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食品级盐中亚铁氰化物离子测定的高效液相色谱法的开发与验证

Development and validation of HPLC method for the determination of ferrocyanide ion in food grade salts.

作者信息

Soo Lim Ho, Young Hwang Ju, Choi EunA, Lee Gunyoung, Sun Yoon Sang, Kim MeeKyung

机构信息

Food Additives and Packaging Division, Ministry of Food and Drug Safety, Cheongju, Chungcheongbuk-do 28159, Republic of Korea.

Food Additives and Packaging Division, Ministry of Food and Drug Safety, Cheongju, Chungcheongbuk-do 28159, Republic of Korea.

出版信息

Food Chem. 2018 Jan 15;239:1167-1174. doi: 10.1016/j.foodchem.2017.07.070. Epub 2017 Jul 15.

Abstract

A rapid, simple, and reliable HPLC method was developed and validated to determine the presence of ferrocyanide ions (FeCNs) in food grade salts. An analytical column coupled with a guard column and mobile phase comprised of sodium perchlorate and sodium hydroxide (NaOH) were employed at a detection wavelength of 221nm. Samples were dissolved in 0.02M NaOH solution and filtered. For processed salts including herbs and spices, a C cartridge was applied to minimize interference from salt matrices. The method validation was based on linearity, accuracy (recovery), precision, LOD, LOQ, and measurement uncertainty. This method exhibits good linearity from 0.1-10mg/L (r=0.9999). The LOD and LOQ values were determined to be 0.02 and 0.07mg/kg, respectively. The FeCN recoveries in six salt matrices ranged from 80.3-102.2% (RSD=0.3-4.4%). These results indicate that the proposed method is suitable for FeCN ion determination in various food grade salts.

摘要

开发并验证了一种快速、简单且可靠的高效液相色谱法,用于测定食品级盐中亚铁氰化物离子(FeCNs)的含量。采用一根分析柱与一根保护柱联用,流动相由高氯酸钠和氢氧化钠(NaOH)组成,检测波长为221nm。将样品溶解于0.02M NaOH溶液中并过滤。对于包括草药和香料在内的加工盐,使用C柱以尽量减少盐基质的干扰。方法验证基于线性、准确度(回收率)、精密度、检测限、定量限和测量不确定度。该方法在0.1 - 10mg/L范围内呈现良好的线性(r = 0.9999)。检测限和定量限分别确定为0.02和0.07mg/kg。六种盐基质中的FeCN回收率在80.3 - 102.2%之间(相对标准偏差 = 0.3 - 4.4%)。这些结果表明,所提出的方法适用于各种食品级盐中FeCN离子的测定。

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