改进的油类碘值反相液相色谱法

IF 1.2 4区 化学 Q4 BIOCHEMICAL RESEARCH METHODS Chromatographia Pub Date : 2024-09-30 DOI:10.1007/s10337-024-04367-3
Sutar Purushottam, Chaturbhuj Ganesh
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引用次数: 0

摘要

碘值是评估油类成分和质量的一个重要参数。常用的碘值测定方法是 Wijs 法。最近,有报道称通过一氯化碘碘化 2-chloroaniline 来测定一氯化碘的 HPLC 方法。本研究提出了一种通过 HPLC 对与油样反应后未反应的一氯化碘进行定量来测定碘值的方法,类似于 Wijs 方法中的反滴定法。色谱条件包括在 C18 色谱柱上使用水和乙腈进行梯度洗脱,检测波长为 304 纳米。油酸的碘值已知(83-103 gI/100 g),被用作方法开发和验证参考化合物。该方法根据国际标准化会议的指导原则进行了验证,在 5 至 20 毫克油酸范围内,准确度(98-102%)、稳定性和线性(r2 = 0.999)良好。重复性和中间精度均在 1%以内。验证后的方法被用于 10 种冷榨油的碘值测定。因此,所建立的高效液相色谱法在油类碘值测定中具有样品要求少、准确度高、人工干预少和精密度高等优点。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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Improved Reverse Phase Liquid Chromatography Method for Iodine Value of Oils

Iodine value is an essential parameter for assessing the composition and quality of oils. A commonly used method for iodine value determination is the Wijs method. Recently, the HPLC method for assay of iodine monochloride via iodination of 2-chloroaniline with iodine monochloride has been reported. This study presents an approach for iodine value determination by HPLC via quantification of the unreacted iodine monochloride after reaction with oil samples, similar to the back titration approach in the Wijs method. Chromatographic conditions consist of gradient elution using water and acetonitrile on the C18 column with a detection wavelength of 304 nm. Oleic acid, with a known iodine value (83–103 gI/100 g), was used as a method development and validation reference compound. The method was validated as per International Conference on Harmonization guidelines and was accurate (98–102%), robust, and linear (r2 = 0.999) for oleic acid ranging from 5 to 20 mg. The repeatability and intermediate precision were within 1%. The validated method was applied for the iodine value determination of 10 cold-pressed oils. Thus, an HPLC method is developed, which offers minimal sample requirements, high accuracy, less manual intervention, and precision for the iodine value determination of oils.

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来源期刊
Chromatographia
Chromatographia 化学-分析化学
CiteScore
3.40
自引率
5.90%
发文量
103
审稿时长
2.2 months
期刊介绍: Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.
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