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Rapid determination of nitrite in foods in acidic conditions by high-performance liquid chromatography with fluorescence detection

机译:高效液相色谱-荧光检测法快速测定酸性条件下的食品中亚硝酸盐

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摘要

In this study, a simple, rapid, and sensitive method for the determination of nitrite (NO2-) in food samples by high-performance liquid chromatography with fluorescence detection in acidic conditions had been developed. The derivatization of the nitrite with 2,3-diaminonaphthalene was performed in acidic conditions to yield the highly fluorescent 2,3-naphthotriazole, which was directly analyzed by high-performance liquid chromatography with fluorescence detection without adjusting the solution to alkaline. The analysis column was reversed-phase C-8 column. A constant flow rate of 1.0 mL/min was employed using water/acetonitrile as the mobile phase in isocratic mode (70: 30, v/v). Fluorescence was monitored with excitation at 375 nm and emission at 415 nm. The standard calibration curves were linear for nitrite in different matrixes in the concentration range of 0-100 mu g/L, and the correlation coefficients ranged from 0.9978 to 0.9998. The limits of detection and quantification were in the ranges of 0.012-0.060 and 0.040-0.20 mg/kg, respectively. The recoveries of nitrite from samples spiked at three different concentrations were 74.0-113.2%, and the relative standard deviations of the recovery results (n = 6) were 1.67-10.8%. The proposed method has good repeatability and is very sensitive and simple. It has been successfully used to determine nitrite in foods.
机译:在这项研究中,开发了一种简单,快速,灵敏的方法,通过在酸性条件下通过荧光检测的高效液相色谱法测定食品样品中的亚硝酸盐(NO2-)。在酸性条件下用2,3-二氨基萘将亚硝酸盐衍生化,得到高荧光的2,3-萘三唑,将其直接通过高效液相色谱仪进行荧光检测,无需检测溶液是否为碱性即可进行分析。分析柱为反相C-8柱。以水/乙腈为流动相,以等度模式(70:30,v / v)使用1.0 mL / min的恒定流速。用375nm的激发和415nm的发射监测荧光。在0-100μg / L的浓度范围内,在不同基质中亚硝酸盐的标准校准曲线是线性的,相关系数范围为0.9978至0.9998。检测限和定量限分别在0.012-0.060和0.040-0.20 mg / kg的范围内。三种不同浓度加标样品中亚硝酸盐的回收率为74.0-113.2%,回收率的相对标准偏差(n = 6)为1.67-10.8%。所提出的方法具有良好的重复性,并且非常灵敏和简单。它已成功用于测定食品中的亚硝酸盐。

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