Validation of spectrophotometric method to detect and quantify nitrite in ham pate

Abstract

The objective of this work was to validate the spectrophotometric method to detect and quantify nitrite using ham pate as a source. The validated analytical conditions were 540 nm wavelength and the samples reading between 40 to 70 minutes after addition of coloring agents. The tested performance criteria were: linearity, matrix effect, selectivity, detection and quantification limit, accuracy, precision and robustness. As the results have obtained linearity in the studied zone (0.125 to 3 g/mL) and matrix effect was not observed, there was not any interference from ascorbic acid, but interference occurred from sodium eritorbate, in concentrations above 2.5 mg/100g. The detection limit was defined as 12.5 mg of nitrite/kg for pate and the quantification limit as 25 mg of nitrite/kg of pate. The method presented repeatability and reproducibility. The accuracy was assessed through recovery values varying from 84 to 110%. Respecting robustness, it was observed that the variations applied to the extraction procedure depended on the concentration of nitrite in the pate sample. In conclusion, the methodology was validated under the tested conditions. Uniterms: Validation. Nitrite. Spectrophotometric method. Ham pate.O objetivo deste trabalho foi validar o método espectrofotométrico para determinação de nitrito usando como matriz patê de presunto. As condições analíticas usadas foram comprimento de onda de 540 nm e leitura das amostras entre 40 e 70 minutos após a adição dos reagentes complexantes. As características de desempenho testadas foram linearidade, efeito de matriz, seletividade, limite de detecção do equipamento e do método, limite de quantificação, exatidão, precisão e robustez. A linearidade foi obtida na faixa de trabalho estudada (0,125 a 3 µg de nitrito/mL) e não foi observado efeito de matriz. A concentração de ácido ascórbico na amostra não interferiu na análise e o eritorbato de sódio possuiu interferência negativa para concentrações acima de 2,5 mg/100g de amostra. O limite de detecção foi definido em 12,5 mg de nitrito/kg de patê e o limite de quantificação em 25 mg de nitrito/kg de amostra. O método apresentou repetitividade e reprodutibilidade intra-laboratorial. A exatidão foi avaliada através dos valores de recuperação que variaram entre 84 e 110%. Na avaliação da robustez, as variações realizadas no procedimento de extração foram dependentes do nível de concentração existente na amostra. Concluiuse que a metodologia pôde ser validada nas condições testadas. Unitermos:Validação. Nitrito. Espectrofotometria. Patê de presunto.

TES CEPAT UNTUK DETEKSI ALBUMINURIA BERBASIS PERAK IODIDA(AgI) dan METILEN BIRU

“…Pengukuran kadar albumin High Performance Liquid Chromatography (HPLC) (Rodchenkov et al, 2008), serta metodeliquid chromatography tandem mass spectrometry (LC-MS/MS) dapat dilakukan untuk mengukur kadar albumin (Ketha and Singh 2016). Semua metode tersebut memerlukan alat analisis yang relatif mahal, biaya analisis tinggi, membutuhkan tenaga ahli dalam pengoperasiannya, dan biaya perawatan instrumen yang tinggi sehingga dinilai tidak ekonomis (Reis et al, 2009). Oleh sebab itu dikembangkan tes cepat untuk deteksi albuminuria Reagent yang digunakan untuk tes cepat ini adalah perak iodida (AgI) dan metilen biru (MB).…”

27 Afthoni et al. Novel Scanometric Assay for Charantin in Bitter Melon ( Momordica charantia ) Extract Based on Immobilized Silver Nitrate and Methylene Blue as Colorimetric Paper

“…The conventional methods for determination of charantin are thin layer chromatography (TLC) [12], high performance thin layer chromatography (HPTLC) [13], high performance liquid chromatography (HPLC) [14], gases chromatography tandem mass spectroscopy (GC-MS) [15]. However, these methods are needed sample preparation, long procedure, and skilled personnel, as well as relatively expensive [16]. Certainly, for the big company or industry using conventional standard methods would not be an issue to comply with all…”