scholarly journals Assessment of Citrinin in Spices and Infant Cereals Using Immunoaffinity Column Clean-Up with HPLC-Fluorescence Detection

Toxins ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 715
Author(s):  
Christopher Mair ◽  
Michael Norris ◽  
Carol Donnelly ◽  
Dave Leeman ◽  
Phyllis Brown ◽  
...  
Keyword(s):  
Fluorescence Detection ◽  
Hplc Analysis ◽  
Limit Of Detection ◽  
Infant Food ◽  
Red Yeast Rice ◽  
Close Monitoring ◽  
Immunoaffinity Column ◽  
Limit Of Quantification ◽  
Infant Foods ◽  
Reliable Quantification

Historically, the analysis of citrinin has mainly been performed on cereals such as red yeast rice; however, in recent years, more complex and abnormal commodities such as spices and infant foods are becoming more widely assessed. The aim of this study was to develop and validate clean-up methods for spices and cereal-based infant foods using a citrinin immunoaffinity column before HPLC analysis with fluorescence detection. Each method developed was validated with a representative matrix, spiked at various citrinin concentrations, based around European Union (EU) regulations set for ochratoxin A (OTA), with recoveries >80% and % RSD <9% in all cases. The limit of detection (LOD) and the limit of quantification (LOQ) were established at 1 and 3 µg/kg for spices and 0.1 and 0.25 µg/kg for infant cereals, respectively. These methods were then tested across a variety of spices and infant food products to establish efficacy with high recoveries >75% and % RSD <5% across all matrices assessed. Therefore, these methods proved suitable for providing effective clean-up of spices and infant cereals, enabling reliable quantification of citrinin detected. Samples such as nutmeg and infant multigrain porridge had higher levels of citrinin contamination than anticipated, indicating that citrinin could be a concern for public health. This highlighted the need for close monitoring of citrinin contamination in these commodities, which may become regulated in the future.

scholarly journals Occurrence of aflatoxins in peanuts and peanut products determined by liquid chromatography with fluorescence detection

2013 ◽  
pp. 27-35 ◽  
Author(s):  
Biljana Stojanovska-Dimzoska ◽  
Zehra Hajrulai-Musliu ◽  
Elizabeta Dimitrieska-Stojkovic ◽  
Risto Uzunov ◽  
Pavle Sekulovski
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Total Content ◽  
Immunoaffinity Column ◽  
Limit Of Quantification ◽  
Three Samples ◽  
The Mean ◽  
Positive Results

Liquid chromatography with fluorescence detection using immunoaffinity column clean-up was a method described for determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2) in peanuts and peanut based products. The validation of the procedure was performed. Good coefficient of correlation was found for all aflatoxins in the range of 0.9993-0.9999. Limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.003-0.005 mg/kg and 0.009-0.023 mg/kg, respectively, which was acceptable. The mean recovery for total aflatoxins was 88.21%. The method also showed acceptable precision values in the range of 0.171-2.626% at proposed concentration levels for all four aflatoxins. RSDR values (within laboratory reproducibility) calculated from the results showed good correlation between two analysts for all aflatoxins and they ranged from 4.93-11.87%. The developed method was applied for the determination of aflatoxins in 27 samples of peanuts and peanut based products. The results showed that 21 peanut samples (77.7%) were below LOD of the method. Three samples had positive results over the MRL. There was one extreme value recorded for the total aflatoxins in peanut (289.2 mg/kg) and two peanut based products, peanut snack and peanut, with total content of aflatoxins being 16.3 mg/kg and 8.0 mg/kg, respectively. The obtained results demonstrated that the procedure was suitable for the de?termination of aflatoxins in peanuts and peanut based products and it could be implemented for the routine analysis.

Survey of T-2 and HT-2 toxins in soybean and soy meal from Argentina using immunoaffinity clean-up and high performance liquid chromatography

2011 ◽  
Vol 4 (2) ◽  
pp. 189-197 ◽  
Author(s):  
G. Barros ◽  
D. García ◽  
M. Oviedo ◽  
M. Ramirez ◽  
A. Torres ◽  
...  
Keyword(s):  
High Performance ◽  
Hplc Analysis ◽  
Limit Of Detection ◽  
Signal To Noise Ratio ◽  
Immunoaffinity Column ◽  
Signal To Noise ◽  
Limit Of Quantification ◽  
Recovery Test ◽  
Relative Standard ◽  
Soy Meal

Soybean and soy meal samples collected during the harvest season 2008-2009 in the soybean-growing area of Córdoba Province in Argentina were analysed for T-2 and HT-2 toxins occurrence. These mycotoxins were detected using HPLC analysis with fluorescence detection after derivatisation with 1-anthronylnitrile and immunoaffinity column clean-up. Characteristics of in-house validated method such as accuracy, precision, detection and quantification limits were defined by means of recovery test with spiked soybean and soy meal samples. Mean recoveries for T-2 within the spiking range 125-500 µg/kg, were 90.9 and 81.3% for soybean and soy meal, respectively with a withinlaboratory relative standard deviation <10%. Analysis of samples spiked with HT-2 in the same range gave a mean recovery of 70.2 and 77.5% for soybean and soy meal, respectively, with relative standard deviations <12%. The limit of detection for the method was 25 µg/kg for T-2 and HT-2, based on a signal-to-noise ratio 3:1 and the limit of quantification was established as three times the detection limit. Out of 64 samples, only two soybean samples showed contamination with A-type trichothecenes evaluated. Confirmatory analyses of the contaminated samples were performed by LC-MS/MS. This study demonstrated low incidences and levels of T-2 and HT-2 in soybean harvested among the areas in the Cordoba Province.

scholarly journals Occurrence of Aflatoxin M1 (AFM1) in Donkey Milk Collected in Northern Italy

2020 ◽  
Vol 7 (4) ◽  
pp. 176
Author(s):  
Alberto Altafini ◽  
Marco Tassinari ◽  
Alessandro Guerrini ◽  
Paola Roncada
Keyword(s):  
Chemical Composition ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Northern Italy ◽  
Aflatoxin M1 ◽  
Donkey Milk ◽  
Limit Of Quantification ◽  
Milk Samples ◽  
Organoleptic Characteristics ◽  
Few Data

Aflatoxin M1 (AFM1) is a well-known mycotoxin that can be found in the milk of animals that have ingested feed contaminated with aflatoxin B1 (AFB1). In Italy, the development of donkey farms is mainly due to growing request of donkey milk, which is considered an incomparable substitute for human mother’s milk for its chemical composition and organoleptic characteristics. The aim of this study was to assess the occurrence of AFM1 in donkey milk produced in a farm in Northern Italy, also in view of the few data available about the presence of this mycotoxin in this type of milk. Therefore, 63 milk samples were collected and analyzed using a fast and sensitive HPLC and fluorescence detection (FLD) method previously optimized and validated. None of the milk samples collected were found to be contaminated at a level above the limit of quantification (LOQ) (0.0125 ng/mL), while only one sample showed traces of the mycotoxin at a concentration between the limit of detection (LOD) and LOQ (0.0044 ng/mL), well below the legal limit established for infant milk and follow-on milk (0.025 ng/mL). These results are in line with those of the few similar surveys carried out on donkey milk and seem to indicate a low risk of AFM1 contamination for this food.

Method Validation for the Quantitative Analysis of Aflatoxins (B1, B2, G1, and G2) and Ochratoxin A in Processed Cereal-Based Foods by HPLC with Fluorescence Detection

2015 ◽  
Vol 98 (4) ◽  
pp. 939-945 ◽  
Author(s):  
Işil Gazioğlu ◽  
Ufuk Kolak
Keyword(s):  
Quantitative Analysis ◽  
Simultaneous Determination ◽  
Ochratoxin A ◽  
Fluorescence Detection ◽  
Aflatoxin B1 ◽  
Hplc Analysis ◽  
Extraction Procedure ◽  
Immunoaffinity Column ◽  
Rp Hplc

Abstract Modified AOAC 991.31 and AOAC 2000.03 methods for the simultaneous determination of total aflatoxins (AFs), aflatoxin B1, and ochratoxin A (OTA) in processed cereal-based foods by RP-HPLC coupled with fluorescence detection were validated. A KOBRA® Cell derivatization system was used to analyze total AFs. One of the modifications was the extraction procedure of mycotoxins. Both AFs and OTA were extracted with methanol–water (75 + 25, v/v) and purified with an immunoaffinity column before HPLC analysis. The modified methods were validated by measuring the specificity, selectivity, linearity, sensitivity, accuracy, repeatability, reproducibility, recovery, LOD, and LOQ parameters. The validated methods were successfully applied for the simultaneous determination of mycotoxins in 81 processed cereal-based foods purchased in Turkey. These rapid, sensitive, simple, and validated methods are suitable for the simultaneous determination of AFs and OTA in the processed cereal-based foods.

Analysis of Citrinin in Cereals, Red Yeast Rice Dietary Supplement, and Animal Feed by Immunoaffinity Column Cleanup and LC with Fluorescence Detection

2016 ◽  
Vol 99 (4) ◽  
pp. 1025-1031 ◽  
Author(s):  
Elaine Marley ◽  
Phyllis Brown ◽  
Dave Leeman ◽  
Carol Donnelly
Keyword(s):  
Dietary Supplement ◽  
Fluorescence Detection ◽  
Animal Feed ◽  
Red Yeast Rice ◽  
Immunoaffinity Column ◽  
Breakfast Cereal ◽  
Method Performance ◽  
Satisfactory Performance ◽  
Red Yeast ◽  
Food And Feed

Abstract The analysis of citrinin in various cereals (wheat, oats, maize, rice, and rye and multigrain breakfast cereal), red yeast rice (dietary supplement and traditional medicine), distillers dried grain with solubles, and barley (animal feed) was carried out using a citrinin immunoaffinity column (IAC) for sample cleanup before LC analysis with fluorescence detection (LC-fluorescence). To establish method performance characteristics, wheat was spiked with citrinin at levels of 10–200 μg/kg, whereas red yeast rice was spiked at levels of 100–3000 μg/kg. Methanol–water (75 + 25, v/v) was used for the extraction of cereals and animal feed, and extraction was with 100% methanol for red yeast rice. Cleanup used a commercial citrinin IAC, followed by LC-fluorescence (λex, 330 nm; λem, 500 nm). Recoveries ranged from 80 to 110%, with r from 0.7 to 4.3%. The LOQ for citrinin in both wheat and red yeast rice was 10 μg/kg, with an LOD of 3 μg/kg. Satisfactory performance was demonstrated in a proficiency testing exercise for a sample of maize contaminated with both citrinin and ochratoxin A. It was concluded that the commercial citrinin IAC was capable of providing an efficient and effective cleanup of complex food and feed matrixes to enable citrinin to be reliably determined with the specific LC-fluorescence system used.

scholarly journals MÉTODO DE VALIDAÇÃO E SEPARAÇÃO DE ISOFLAVONAS PRESENTES EM MELAÇO DE SOJA

e-xacta ◽  
2018 ◽  
Vol 11 (1) ◽  
pp. 97
Author(s):  
Daniel Mantovani ◽  
Aline Takaoka Alves Baptista ◽  
Charleston De Oliveira Bezerra ◽  
Driano Rezende ◽  
Luis Fernando Cusioli ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Human Body ◽  
Hplc Analysis ◽  
High Efficiency ◽  
Limit Of Detection ◽  
The Body ◽  
Physiological Effects ◽  
Analysis Method ◽  
Limit Of Quantification ◽  
Functional Forms

<p><em>As isoflavonas atuam no organismo humano com efeitos fisiológicos de forma benéfica tornando os alimentos que contém isoflavonas em formas funcionais ao organismo. Assim, neste trabalho foi desenvolvido um método de análise por Cromatografia Líquida de Alta Eficiência (CLAE) bem como, separação e quantificação de isoflavonas presentes no melaço de soja. A validação do método foi baseada pela linearidade, limite de detecção (LD) e limite de quantificação (LQ) com estabelecimentos de critérios de análise para aceitação da metodologia proposta. Os resultados obtidos na separação dos isômeros de isoflavonas bem como a quantificação trouxeram melhorias relacionadas ao tempo de retenção de cada isômero estudado e separação dos compostos. Com relação ao método aplicado ao longo do estudo este apresentou resultados pertinentes para utilização e expansão do método proposto focado nos compostos de isoflavonas formas glicosídicas e agliconas presentes no melaço de soja.</em></p><p> </p><p><em>ABSTRACT</em></p><p><em>Isoflavones act in the human body with physiological effects in a beneficial way making foods containing isoflavones in functional forms to the body. Thus, in this work a high efficiency liquid chromatography (HPLC) analysis method was developed, as well as, separation and quantification of isoflavones from in soybean molasses. The validation of the method was based on linearity, limit of detection (LD) and limit of quantification (LQ) with establishments of analysis criteria for acceptance of the proposed methodology. The results obtained in the separation of the isoflavone isomers as well as the quantification brought improvements related to the retention time of each studied isomer and separation of the compounds. In relation to the method applied throughout the study, it presented relevant results for the use and expansion of the proposed method focused on the isoflavone compounds glycosidic forms and aglycones from soybean molasses.</em></p>

Determination of levofloxacin by HPLC with fluorescence detection in human breast milk

Bioanalysis ◽  
2021 ◽  
Author(s):  
Sıdıka Ertürk Toker ◽  
Gamze Ergin Kızılçay ◽  
Olcay Sagirli
Keyword(s):  
Breast Milk ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Human Breast Milk ◽  
Human Breast ◽  
Limit Of Quantification

Aim: A new HPLC method with fluorescence detection has been developed and validated for the determination of levofloxacin, one of the fluoroquinolone class antibiotics, in breast milk. Materials & methods: Chromatographic separation was carried out on a reversed phase C18 column with acetonitrile and 10 mM o-phosphoric acid (25:75,v/v) mobile phase composition. Moxifloxacin was used as internal standard and the peaks were detected by fluorescence detection. Results & conclusion: Calibration graph was found linearly within the range of 2.5–500 ng/ml. Limit of detection and limit of quantification were found to be 0.63 and 2.11 ng/ml, respectively. Mean absolute recovery was 96.18%. The developed method has been successfully applied to the determination of levofloxacin in human breast milk taken from two healthy volunteers.

Measurement of T-2 and HT-2 Toxins in Eggs by High-Performance Liquid Chromatography with Fluorescence Detection†

2006 ◽  
Vol 69 (11) ◽  
pp. 2773-2776 ◽  
Author(s):  
CHRIS M. MARAGOS
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
High Performance ◽  
Limit Of Detection ◽  
Immunoaffinity Column ◽  
Florisil Column ◽  
Coefficients Of Variation ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic

T-2 toxin is a mycotoxin produced by several species of common fungi capable of infesting human food and animal feeds. Lower-quality feeds given to chickens may be contaminated with T-2 toxin, which may affect their health. The literature suggests that T-2 toxin is transmitted from the hen to the eggs. This article describes the development of a liquid chromatographic assay for T-2 and the related mycotoxin HT-2 in eggs. T-2 and HT-2 toxins were isolated from spiked eggs with a tandem charcoal-alumina-Florisil column and immunoaffinity column cleanup. The isolated toxins were derivatized with the fluorophore 1-anthroyl nitrile, separated by high-performance liquid chromatography, and quantitated by fluorescence. The limit of detection of the method was 1 ng ml−1 (parts per billion) of T-2 and HT-2 in whole (with shell removed) eggs. The limit of quantitation for both toxins was 5 ng ml−1. Recoveries from spiked eggs over the range from 5 to 50 ng ml−1 averaged 89.2% for T-2 and 100.3% for HT-2, with coefficients of variation of 3.5 and 8.2%, respectively. This method is sensitive enough to be used to check for the presence of T-2 or HT-2 toxins in eggs.

scholarly journals Rapid Determination of Total Tryptophan in Yoghurt by Ultra High Performance Liquid Chromatography with Fluorescence Detection

Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5025
Author(s):  
Mena Ritota ◽  
Pamela Manzi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
High Performance ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Internal Standard ◽  
Milk Proteins ◽  
Reversed Phase ◽  
Limit Of Quantification

Tryptophan (TRP) is an essential amino acid which cannot be synthesized by humans and animals, but has to be supplied by exogenous sources, notably through the diet. The bulk of dietary TRP flows into the synthesis of body’s proteins, but the TRP metabolism also involves several biochemical reactions (i.e., serotonin and kynurenine pathways). Defects in the TRP transport mechanism or catabolism are related to a large number of clinical abnormalities. Therefore, dietary TRP intake is necessary not only for the body’s growth but also for most of the body’s metabolic functions. Among protein-based foods, milk proteins provide a relatively high amount of TRP. In this paper, a rapid chromatographic method for TRP determination in yoghurt, by ultra high performance liquid chromatography on a reversed-phase column with fluorescence detection (280 nm Ex; 360 nm Em), is provided. A linear gradient elution of acetonitrile in water allowed TRP analysis in 8.0 min. The limit of detection and limit of quantification of the method were 0.011 ng/µL and 0.029 ng/µL, respectively, using 5-methyl-l-tryptophan as the internal standard. The analytical method was successfully applied to commercial yoghurts from different animal species, and the TRP values ranged between 35.19 and 121.97 mg/100 g (goat and cow Greek type yoghurt, respectively).

scholarly journals Development and Validation of an Analytical Method for Determination of Ergot Alkaloids in Animal Feedingstuffs with High Performance Liquid Chromatography-fluorescence Detection

2016 ◽  
Vol 19 (3) ◽  
pp. 559-565 ◽  
Author(s):  
E. Kowalczyk ◽  
E. Patyra ◽  
A. Grelik ◽  
K. Kwiatek
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
High Performance ◽  
Limit Of Detection ◽  
Ergot Alkaloids ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Modified Quechers

Abstract A high performance liquid chromatography combined with fluorescence detection (HPLC-FLD) method was developed for determination of five ergot alkaloids (EA): ergometrine, ergotamine, ergocornine, ergocrypine and ergocristine in animal feedingstuffs. The method was based on the application of QuEChERS salts for extraction and modified QuEChERS dispersive SPE for the cleanup step. Alkaloids separation was performed on a C18, 250 mm x 4.6 mm, 5 μm column with the mobile phase containing ammonium carbonate and acetonitrile. The excitation and emission wavelengths were 330 and 420 nm respectively. The method was validated according to the Commission Decision 2002/657/EC and all parameters are in agreement with the requirements of the Decision. Linearity was determined for the concentration range of 25-400 μg/kg. The coefficient of determination (R2) for all curves was from 0.985 to 0.996. The limit of detection (LOD) was in the range 3.23 to 6.53 μg/kg and the limit of quantification (LOQ) from 11.78 to 13.06 μg/kg. The decision limit (CCα) ranged from 29.56 to 43.08 μg/kg and detection capability (CCβ) from 40.65 to 51.01 μg/kg. The highest coefficient of variation (CV) for repeatability was 14.3% and for reproducibility 15.4%.

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