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一种通过手动进样流动注射系统测定植物油中游离脂肪酸的新方法。

A novel approach for determination of free fatty acids in vegetable oils by a flow injection system with manual injection.

作者信息

Ayyildiz H Filiz, Kara Huseyin, Sherazi S T H

机构信息

Department of Chemistry, Selcuk University, Campus-Konya, Turkey.

出版信息

Lipids. 2011 Dec;46(12):1181-90. doi: 10.1007/s11745-011-3610-9. Epub 2011 Sep 9.

Abstract

A non-aqueous flow injection method for determining free fatty acid (FFA) content in corn and sunflower oil samples was developed. A single-line manifold system was built by modification of an HPLC for flow injection analysis (FIA). Without pre-treatment, oil samples were injected into a n-propanol solution containing KOH and phenolphthalein (PHP). The main parameters, such as flow rate of carrier phase, length, geometry, inner diameters of the coils and reagent concentration were all optimized. The proposed FIA method was validated for precision, accuracy, linear region, limit of detection (LOD) and limit of quantification (LOQ). The intra- and inter-day measurements of the precision of the method were found to be within the limits of acceptance criteria (RSD < 1%), and were rugged when the method was performed by a different analyst. The linear concentration range was calculated as 0.09-1.50 and 0.07-1.40 FFA% for corn and sunflower oils, correspondingly. The LOD and LOQ were found to be 7.53 × 10(-4)-2.28 × 10(-3) oleic acid % and 7.11 × 10(-4)-2.23 × 10(-3) oleic acid % for corn and sunflower oils, respectively. The results were compared with those obtained by the AOCS (Ca-5a-40) method using statistical t and F tests, and a significant difference was not observed between the methods at a 95% confidence level. The proposed method is suitable for quality control of routine applications due to its simplicity, high sample throughput, and economy of solvents and sample, offering considerable promise as a low cost analytical system that needs minimum human intervention over long periods of time.

摘要

建立了一种非水流动注射法,用于测定玉米和葵花籽油样品中的游离脂肪酸(FFA)含量。通过对高效液相色谱(HPLC)进行改造构建了单通道流路系统,用于流动注射分析(FIA)。油样无需预处理,直接注入含有氢氧化钾和酚酞(PHP)的正丙醇溶液中。对诸如载流相流速、盘管长度、几何形状、内径以及试剂浓度等主要参数进行了优化。对所提出的流动注射分析法进行了精密度、准确度、线性范围、检测限(LOD)和定量限(LOQ)的验证。该方法日内和日间精密度测量结果均在可接受标准范围内(相对标准偏差<1%),且不同分析人员操作时方法稳定性良好。玉米和葵花籽油的线性浓度范围分别计算为0.09 - 1.50 FFA%和0.07 - 1.40 FFA%。玉米和葵花籽油的检测限分别为7.53×10⁻⁴ - 2.28×10⁻³油酸%和7.11×10⁻⁴ - 2.23×10⁻³油酸%,定量限分别为相应数值。使用统计t检验和F检验将结果与采用美国油脂化学家协会(AOCS,Ca - 5a - 40)方法获得的结果进行比较,在95%置信水平下未观察到两种方法之间存在显著差异。所提出的方法因其简单性、高样品通量以及溶剂和样品的经济性,适用于常规应用的质量控制,作为一种长期需要最少人工干预的低成本分析系统具有很大的前景。

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