Sensitive determination of domoic acid in shellfish by on-line coupling of weak anion exchange solid-phase extraction and liquid chromatography–diode array detection–tandem mass spectrometry

Regueiro, Jorge; Martín-Morales, Eva; Álvarez, Gonzalo; Blanco, Juan

doi:10.1016/j.foodchem.2011.05.004

Cited by 21 publications

(8 citation statements)

References 22 publications

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“…Our MDL was very similar to the value (6 ng g −1 ) obtained with the less selective fluorimetric method [ 9 ]. Our MDL value was higher than the value (0.28 ng g −1 ) reported by Regueiro et al [ 15 ] through a one-line SPE step. We have proposed a simpler and cheaper procedure with high sensitivity and selectivity using a LC-MS/MS system.…”

Section: Resultscontrasting

confidence: 90%

“…In the literature, one of the main problems in the DA determination of mussel samples is the matrix effect and a labor-intensive anion exchange solid phase extraction is usually carried out for an efficient sample cleanup [ 13 , 14 ]. Regueiro et al [ 15 ] developed an online purification method coupled to LC-MS analysis, minimizing the matrix 2 effect and with a preconcentration of samples.…”

Section: Introductionmentioning

confidence: 99%

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Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue

Barbaro

Zangrando

Barbante

et al. 2016

The Scientific World Journal

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Domoic acid (DA), a neurotoxic amino acid produced by diatoms, is the main cause of amnesic shellfish poisoning (ASP). In this work, we propose a very simple and fast analytical method to determine DA in mussel tissue. The method consists of two consecutive extractions and requires no purification steps, due to a reduction of the extraction of the interfering species and the application of very sensitive and selective HILIC-MS/MS method. The procedural method was validated through the estimation of trueness, extract yield, precision, detection, and quantification limits of analytical method. The sample preparation was also evaluated through qualitative and quantitative evaluations of the matrix effect. These evaluations were conducted both on the DA-free matrix spiked with known DA concentration and on the reference certified material (RCM). We developed a very selective LC-MS/MS method with a very low value of method detection limit (9 ng g−1) without cleanup steps.

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Section: Resultscontrasting

confidence: 90%

Section: Introductionmentioning

confidence: 99%

Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue

Barbaro

Zangrando

Barbante

et al. 2016

The Scientific World Journal

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“…Solid-phase extraction (SPE) is a common method that is usually extensively applied in sample preparation before the quantitative analysis of the target analytes. The commercially available SPE phases used for the cleanup in DA assay include reversed phase C 18 [ 24 ], strong or weak anion exchange [ 25 , 26 ] and strong cation-exchange cartridges [ 27 ]. In addition, some references have reported using sol-gel amorphous titania (TiO 2 ), molecularly-imprinted polymer as the solid phase sorbents for the extraction of DA from several matrices [ 28 , 29 ].…”

Section: Introductionmentioning

confidence: 99%

A Rapid LC-HRMS Method for the Determination of Domoic Acid in Urine Using a Self-Assembly Pipette Tip Solid-Phase Extraction

Zhang

Chen

Hong

2015

Toxins

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In this study, we developed a self-assembly pipette tip solid-phase extraction (PTSPE) method using a high molecular weight polymer material (PAX) as the adsorbent for the determination of domoic acid (DA) in human urine samples by liquid chromatography high-resolution mass spectrometry (LC-HRMS) analysis. The PTSPE cartridge, assembled by packing 9.1 mg of PAX as sorbent into a 200 μL pipette tip, showed high adsorption capacity for DA owing to the strong cationic properties of PAX. Compared with conventional SPE, the PTSPE is simple and fast, and shows some advantages in the aspects of less solvent consumption, low cost, the absence of the evaporation step, and short time requirement. All the parameters influencing the extraction efficiency such as pH, the amount of sorbent, the number of aspirating/dispensing cycles, and the type and volume of eluent in PTSPE were carefully investigated and optimized. Under the optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) values of DA were 0.12 μg/L and 0.37 μg/L respectively. The extraction recoveries of DA from the urine samples spiked at four different concentrations were in a range from 88.4% to 102.5%. The intra- and inter-day precisions varied from 2.1% to 7.6% and from 2.6% to 12.7%, respectively. The accuracy ranged from −1.9% to −7.4%.

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“…In Table 4, a comprehensive comparison of the proposed method with other existing methods for DA determination was summarized in term of extraction, clean-up, LOD, linear range and recovery. Zhang et al [22] proposed an MSPE method for LC-MS/MS analysis of DA in shellfish samples by synthesizing Fe 3 O 4 ·SiO 2 ·UiO-66 magnetic microspheres, and Regueiro et al [37] utilized online coupling of weak anion exchange SPE and LC-UV-MS/MS to realize sensitive determination of DA in shellfish. Though LODs of the analyte in these two studies were reported at the level of pg·g −1 and sub ng·g −1 , respectively, linear ranges constructed in the corresponding methods both fell outside of the one regulated by Codex Stan 292-2008.…”

Section: Resultsmentioning

confidence: 99%

Development and Application of Immunoaffinity Column Purification and Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Domoic Acid in Shellfish

Chen

Zhang

Yan

et al. 2019

Toxins

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Domoic acid (DA) is a neurotoxin associated with amnesic shellfish poisoning (ASP). Though LC coupled to tandem mass spectrometry (LC-MS/MS) has become the preferred method for DA determination, traditional sample pretreatment is still labor-intensive. In this study, a simple, efficient and selective method for LC-MS/MS analysis of DA in shellfish was established by optimizing clean-up procedures on a self-assembly immunoaffinity column (IAC). Shellfish was extracted with 75% methanol twice and diluted with phosphate buffered saline (PBS, 1:2). The mixture was purified on IAC as follows: preconditioned with PBS, loaded with sample, washed by 50% MeOH, and eluted with MeOH containing 2% ammonium hydroxide. Concentrated analyte was monitored by multiple reaction monitoring (MRM) using electrospray (ESI) positive ion mode throughout the LC gradient elution. Based on the post-extraction addition method, matrix effects for various shellfish matrices were found to be less than 8%. The developed method was fully validated by choosing mussel as the representative matrix. The method had a limit of detection (LOD) of 0.02 µg·g−1, showed excellent linear correlation in the range of 0.05–40 µg·g−1, and obtained ideal recoveries (91–94%), intra-day RSDs (6–8%) and inter-day RSDs (3–6%). The method was successfully applied to DA determination in 59 shellfish samples, with a detection rate of 10% and contaminated content of 0.1–14.9 µg·g−1.

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Sensitive determination of domoic acid in shellfish by on-line coupling of weak anion exchange solid-phase extraction and liquid chromatography–diode array detection–tandem mass spectrometry

Cited by 21 publications

References 22 publications

Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue

Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue

A Rapid LC-HRMS Method for the Determination of Domoic Acid in Urine Using a Self-Assembly Pipette Tip Solid-Phase Extraction

Development and Application of Immunoaffinity Column Purification and Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Domoic Acid in Shellfish

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