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半制备整体柱液相色谱法测定食品中泛酸的含量

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目的:建立半制备整体柱液相色谱法测定食品中泛酸含量的分析方法.方法:样品中泛酸用热水提取,以磷酸二氢钾溶液和乙腈为流动相,流速 2 mL·min-1,进样量 500 μL,柱温 30℃,检测波长200 nm,经Merck半制备整体柱净化,在泛酸出峰处收集溶液,收集液经反相C18 柱定量分析.结果:泛酸浓度在 0.001~0.032 μg·L-1 具有良好的线性关系,相关系数为0.999 9,方法检出限为0.025 mg/100 g,定量限为0.08 mg/100 g,泛酸在食品中测定结果的相对标准偏差为2.4%~3.6%,加标回收率均大于90%.结论:针对含有蛋白、肽、淀粉等复杂基质的食品,本半制备整体柱液相色谱法的检测一致性较好,分离度、精密度、准确性等均符合要求.有效解决复杂基质、杂质干扰下目标峰难分离、检测结果不稳定、平行差的问题.
Determination of Pantothenic Acid in Food by Semi-Preparative Monolithic Column Liquid Chromatography
Objective:To establish.an analytical method for the determination of pantothenic acid content in food using semi-preparative monolithic column liquid chromatography.Method:Pantothenic acid in the sample is extracted with hot water,using a solution of potassium dihydrogen phosphate and acetonitrile as the mobile phase,with a flow rate of 2 mL·min-1,an injection volume of 500 μL,a column temperature of 30℃,and a detection wavelength of 200 nm.The solution is purified on a Merck semi-preparative monolithic column,and the solution is collected at the elution peak of pantothenic acid.The collected liquid is then quantitatively analyzed on a reverse-phase C18 column.Result:Pantothenic acid exhibits good linearity within the concentration range of 0.001~0.032 μg·L-1,with a correlation coefficient of 0.999 9.The limits of detection is 0.025 mg/100 g,and limits of quantification is 0.08 mg/100 g.The relative standard deviation of the pantothenic acid determination results in food is between 2.4%and 3.6%.The recovery rates of spiked samples are greater than 90%.Conclusion:For foods containing complex matrices such as proteins,peptides,and starch,this semi-preparative monolithic column liquid chromatography method demonstrates good consistency in detection,with separation,precision,and accuracy all meeting the necessary standards.It effectively addresses issues such as difficult peak separation,unstable detection results and poor parallelism under complex matrices and impurity interference.

high performance liquid chromatographypantothenic acidsemi-preparative monolithic column

陈汉峰、杨静、黎俊威、侯少平、刘春丽

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捷通(广州)检测技术服务有限公司,广东 广州 510730

高效液相色谱 泛酸 半制备整体柱

2024

食品安全导刊
商业科技质量中心 北京肉类食品协会

食品安全导刊

影响因子:0.065
ISSN:1674-0270
年,卷(期):2024.(31)