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液相色谱-串联质谱法快速测定液态奶、奶粉、婴儿配方奶粉和乳基营养产品中生物素和叶酸的方法

A Rapid Method for the Determination of Biotin and Folic Acid in Liquid Milk, Milk Powders, Infant Formula, and Milk-Based Nutritional Products by Liquid Chromatography-Tandem Mass Spectrometry.

作者信息

Gill Brendon D, Saldo Sheila, Wood Jackie E, Indyk Harvey E

机构信息

Fonterra Cooperative Group Ltd, PO Box 7, Waitoa 3341, New Zealand.

出版信息

J AOAC Int. 2018 Sep 1;101(5):1578-1583. doi: 10.5740/jaoacint.18-0065. Epub 2018 May 31.

DOI:10.5740/jaoacint.18-0065
PMID:29852890
Abstract

BACKGROUND

Biotin and folate are B-group vitamins that play a critical role in numerous metabolic reactions, and they are supplemented to infant and adult nutritional formulas as free biotin and folic acid.

OBJECTIVE

We describe a rapid method for the analysis of biotin and folic acid that is applicable to liquid milk, milk powders, infant formula, and milk-based nutritional products.

METHODS

Samples are autoclaved, centrifuged, filtered, and analyzed by HPLC-MS/MS, with quantitation accomplished by the internal standard technique.

RESULTS

The method was shown to be accurate, with acceptable spike recovery (biotin: 96.5-108.2%; folic acid: 92.6-104.4%), and no bias (α = 0.05) against either a certified reference material (biotin: P = 0.70; folic acid: P = 0.23) or established analytical method (biotin: P = 0.10; folic acid: P = 0.48) was found. Acceptable precision was confirmed with repeatability relative standard deviation (RSDr) and Horwitz ratio (HorRat) values (biotin: RSDr = 0.5-5.6%, HorRatr = 0.1-0.6; folic acid: RSDr = 2.0-3.1%, HorRatr = 0.3-0.5). Method detection limit and ruggedness experiments further demonstrated the suitability of this method for routine compliance testing.

CONCLUSIONS

This rapid method is intended for use in high-throughput laboratories as part of the routine product compliance release testing of biotin and folic acid in the manufacturing of infant formulas and adult nutritional products.

摘要

背景

生物素和叶酸是B族维生素,在众多代谢反应中起关键作用,它们以游离生物素和叶酸的形式添加到婴儿和成人营养配方食品中。

目的

我们描述了一种适用于液态奶、奶粉、婴儿配方食品和乳基营养产品的生物素和叶酸快速分析方法。

方法

样品经高压灭菌、离心、过滤后,采用高效液相色谱-串联质谱法(HPLC-MS/MS)进行分析,通过内标技术进行定量。

结果

该方法被证明是准确的,加标回收率可接受(生物素:96.5-108.2%;叶酸:92.6-104.4%),并且相对于有证标准物质(生物素:P = 0.70;叶酸:P = 0.23)或既定分析方法(生物素:P = 0.10;叶酸:P = 0.48)均无偏差(α = 0.05)。通过重复性相对标准偏差(RSDr)和霍维茨比率(HorRat)值确认了可接受的精密度(生物素:RSDr = 0.5-5.6%,HorRatr = 0.1-0.6;叶酸:RSDr = 2.0-3.1%,HorRatr = 0.3-0.5)。方法检出限和耐用性实验进一步证明了该方法适用于常规合规性检测。

结论

这种快速方法旨在用于高通量实验室,作为婴儿配方食品和成人营养产品生产中生物素和叶酸常规产品合规性放行检测的一部分。

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