高效液相色谱法测定面粉及面粉处理剂中新型非法添加剂

引用本文: 国振, 周霞, 赵博, 赵光亮, 李先江, 李秀琴, 张庆合. 高效液相色谱法测定面粉及面粉处理剂中新型非法添加剂[J]. 分析化学, 2021, 49(4): 504-511. doi: 10.19756/j.issn.0253-3820.201632 shu

Citation: GUO Zhen, ZHOU Xia, ZHAO Bo, ZHAO Guang-Liang, LI Xian-Jiang, LI Xiu-Qin, ZHANG Qing-He. Determination of New Illegal Additives in Wheat Flour and Flour Treatment Agent by High Performance Liquid Chromatography[J]. Chinese Journal of Analytical Chemistry, 2021, 49(4): 504-511. doi: 10.19756/j.issn.0253-3820.201632 shu

高效液相色谱法测定面粉及面粉处理剂中新型非法添加剂

中国计量科学研究院化学计量与分析科学研究所北京 100029

通讯作者: 李秀琴,E-mail:lixq@nim.ac.cn

基金项目:
国家市场监督管理总局技术保障专项项目（No.2020YJ040）资助。

摘要: 建立了同时检测面粉及面粉处理剂中4种非法添加剂（曲酸、苯甲羟肟酸、噻二唑和噻苯咪唑）的高效液相色谱-二极管阵列检测器（High performance liquid chromatography-diode array detector，HPLC-DAD）定量分析方法。样品经甲醇提取后，采用C₁₈色谱柱分离、甲醇-0.01% H₃PO₄溶液梯度洗脱、二极管阵列检测器检测，以外标法进行定量分析。对色谱条件和前处理方法进行了优化，考察了流动相组成对分离度的影响，以及提取溶剂种类、提取方式等对提取效率的改善。结果表明，4种非法添加剂在0.1~2.0 μg/mL范围内线性关系良好（R²≥0.9998），方法检出限（S/N≥3）介于0.3~0.7 mg/kg之间，3个浓度水平的加标回收率为80.8%~95.9%，相对标准偏差为0.5%~4.9%（n=6）。本方法操作简便、净化效果好、准确度高，适用于面粉及面粉处理剂中非法添加剂的筛查和检测。

关键词:

English

Determination of New Illegal Additives in Wheat Flour and Flour Treatment Agent by High Performance Liquid Chromatography

Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China

Corresponding author: LI Xiu-Qin, lixq@nim.ac.cn

Received Date: 29 October 2020
Revised Date: 19 February 2021
Fund Project:
Supported by the Special Project of State Administration for Market Regulation for Technical Support (No.2020YJ040).

Abstract: A method for determination of four kinds of illegal additives kojic acid, benzodiazepine acid, 2-mercapto-5-methyl-1,3,4-thiadiazole and thiabendazole in wheat flour and flour treatment agent was developed by using high performance liquid chromatography (HPLC). The sample was first extracted with methanol. Then the analytes were separated on a ZORBAX Eclipse Plus C₁₈ column, separated by gradient elution with methanol and 0.01% H₃PO₄ aqueous solution, detected by diode array detector, and quantified by external standard method. The chromatographic conditions and pretreatment methods were optimized. Effects of several important factors, including influence of mobile phase composition on separation degree and the improvement of extraction efficiency by different extraction solvents, were investigated to acquire optimum conditions. The results showed that the 4 kinds of illegal additives had good linear relationship in the concentration range of 0.1-2.0 μg/mL (R² ≥ 0.9998). The limits of detection (LODs, S/N ≥ 3) for the 4 kind of illegal additives were 0.3-0.7 mg/kg, and the recoveries in wheat flour and flour treatment agent were 80.8%-95.9% at 3 spiking levels with the relative standard deviations (RSDs) of 0.5%-4.9% (n=6). This method was simple, accurate, and had good purification effect, which was suitable for the screening and determination of illegal additives in wheat flour and flour treatment agent.

Key words:

Wheat flour
/ Flour treatment agent
/ High performance liquid chromatography
/ Kojic acid
/ Benzohydroxamic acid
/ 2-Mercapto-5-methyl-1,3,4-thiadiazole
/ Thiabendazole

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沈阳化工大学材料科学与工程学院沈阳 110142

高效液相色谱法测定面粉及面粉处理剂中新型非法添加剂

通讯作者: 李秀琴,E-mail:lixq@nim.ac.cn

English

Determination of New Illegal Additives in Wheat Flour and Flour Treatment Agent by High Performance Liquid Chromatography

Corresponding author: LI Xiu-Qin, lixq@nim.ac.cn

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高效液相色谱法测定面粉及面粉处理剂中新型非法添加剂

通讯作者: 李秀琴,E-mail:lixq@nim.ac.cn

English

Determination of New Illegal Additives in Wheat Flour and Flour Treatment Agent by High Performance Liquid Chromatography

Corresponding author: LI Xiu-Qin, lixq@nim.ac.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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