Total Arsenic and Arsenic Species Determination in

Overview

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Key numbers

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measurements. Both procedures were characterized by short-term and long-term precision: 2.2%
(TAs) up to 4.2% (AsB), and 3.6% (TAs) up to 7.2% (DMA), respectively. Limits of detection (LD ) were
in the range from 0.056 µg L−1 for TAs to 0.15 µg L−1 for As(V). Obtained recoveries were in the
range of 85%–116%. Developed methods were applied to freshwater fish samples analysis.
are presented in Table 1 They indicate that the best mode for TAs determination is to monitor 91 AsO+
Table 1. Total arsenic concentration in certified reference materials of Tuna Fish Tissue BCR-627 and
91 AsO+ ion with use of DRC without an internal standard (Table 2). Therefore, in subsequent studies
arsenic was determined as 91 AsO+ with DRC. Significantly better recoveries, ranging from 92% to
99% for all used CRMs, were obtained when the samples were extracted with water in comparison to
There are reports in the literature that extraction efficiency of As species are much less than 100%,
often in the range of 40%–60% when anion-exchange column was used (5,25,26), or 16%–42% for
Table 2. Total arsenic concentration in certified reference materials of Tuna Fish Tissue BCR 627 and
Herring Tissue MODAS-3 in extracted samples (n = 3).
The calibration curve for TAs was constructed in the concentration range of 0.2 µg L−1 to
were equal to 2.2% and 3.6%, respectively. To evaluate the trueness of the method, the following
significant differences between these values. The Student’s t-test at a 95% confidence level showed
Table 3. Characteristics of developed analytical procedures for total arsenic and arsenobetaine,
range of 0.5 µg L−1 to 10 µg L−1 . Chromatographic separation obtained for analytes in standards in
mentioned concentration ranges is presented in the Figure 2. Three independent solutions of calibration
the same way as for TAs. Short-term repeatability was in the range of 3.3% to 4.2% and long-term
repeatability was in the range of 4.2% to 7.2%. Due to the unavailability of certified reference materials
of 3.3% to 4.2% and long-term repeatability was in the range of 4.2% to 7.2%. Due to the
calibration curves) in the range of: 0.5 µg L to 10.0 µg L obtained using a mixture of 10 mmol
Table 4. Results for As species in certified reference material presented as the average and standard
different CRM are shown in Table 3. in order to determine AsB concentration. The results for As
species determination in different CRM are shown in Table 3.
contained AsB. A trace amount of As(V) was stated; this form comprised from 0.72% to 3.34% of
Table 5. Concentration of total arsenic and arsenic species in selected freshwater fish samples from Wielkopolska and Lower Silesia provinces (n = 3).
an arsenic contaminated lake in Pakistan in the concentration range from 1.19 µg g−1 to 2.05 µg g−1
(58%–96% of all As species in methanol/water extract) with traces of DMA, TMAO, and arseno-sugars,
from Xiang River in China, with a mean concentration of TA in fish muscle equal to 0.75 µg g−1 (12).
authors reported a large percentage of non-extractable As species, contributing more than 50% of the
range 0.2–0.3, which is an important and positive conclusion form the point of view of the general
Ontario, Canada). The HPLC and ICP-MS operating conditions are presented in Table 6.
Table 6. Optimization parameters for separation and determination of TAs and AsB, As(III), DMA,
Christiansburg, Virginia, USA). DMA (a purity of 99%), MMA prepared from monosodium acid
methane arsonate sesquihydrate (a purity of 98.5%), and AsB (a purity of 95%) were purchased from
Ammonium phosphate dibasic (a purity of 99.9999%), ammonium nitrate (a purity of 99.999%),
were used as mobile phase components. Methanol HPLC Gradient Grade with a purity of 99.8% used
Sodium hydroxide pellets (used as a 30% solution), Suprapur ammonia solution of 25% (v/v), and
Suprapur nitric acid of 65% (v/v) used for pH adjustment were purchased from Merck (Darmstadt,
Concentrated nitric acid (65% HNO3 Suprapur, Merck, Germany) and hydrogen peroxide

Methods (brief)

Freshwater Fish by ICP-DRC-MS and
HPLC/ICP-DRC-MS Techniques
(arsenite—As(III), arsenate—As(V), monomethylarsenic acid—MMA, dimethylarsenic acid—DMA
and arsenobetaine—AsB) in freshwater fish samples were developed. Inductively coupled
plasma mass spectrometry with dynamic reaction cell (ICP-DRC-MS) and high-performance liquid
chromatography hyphenated to ICP-DRC-MS were used for TAs and arsenic species determination,
respectively. The DRC with oxygen as a reaction gas was used. Sample preparation, digestion, and
extraction were optimized. Microwave assisted digestion and extraction provided good recovery
(TAs) up to 4.2% (AsB), and 3.6% (TAs) up to 7.2% (DMA), respectively. Limits of detection (LD ) were
range of 85%–116%. Developed methods were applied to freshwater fish samples analysis.
Keywords: arsenic; speciation; freshwater fish; ICP-DRC-MS; HPLC/ICP-DRC-MS
arsenic speciation analysis in seawater samples, which is extensively researched and attracts greater
Some papers report less concentration of total arsenic (TAs) in freshwater fish samples, while some
freshwater fish samples, AsB is a major species, however, others suggest that freshwater fish may be a
In order to distinguish differences in the toxicity, which demonstrate the investigated samples, it
information about the toxicity of the sample. In the context of food analysis, determination of toxic
methylacids, such as MMA and dimethylarsenic acid (DMA), is essential. It is also important to
to MMA and DMA may result in gastrointestinal, kidney, and bladder damage (11). The sources of

Implications

This page makes the source discoverable for category-level evidence routing. Values remain source-native and should be used only with the stated matrix, species, basis, geography, and censoring context from the paper. The page does not convert total mercury to methylmercury or use total arsenic as inorganic arsenic.

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Update history

The five most recent substantive edits to this page, classified major (evidence or structure moved), correction (a published value or statement was wrong and has been fixed), or minor (narrative rewritten without changing the underlying evidence). Each description is derived from what the edit did to this page; the linked commit is the authoritative record, routine regeneration passes are excluded, and the full version history lives in git. When DOI minting comes online (see schema docs), each entry below will also link to a version-pinned DataCite DOI.

Commit	Date	Change	Description
b01ec52c	2026-08-04	major	2 sections added
d49e450f	2026-08-03	major	5 sections added; narrative text revised