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高效液相色谱-电感耦合等离子体质谱法测定鱼油及鱼油胶囊中的无机砷。

Determination of Inorganic Arsenic in Fish Oil and Fish Oil Capsules by LC-ICP-MS.

机构信息

Japan Food Research Laboratories, 6-11-10 Nagayama, Tama, Tokyo, Japan, 206-0025.

National Fisheries University, 2-7-1 Nagatahonmachi, Shimonoseki, Yamaguchi, Japan, 759-6595.

出版信息

J AOAC Int. 2021 May 21;104(2):397-403. doi: 10.1093/jaoacint/qsaa135.

DOI:10.1093/jaoacint/qsaa135
PMID:33017005
Abstract

BACKGROUND

As inorganic arsenic is a highly toxic compound, its concentration in foods should be determined.

OBJECTIVE

Develop an analytical method for determining inorganic arsenic in fish oil and fish oil capsules.

METHOD

Inorganic arsenic was extracted from fish oil by heating at 80°C in 1.6% tetramethylammonium hydroxide-ethanol. The concentration of inorganic arsenic in fish oil was determined by liquid chromatography (LC) inductively coupled plasma (ICP) MS using an octadecylsilane (ODS) column with a mobile phase containing an ion-pair reagent.

RESULTS

The LOD (0.005, 0.004 mg/kg), LOQ (0.016, 0.011 mg/kg), repeatability (4.2, 3.5%), intermediate precision (5.4, 3.5%), and trueness (recoveries 94-109% based on spiked samples) of the proposed method were satisfactory for inorganic arsenic in fish oil and fish oil capsules. A low level of inorganic arsenic was detected only in anchovy oil among all fish oil samples that were used in this study. Inorganic arsenic levels were below the quantitation limit in all fish oil capsules.

CONCLUSIONS

Inorganic arsenic was determined after extraction from fish oil by heating at 80°C in 1.6% tetramethylammonium hydroxide-ethanol. The level of inorganic arsenic in all fish oil samples examined in this study was lower than 0.1 mg/kg of the maximum level defined in the Codex.

HIGHLIGHTS

Arsenic speciation in fish oil and fish oil capsules was analyzed by LC-ICP-MS using an ODS column with a mobile phase containing an ion-pair reagent. A low level of inorganic arsenic was detected only in anchovy oil. No inorganic arsenic was detected in fish oil capsules.

摘要

背景

由于无机砷是一种剧毒化合物,因此应测定其在食品中的浓度。

目的

建立一种测定鱼油和鱼油胶囊中无机砷的分析方法。

方法

将鱼油在 80°C 下用 1.6%四甲基氢氧化铵-乙醇加热提取无机砷。采用含离子对试剂的流动相的十八烷基硅烷(ODS)柱通过液相色谱(LC)-电感耦合等离子体质谱(ICP-MS)法测定鱼油中的无机砷浓度。

结果

该方法对鱼油和鱼油胶囊中无机砷的检出限(0.005、0.004mg/kg)、定量限(0.016、0.011mg/kg)、重复性(4.2%、3.5%)、中间精密度(5.4%、3.5%)和准确度(基于加标样品的回收率为 94%-109%)均令人满意。在所研究的所有鱼油样品中,仅在凤尾鱼油中检测到低水平的无机砷。所有鱼油胶囊中的无机砷含量均低于法规规定的限量。

结论

通过在 80°C 下用 1.6%四甲基氢氧化铵-乙醇加热从鱼油中提取无机砷后进行测定。在所研究的所有鱼油样品中,无机砷的水平均低于法规规定的限量 0.1mg/kg。

重点

采用含离子对试剂的流动相的 ODS 柱通过 LC-ICP-MS 法分析鱼油和鱼油胶囊中的砷形态。仅在凤尾鱼油中检测到低水平的无机砷。在鱼油胶囊中未检测到无机砷。

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