Determination of mesalamine by spectrofluorometry in human serum after solid-phase extraction with Ni-Al layered double hydroxide as a nanosorbent

Abstract

Hidróxido duplo lamelar de níquel-alumínio nanoestruturado foi sintetizado e o potencial do material obtido, foi avaliado como sorvente para extração em fase sólida (SPE), na separação e pré-concentração de quantidades traço de mesalazina (ácido 5-aminossalicílico) usando o método de coluna. O analito retido em Ni-Al LDH foi removido por solução de NaOH e a concentração de 5-ASA eluída foi então determinada espectrometricamente em λ em = 480 nm com excitação em λ ex = 340 nm. Vários parâmetros experimentais afetando a eficiência da extração de mesalazina em Ni-Al (NO 3 -) LDH, tais como pH, quantidade de sorvente, taxa de fluxo da quantidade de amostra, condições de eluição e volume de amostra, foram investigados. Nas condições experimentais ideais, o limite de detecção e o fator de enriquecimento foram 0,04 e 40 µg L −1 , respectivamente. A curva de calibração do sistema de pré-concentração foi linear no intervalo de 0,1-45,0 µg L −1 com um coeficiente de correlação 0,998. O desvio padrão relativo resultante da análise de seis repetições de soluções de 100 mL contendo 1,0 µg L -1 de mesalazina foi 2,05%. O método otimizado foi aplicado com sucesso na determinação de mesalazina em amostras de soro de sangue. Nanostructured nickel-aluminum layered double hydroxide (Ni-Al LDH) was synthesized and the potential of the obtained material, as solid-phase extraction (SPE) sorbent, for separation and pre-concentration of trace amount of mesalamine (5-aminosalicylic acid) was assessed using column method. The retained analyte on Ni-Al LDH was eluted with NaOH solution and the concentration of the elueted 5-ASA was then spectrofluorometrically determined at λ em = 480 nm with excitation at λ ex = 340 nm. Various experimental parameters affecting the extraction efficiency of mesalamine on Ni-Al (NO 3 -) LDH, such as pH, amount of sorbent, sample loading flow rate, elution conditions and sample volume, were investigated. In the optimum experimental conditions, the limit of detection and enrichment factor were 0.04 and 40 µg L −1 , respectively. The calibration graph for the pre-concentration system was linear in the range of 0.1-45.0 µg L −1 with a correlation coefficient of 0.998. The relative standard deviation (RSD) resulting from the analysis of six replicates of 100 mL solutions containing 1.0 µg L -1 mesalamine was 2.05%. The optimized method was successfully applied to the determination of mesalamine in blood serum samples.

Effect of polarization switching on piezoelectric and dielectric performance of electrospun nanofabrics of poly(vinylidene fluoride)/Ca–Al LDH nanocomposite

“…The strong band centered at 1382 cm −1 relates to the stretching vibrations of NO 3 − ions intercalated at the interlayer space of LDH. The bands at 789, 576, 532, and 424 cm −1 are ascribed to the metal–oxygen (Ca 2+ /Al 3+ ) lattice vibrations (M − O, M − O – M, and O − M − O) …”

“…The strong band centered at 1382 cm −1 relates to the stretching vibrations of NO 3 − ions intercalated at the interlayer space of LDH. The bands at 789, 576, 532, and 424 cm −1 are ascribed to the metal- 34,35 The morphological features of Ca-Al LDH were examined by SEM and TEM. Figure 3 shows the SEM images of Ca-Al LDH at different magnifications.…”

Direct synthesis of Ni2Al(OH)7−x(NO3)x·nH2O layered double hydroxide nanolayers by SILD and their capacitive performance

“…It corresponds to inclusion of water molecules and nitrate anions into the studied films, which were trapped during the film synthesis from Ni and Al nitrates solutions. Bands at 634, 583 and 417 cm À 1 may be assigned to vibrations of metal-oxygen bonds [14]. XRD, EDX and FTIRspectroscopy data allow one to identify studied LDH as Ni 2 Al (OH) 7 …”

Electrochemical sensing of mesalazine and its N-acetylated metabolite in biological samples using functionalized carbon nanotubes

“…Various analytical methods were described in the literature for the determination of 5-ASA, such as liquid chromatography coupled to mass spectrometry for drug quantification in plasma samples [3], HPLC with UV detection for stability-indicating assays [4] and analysis in pharmaceutical formulations [5], capillary electrophoresis for drug impurity profiling [6], spectrophotometry [7], fluorescence spectroscopy [8], automated chemiluminescence [9] and ultra-performance liquid chromatography [10]. At present, several HPLC methods with a fluorescence [11][12][13], electrochemical [14,15] and mass spectrometry detection [16,17] were developed for simultaneous quantification of 5-ASA and its N-acetylated metabolite.…”