Method validation for determination of 13 elements in honey samples by ICP-MS

Chudzińska, Maria; Debska, Anna; Barałkiewicz, Danuta

doi:10.1007/s00769-011-0812-z

Cited by 45 publications

(35 citation statements)

References 20 publications

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“…Validation of the multianalyte procedure included evaluation of the performance parameters such as limit of detection (LOD), limit of quantification (LOQ), precision (repeatability and within-laboratory reproducibility), recovery and uncertainty [15][16][17][18]. LOD was calculated as three times of standard deviation (LOD = 3s) of relatively low concentration of AAs determined in rye sample and LOQ as six times of the standard deviation (LOQ = 6s, n = 8).…”

Section: Results Calculationmentioning

confidence: 99%

Method validation for determination of amino acids in feed by UPLC

et al. 2017

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The paper presents results of validation of an analytical procedure based on ultra-performance liquid chromatography technique (UPLC) for determination of 17 amino acids in different feeds. The following performance characteristics were determined for the investigated feeds: relative standard deviations of repeatability and intermediate precisions ranged from 0.4 % to 4.6 %, and from 0.8 % to 7.9 %, respectively; recovery rates ranged from 87 % to 104 %, and limit of detection was from 0.06 g kg -1 (methionine) to 0.72 g kg -1 (glutamic acid). Two approaches were used to estimate measurement uncertainty giving values in a range of 5.1 % to 5.5 %. These performance characteristics are in agreement with the values reported in Commission Regulation (EU) No 152/2009 for the ion exchange chromatography with spectrophotometric detection.

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Section: Results Calculationmentioning

confidence: 99%

Method validation for determination of amino acids in feed by UPLC

et al. 2017

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“…The most commonly employed method is to evaluate LOQ as 3 times the LOD [1]. In some papers, LOQ was calculated as 10 times the LOD, 6 or 10 times the standard deviation of the blank sample [24][25][26]. Other authors have estimated LOQ using the standard deviation/slope method described above [27,28].…”

Section: Lod and Loqmentioning

confidence: 99%

“…The advantage of this approach is that it indicates critical control points of the method. Nevertheless, the modelling concept is time consuming and requires an extensive knowledge of the analytical procedure [26,37].…”

Section: Truenessmentioning

confidence: 99%

Speciation analysis of chromium in drinking water samples by ion-pair reversed-phase HPLC–ICP-MS: validation of the analytical method and evaluation of the uncertainty budget

et al. 2013

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The approach presented in this article refers to the modification of a method for the detection and quantitative determination of chromium species in water by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The main aim of this work was to establish a detailed validation of the analytical procedure and an estimation of the budget of measurement uncertainty which was helpful in recognizing the critical points of the presented method. As a result of the method validation experiment, the obtained limit of quantification, repeatability and intermediate precision were satisfied for the quantification Cr(III) and Cr(VI) in water matrices. The trueness of the method was verified via an estimation of the recovery of the spiked real samples. The recovery rate of both determined analytes was found to be between 93 and 115 %. Considering that the validation of the method and the evaluation of measurement uncertainty are crucial for quantitative analysis, the above-mentioned assessment of the uncertainty budget was performed in two different ways: a modelling approach and a single-laboratory validation approach. The measurement uncertainties of the results were found to be 4.4 and 7.8 % for Cr(III), 4.2 and 7.9 % for Cr(VI) using the classical concept and method validation data, respectively. This paper is the first publication to presenting all the steps needed to evaluate the measurement uncertainty for the speciation analysis of chromium species. In summary, the obtained results demonstrate that the method can be applied effectively for its intended use.

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“…Many compounds have MRLs in the range of 0.01-0.05 mg kg . Therefore, the determination of pesticide residues in honey is a challenge, especially because of the low concentration of analytes and large amounts of interfering substances which can be coextracted with analytes, and in most cases, adversely affect analysis results (Chudzinska et al 2012;Kujawski and Namiesnik 2008). Honey contains a large amount of sugars, proteins, amino acids, vitamins, antioxidants, and pigments (Zhou et al 2014;Ferreira et al 2009).…”

Section: Introductionmentioning

confidence: 99%

Liquid Chromatographic MS/MS Analysis of a Large Group of Insecticides in Honey by Modified QuEChERS

2018

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The analytical tool for analysis of pesticide residues in honey must still be improved. Therefore, a sensitive, selective, rapid, and reliable analytical method for the analysis of pesticide residue belonging to 29 different classes at very low concentration levels was developed. Over 130 insecticides were extracted from the honey matrix using different amounts of sample, concentrations of the extraction solvent, and cleanup sorbents. Acceptable extraction recoveries accounting for matrix effect were obtained using the cleanup sorbent combination chitosan/aluminum oxide/C8 (200/200/200 mg) and 1% FA in ACN. Determinations were made by liquid chromatography-tandem mass spectrometry (LC-MS/MS). For most compounds, the recoveries range from 70 to 120%, with relative standard deviations < 20%. Linear correlation coefficients (r2) were higher than 0.99 at concentration levels of 0.001-0.100 mg kg−1. A positive matrix effect was observed for up to 95% of organophosphates and 43% of pyrethroids and a negative effect for 37% of neonicotinoids. This work showed that the presented method is convenient and reliable for quick monitoring of insecticides in honey samples.

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Method validation for determination of 13 elements in honey samples by ICP-MS

Cited by 45 publications

References 20 publications

Method validation for determination of amino acids in feed by UPLC

Method validation for determination of amino acids in feed by UPLC

Speciation analysis of chromium in drinking water samples by ion-pair reversed-phase HPLC–ICP-MS: validation of the analytical method and evaluation of the uncertainty budget

Liquid Chromatographic MS/MS Analysis of a Large Group of Insecticides in Honey by Modified QuEChERS

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