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高效液相色谱-荧光检测法的方法验证及对各种食品中谷氨酸钠的快速测定和高效液相色谱-蒸发光散射检测法(无需衍生化)的方法优化

Method Validation and Rapid Determination of Monosodium Glutamate in Various Food Products by HPLC-Fluorescence Detection and Method Optimization of HPLC-Evaporative Light Scattering Detection Approach without Derivatization.

机构信息

Department of Medical Services and Techniques, Yunus Emre Vocational School of Health Services, Anadolu University, 26470 Eskişehir, Turkey.

Department of Analytical Chemistry, Faculty of Pharmacy, Anadolu University, 26470 Eskişehir, Turkey.

出版信息

J Chromatogr Sci. 2022 Oct 3;60(8):760-769. doi: 10.1093/chromsci/bmab122.

DOI:10.1093/chromsci/bmab122
PMID:34599321
Abstract

In this study, an effective, simple and rapid high-performance liquid chromatography (HPLC) using fluorescence (FLD) method was developed and validated for the determination of monosodium glutamate (MSG) in 57 various food samples. Besides, HPLC-Evaporate Light Scattering Detection (ELSD) method was carried out for determination of MSG without derivatization. MSG analysis was performed by derivatization with dansyl chloride at excitation 328, emission 530nm with fluorescence detector. HPLC-FLD method was carried out by using C18 (150 mm, 4.6 mm, 2.7 μm) column with the mobile phase consisting of (Water: Methanol:Glacial Acetic Acid)/(54:45:1,v/v/v). The column temperature was set at 25°C and the flow rate was set at 0.5 mL min-1 with an injection volume 20 μL. The results were linear (R2 = 0.9999) with very low quantification limits. The applied method was optimized and the validated parameters such as LOD, LOQ, accuracy, precision, linearity and robustness were calculated. The obtained results were statistically compared with each other. The validated HPLC-FLD method was successfully applied for the analysis of MSG in all of the food samples. Moreover, HPLC-ELSD method was optimized and successfully demonstrated for detect the MSG without derivatization.

摘要

本研究建立并验证了一种高效、简单、快速的高效液相色谱(HPLC)-荧光(FLD)法,用于测定 57 种不同食品样品中的谷氨酸单钠(MSG)。此外,还进行了 HPLC-蒸发光散射检测(ELSD)法测定,无需衍生化即可测定 MSG。用荧光检测器在 328nm 激发和 530nm 发射下用丹磺酰氯衍生化进行 MSG 分析。HPLC-FLD 法采用 C18(150mm、4.6mm、2.7μm)柱,流动相为(水:甲醇:冰醋酸)/(54:45:1,v/v/v)。柱温设定为 25°C,流速设定为 0.5mL/min,进样量为 20μL。结果呈线性(R2=0.9999),定量下限非常低。优化了应用方法,并计算了验证参数,如 LOD、LOQ、准确度、精密度、线性和稳健性。对所得结果进行了统计学比较。验证的 HPLC-FLD 方法成功地应用于所有食品样品中 MSG 的分析。此外,还优化了 HPLC-ELSD 法,成功地用于无需衍生化检测 MSG。

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