradient elution using deionized water, 0. 2 mol/L NaOH solution and 0. 4 mol/L NaAc solution as the mobile phases. The flow rate was 0. 4 mL/min. The column temperature was 30 °C; and the injection volume was 25 µL. Good linear response was observed in the concentration range of 0.05-10 mg/L (r2 >0. 9993). The limits of quantification were 0. 02, 0. 005 and 0. 02 mg/L for 1-kestose, nystose and fructofuranosyl-nystose, respectively. The mean recoveries varied from 86. 0% to 114. 0% at three spiked levels of 0. 5, 1. 0 and 5. 0 mg/L. The short-chain fructooligosaccharides from inulooligosaccharides (IOS) were successfully separated by the developed HPAEC-PAD method. The method is simple, accurate, sensitive, and helpful for the quality control of milk powder.
低聚果糖(FOS)通常作为一种益生元添加到奶粉中。因此,低聚果糖的定量分析对于奶粉的质量控制非常重要。在本研究中,建立了一种通过高效阴离子交换色谱-脉冲安培检测法(HPAEC-PAD)同时测定奶粉中三种聚合度(DP)为3-5的低聚果糖成分的简单方法。样品用50%(v/v)乙醇水溶液提取,并用On Guard RP预处理柱脱脂。在CarboPac PA200柱上进行分离,使用去离子水、0.2 mol/L NaOH溶液和0.4 mol/L NaAc溶液作为流动相进行梯度洗脱。流速为0.4 mL/min。柱温为30℃;进样体积为25μL。在0.05-10 mg/L的浓度范围内观察到良好的线性响应(r2>0.9993)。1-蔗果三糖、蔗果四糖和呋喃果糖基蔗果四糖的定量限分别为0.02、0.005和0.02 mg/L。在0.5、1.0和5.0 mg/L的三个加标水平下,平均回收率在86.0%至114.0%之间。通过所建立的HPAEC-PAD方法成功分离了菊粉型果聚糖(IOS)中的短链低聚果糖。该方法简单、准确、灵敏,有助于奶粉的质量控制。