使用离子选择性电极和直接测量技术测定牛奶、大豆和水基产品中的氟化物:单实验室验证,首次行动 2022.05。

IF 1.7 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Journal of AOAC International Pub Date : 2024-01-04 DOI:10.1093/jaoacint/qsad104
Renée M Erney, Charles K Black
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引用次数: 0

摘要

背景:AOAC 婴儿配方奶粉和成人营养品利益相关者小组发布了一项关于婴儿配方奶粉中氟测定方法的征集令。标准方法性能要求 (SMPR®) 2014.016 获得批准:完成了氟离子选择电极 (F-ISE) 方法的单实验室验证 (SLV):方法: 对五份粉末样品进行重组,并加入盐酸溶解和释放结合的氟化物。样品包括由牛奶、乳清或大豆制成的婴幼儿和成人营养品,含有完整、部分水解或水解蛋白。加入柠檬酸钠缓冲液以络合任何干扰离子,并调节 pH 值和离子强度。使用 F-ISE 对样品进行为期 6 天的重复分析:根据两条最小二乘(对数拟合)标准曲线(0.02 至 0.1 µg/100 g 或 0.1 至 2.0 µg/100 g)中的一条计算结果。该方法的 LOQ 被确定为 3.3 µg/100 g,远远低于 SMPR 要求的 30 µg/100 g 的最低分析值。氟浓度范围约为 3 至 14 微克/100 克重组粉末,中间精度 RSDr 范围为 0.7 至 12.4%。尽管由于氟含量较低,所有这些结果都超出了 SMPR 的范围,但值得注意的是,氟浓度约为 9 至 14 µg/100 g 的配方的 RSDr 为 0.7% 至 4.3%,而氟浓度达到或低于方法理论检测限的两种配方的 RSDr 仅为 10% 和 12.4%。用 NIST 可追溯标准溶液对三个水平的样品进行添加,回收率在 94% 到 98% 之间,符合 SMPR 标准:结论:F-ISE 方法符合 SMPR 标准,并被采纳为第一行动正式方法(First Action Official MethodSM):本文介绍的氟离子选择电极法经济实惠,易于操作。在样品中加入酸可溶解任何可能与氟结合的矿物质。
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Fluoride Determination in Milk, Soy, and Water-Based Products Using Ion-Selective Electrode and Direct Measurement Technique: Single-Laboratory Validation, First Action 2022.05.

Background: The AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals issued a call for methods for the determination of fluoride in infant formula. Standard Method Performance Requirement (SMPR®) 2014.016 was approved.

Objective: A single-laboratory validation (SLV) of a fluoride ion-selective electrode (F-ISE) method was completed.

Methods: Five powder samples were reconstituted, and hydrochloric acid was added to dissolve and release any bound fluoride. Samples included infant and adult nutritional products made from milk, whey, or soy, containing intact, partially hydrolyzed, or hydrolyzed proteins. Sodium citrate buffer was added to complex any interfering ions and adjust pH and ionic strength. Samples were analyzed in duplicate over 6 days using F-ISE.

Results: Results were calculated based on one of two least-squares (log fit) standard curves (0.02 to 0.1 µg/100 g or 0.1 to 2.0 µg/100 g). The LOQ for the method was determined to be 3.3 µg/100 g, which was far below the minimum analytical value of 30 µg/100 g required in the SMPR. The fluoride concentrations ranged from approximately 3 to 14 µg/100 g reconstituted powder and the intermediate precision, RSDr, ranged from 0.7 to 12.4%. Although all of these results are out of scope for the SMPR due to their low fluoride, it should be noted that the RSDr for formulas with fluoride concentrations ranging from approximately 9 to 14 µg/100 g ranged from 0.7 to 4.3%, and the RSDr for the two formulas with fluoride concentrations at or below the theoretical detection limit of the method were only approximately10 and 12.4%. Recoveries ranged from 94 to 98% for samples spiked at three levels with NIST-traceable standard solutions, meeting the SMPR.

Conclusion: The F-ISE method meets the SMPR and was adopted as a First Action Official MethodSM.

Highlights: The fluoride ion-selective electrode method presented here is affordable and easy to run. The addition of acid to the samples dissolves any minerals which may bind the fluoride.

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来源期刊
Journal of AOAC International
Journal of AOAC International 医学-分析化学
CiteScore
3.10
自引率
12.50%
发文量
144
审稿时长
2.7 months
期刊介绍: The Journal of AOAC INTERNATIONAL publishes the latest in basic and applied research in analytical sciences related to foods, drugs, agriculture, the environment, and more. The Journal is the method researchers'' forum for exchanging information and keeping informed of new technology and techniques pertinent to regulatory agencies and regulated industries.
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