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冷冻辅助糖析液液萃取结合 LC-MS/MS 定量测定蜂蜜中的高氯酸盐。

Freezing-assisted sugaring-out liquid-liquid extraction coupled with LC-MS/MS for quantitative determination of perchlorate in honey.

机构信息

Yunnan Center for Disease Control and Prevention, 158 Dongsi Street, Xishan District, Kunming 650022,China.

Yunnan Center for Disease Control and Prevention, 158 Dongsi Street, Xishan District, Kunming 650022,China; College of Public Health, Dali University, Dali 671000, China.

出版信息

Food Chem. 2024 Mar 1;435:137604. doi: 10.1016/j.foodchem.2023.137604. Epub 2023 Sep 28.

Abstract

For the first time, a simple, quick, sensitive, and low cost method for quantification of perchlorate in honey using liquid chromatography-tandem mass spectrometry was developed. Through freezing-assisted sugaring-out liquid-liquid extraction, one-step simultaneous extraction and clean-up of perchlorate from honey were perfectly achieved. Glucose and fructose, the most abundant sugars in honey, were almost completely removed from the extract without use of any clean-up materials. Under optimum conditions, the proposed approach exhibited satisfactory linearity, negligible matrix effects, and low detection limit of 0.05 µg/kg, providing recoveries of 96.7 %-102.3 % with relative standard deviation of < 9 % for honey samples. The validated method was applied to the analysis of perchlorate in 36 honey samples, and detection rate was 94.4 %. This work provided a simple and reliable method for extensive monitoring of perchlorate in honey and opened- up new insights for analysis of contaminants in honey matrixes.

摘要

首次开发了一种简单、快速、灵敏且低成本的方法,可使用液相色谱-串联质谱法定量蜂蜜中的高氯酸盐。通过冷冻辅助加糖液-液萃取,可从蜂蜜中一步同时提取和净化高氯酸盐。无需使用任何净化材料,就可将蜂蜜中最丰富的两种糖,葡萄糖和果糖,几乎完全从提取物中去除。在最佳条件下,所提出的方法表现出令人满意的线性、可忽略的基质效应和低检测限(0.05μg/kg),对蜂蜜样品的回收率为 96.7%-102.3%,相对标准偏差<9%。该经验证的方法已应用于 36 个蜂蜜样品中高氯酸盐的分析,检测率为 94.4%。这项工作为广泛监测蜂蜜中的高氯酸盐提供了一种简单可靠的方法,并为蜂蜜基质中污染物的分析开辟了新的思路。

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