Direct Determination of Major and Trace Elements in Milk by Inductively Coupled Plasma Atomic Emission and Mass Spectrometry

Nóbrega, Joaquim A.; Gélinas, Yves; Krushevska, Antoaneta; Barnes, Ramon M.

doi:10.1039/a607492h

Cited by 70 publications

(26 citation statements)

References 11 publications

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“…For Ca ( Figure 4B) and Mg ( Figure 4C), the smaller volume of the reagent showed higher signals. In this study we show that small amounts of TMAH are needed in the sample solubilization, which is consistent with the predicted by Matusiewicz et al 4 and Nobrega et al 21 Thus, targeting a lower reagent consumption and consequently a smaller waste generation, the TMAH volume of 100 µL was fixed. Therefore, the optimal condition for the alkaline solubilization was: 500 mg of sample in the presence of 100 µL TMAH.…”

Section: Experimental Designsupporting

confidence: 77%

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Use of MIP OES and F AAS/AES for determination of Ca, K, Na and Mg in brazilian cream cheese

et al. 2017

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publicado na web em 15/05/2017 In this work, two sample preparation procedures for subsequent determination of Na, K, Ca and Mg by techniques of atomic spectrometry in samples of Brazilian cream cheese were evaluated. The determinations were performed on two equipments, F AAS and MIP OES, which presented similar results, being evident the advantages of MIP OES since it is a multielementar technique with low operational cost and high efficiency. The first procedure was carried out by acidic decomposition (HNO 3 /H 2 SO 4 ) in a reflux system, and the second used the alkaline solubilization with tetramethylammonium hydroxide. The accuracy was verified by recovery tests and the results were between 80 and 104% for both procedures. A comparison with a reference procedure was also performed and no significant differences have been observed at the 95% confidence level. The evaluated elements were not in accordance with the values indicated on the labels of all products, showing the importance for monitoring these products. The methods of sample preparation proposed showed to be simple, inexpensive, providing accurate and precise results, and are a promising alternative to be used for the quality control of these routine test samples.

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Section: Experimental Designsupporting

confidence: 77%

“…20 and Nobrega et al. 21 used the solubilization with TMAH in milk samples for determination of various elements by ICP OES and ICP MS.…”

Section: -13mentioning

confidence: 99%

Use of MIP OES and F AAS/AES for determination of Ca, K, Na and Mg in brazilian cream cheese

et al. 2017

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“…Nobrega et al (1997) tested the direct analysis of milk without mineralization using a dilution in an aqueous solution at pH 8 containing a tertiary amine mixed at 5 and 10% to prevent the precipitation of proteins. Murcia et al (1999) performed direct analysis of diluted milk samples (1:50) by addition of Fluka Triton X-100 (polyethylene glycol tert-octylphenyl ether; Sigma-Aldrich, Birnem, Belgium) as a tensioactive dispersant to improve the repeatability of measurements.…”

Section: Reference Methodsmentioning

confidence: 99%

Potential estimation of major mineral contents in cow milk using mid-infrared spectrometry

Soyeurt

Bruwier

Romnee

et al. 2009

Journal of Dairy Science

112

123

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Milk and dairy products are a major source of minerals, particularly calcium, involved in several metabolic functions in humans. Currently, several dairy products are enriched with calcium to prevent osteoporosis. The development of an inexpensive and fast quantitative analysis for minerals is required to offer dairy farmers an opportunity to improve the added value of the produced milk. The aim of this study was to develop 5 equations to measure Ca, K, Mg, Na, and P contents directly in bovine milk using mid-infrared (MIR) spectrometry. A total of 1,543 milk samples were collected between March 2005 and May 2006 from 478 cows during the Walloon milk recording and analyzed by MIR spectrometry. Using a principal component approach, 62 milk samples were selected by their spectral variability and separated in 2 calibration sets. Five outliers were detected and deleted. The mineral contents of the selected samples were measured by inductively coupled plasma atomic emission spectrometry. Using partial least squares combined with a repeatability file, 5 calibration equations were built to estimate the contents of Ca, K, Mg, Na, and P in milk. To assess the accuracy of the developed equations, a full cross-validation and an external validation were performed. The cross-validation coefficients of determination (R 2 cv) were 0.80, 0.70, and 0.79 for Ca, Na, and P, respectively (n = 57), and 0.23 and 0.50 for K and Mg, respectively (n = 31). Only Ca, Na, and P equations showed sufficient R 2 cv for a potential application. These equations were validated using 30 new milk samples. The validation coefficients of determination were 0.97, 0.14, and 0.88 for Ca, Na, and P, respectively, suggesting the potential to use the Ca and P calibration equations. The last 30 samples were added to the initial milk samples and the calibration equations were rebuilt. The R 2 cv for Ca, K, Mg, Na, and P were 0.87, 0.36, 0.65, 0.65, and 0.85, respectively, confirming the potential utilization of the Ca and P equations. Even if new samples should be added in the calibration set, the first results of this study showed the feasibility to quantify the calcium and phosphorus directly in bovine milk using MIR spectrometry.

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“…No entanto, o coeficiente de variação dos sinais obtidos com o uso do modificador químico foi elevado devido ao acúmulo de gordura na parede interna do capilar após algumas medidas; os coeficientes de variação das medidas foram de 15% com o uso de modificador e de 2% com o uso de mistura de aminas. Provavelmente a função das aminas terciárias seria desestruturar a caseína do leite deixando o metal livre para ser atomizado 23 . Verificou-se que não há ganho de sensibilidade com a utilização da mistura de aminas terciárias, no entanto, a repetibilidade dos sinais é excelente quando comparado com o modificador químico.…”

Section: Leiteunclassified

Determinação direta de crômio em açúcar e leite por espectrometria de absorção atômica com atomização eletrotérmica em forno de grafite

Quináia

Nóbrega

2000

Quím. Nova

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Recebido em 26/1/99; aceito em 26/7/99 DIRECT DETERMINATION OF CHROMIUM IN SUGAR AND MILK USING GRAPHITE FUR-NACE ATOMIC ABSORPTION SPECTROMETRY.A fast and direct method for the determination of Cr in milk and cane sugar suspensions using graphite furnace atomic absorption spectrometry with Zeeman-effect background correction is described. No sample pre-treatment was necessary, minimizing the risk of contamination. The concentration of chromium in cane sugar was evaluated using Cr reference solutions prepared in 1% v/v HNO 3 solution. The milk samples were introduced into the furnace with a mixture of amines for avoiding the autosampler blockage and foaming of milk. Chromium determination in milk was based on the standard additions method (SAM). The limit of detection and characteristic mass for cane sugar sample (30 µL) were 0,13 ng/ ml and 4,3 pg, and for milk sample (10 µL) were 0,23 ng/ml and 7,8 pg, respectively. The graphite tube lifetime was 300 firings for sugar-cane sample and 100 firings for milk sample. The heating program was implemented in 68 s.Keywords: milk; sugar-cane; chromium; graphite furnace; electrothermal atomization. ARTIGO INTRODUÇÃOA determinação de baixas concentrações de Cr é relevante considerando-se os efeitos fisiológicos desse elemento. O Cr possui papel importante no metabolismo da glicose, formando um complexo com moléculas de ácido nicotínico que auxiliam os processos de degradação do açúcar no sangue pela ação da insulina. Por outro lado, concentrações elevadas são letais, principalmente do metal na forma mais oxidada 1 . A determinação de Cr em matrizes complexas ainda é um desafio analítico criticamente afetado por contaminação durante processos de preparo de amostras, que podem causar elevados sinais para o branco analítico 2 . A cana contém 73-76% de água e 24-27% de sólidos, sendo que 10-17% são sólidos solúveis e 11-16 % são fibras. Considerando a baixa concentração de Cr e a complexidade do açúcar, que é essencialmente composto por material orgânico, como glicose (2-4%), sacarose (70-88%), frutose (2-4%), sais de áci-dos inorgânicos e orgânicos, proteínas, amido, goma, ceras e gorduras, a determinação de Cr nessa matriz não é trivial. Os principais aminoácidos encontrados na cana são ácido aspartático e glutâmico e os principais sais inorgânicos são cloretos e sulfatos de potássio, cálcio e magnésio 3 . O conteúdo de metais em cana de açúcar é variável e dependente da região de cultivo. Quanto maior for o número de processos envolvidos no tratamento para refino, menor será a quantidade de metais encontrados no açúcar 4 . O processo de refino do açúcar de cana envolve três etapas de clarificação (fosfatação, talo-fosfatação e carbonação) seguidas por procedimentos combinados com resinas de troca iônica e carvão ativo 3 . Dessa forma, o refinamento do açúcar geralmente causa completa eliminação do Cr 4 . Assim, maiores teores de Cr devem ser encontrados no açúcar mascavo e em derivados desse, como por exemplo a rapadura. Na legislação brasileira, segundo o Decreto 55871 5 ...

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Direct Determination of Major and Trace Elements in Milk by Inductively Coupled Plasma Atomic Emission and Mass Spectrometry

Cited by 70 publications

References 11 publications

Use of MIP OES and F AAS/AES for determination of Ca, K, Na and Mg in brazilian cream cheese

Use of MIP OES and F AAS/AES for determination of Ca, K, Na and Mg in brazilian cream cheese

Potential estimation of major mineral contents in cow milk using mid-infrared spectrometry

Determinação direta de crômio em açúcar e leite por espectrometria de absorção atômica com atomização eletrotérmica em forno de grafite

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