Detection of Deoxynivalenol Contamination in Wheat Products in Thailand

2008 ◽  
Vol 71 (9) ◽  
pp. 1931-1933 ◽  
Author(s):  
AMNART POAPOLATHEP ◽  
SARANYA POAPOLATHEP ◽  
NARUMOL KLANGKAEW ◽  
YOSHIKO SUGITA-KONISHI ◽  
SUSUMU KUMAGAI

A total of ninety samples in three kinds of wheat products (30 noodle, 30 bread, and 30 cereal samples) were collected from the supermarkets in Bangkok, Thailand, from February to April 2007. The occurrence of deoxynivalenol (DON) contamination in wheat products was investigated using high-performance liquid chromatography equipped with a UV light detector. The extraction method was performed using a multifunctional cleanup column. The limit of quantification was 0.10 μg·g−1 from the range obtained in a linear calibration. The survey found almost 94% of the DON-contaminated samples below 1 μg·g−1, which corresponds to the U.S. Food and Drug Administration advisory level. DON was detected in 18.9% (17 of 90) of all samples, in 6.67% (2 of 30) and 16.67% (5 of 30) of noodle and bread samples at levels from 0.17 to 0.35 and 0.14 to 1.13 μg·g−1, respectively, while it was in 33.33% (10 of 30) of cereal samples at levels from 0.13 to 0.39 μg·g−1. The results suggest that the exposure to DON from the consumption of wheat products, especially noodles, bread, and cereal, is at a very low risk level.

Toxins ◽  
2021 ◽  
Vol 13 (5) ◽  
pp. 316
Author(s):  
Laura Carbonell-Rozas ◽  
Choukri Khelifa Mahdjoubi ◽  
Natalia Arroyo-Manzanares ◽  
Ana M. García-Campaña ◽  
Laura Gámiz-Gracia

The natural occurrence of six major ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers, were investigated in 60 cereal samples (barley and wheat) from Algeria. Ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) and a QuEChERS extraction method were used for sample analysis. The results revealed that 12 out of 60 samples (20%) were contaminated with ergot alkaloids. Wheat was the most contaminated matrix, with an incidence of 26.7% (8 out of 30 samples). The concentration of total ergot alkaloids ranged from 17.8 to 53.9 µg/kg for barley and from 3.66 to 76.0 μg/kg for wheat samples. Ergosine, ergokryptine and ergocristine showed the highest incidences in wheat, while ergometrine was the most common ergot in barley.


1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.


2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.


Author(s):  
PULAGURTHA BHASKARARAO ◽  
GOWRI SANKAR DANNANA

Objective: Noscof tablet is a fixed dosage combination formulation having diphenhydramine (DH), ephedrine (ED), noscapine (NP), and glycerol glycolate (GG). A sensitive, selective, accurate, precise, and stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method with photodiode array detection has been developed and validated for simultaneous analysis of DH, ED, NP, and GG in bulk drug and Noscof tablets. Methods: Reversed-phase chromatographic separation and analysis of DH, ED, NP, and GG were done on an Altima C18 column with 0.01 M KH2PO4 buffer (pH 3.5) and acetonitrile (50:50%, v/v) as mobile phase at 0.8 ml/min flow rate in isocratic mode. Detection was performed at 260 nm. The method was validated in harmony with International Conference on Harmonization (ICH) guidelines. The tablet sample solution was subjected to diverse stress conditions using ICH strategy such as hydrolytic degradation (neutral - with distilled water, alkaline - with 2 N NaOH, and acidic - with 2 N HCl), oxidation (with 10% H2O2), photodegradation (exposing to UV light), and dry heat degradation (exposing to 105°C). Results: Using the above stated chromatographic conditions, sharp peaks were obtained for ED, NP, DH, and GG with retention time of 3.272 min, 4.098 min, 5.467 min, and 6.783 min, respectively. Good regression coefficient values were obtained in the range of 2–12 μg/ml for ED, 3.75–22.5 μg/ml for NP, 3.125–18.75 μg/ml for DH, and 25–150 μg/ml for GG. The quantification limits were 0.181 μg/ml, 0.187 μg/ml, 0.246 μg/ml, and 1.114 μg/ml for ED, NP, DH, and GG, respectively. The values of validation parameters are within the acceptance limits given by ICH. The ED, NP, DH, and GG showed more percent of degradation in acid condition and less percent of degradation in the neutral condition. The peaks of degradants did not interfere with the peaks of analytes. ED, NP, DH, and GG were assessed with a good percentage of the assay (near to 100%) and low percent relative standard deviation (<2%) in Noscof tablets using the proposed method. Conclusion: The stability indicating RP-HPLC method developed was suitable for quantifying ED, NP, DH, and GG simultaneously in bulk as well as in tablet formulation.


2019 ◽  
Vol 18 (2) ◽  
pp. 73-77
Author(s):  
L. M. Fedoseeva ◽  
Yu. I. Chistova

The purpose of this work is to study of phenolic compounds in the dry extract of dandelion herb and large burdock leaf tea.Materials and methods . The separation and identification of phenolic compounds of dry extract of dandelion herb and large burdock leaf tea by thin-layer chromatography and high-performance liquid chromatography with UV-detectionhas been carried out.Results . As a result of research, it has been established that during TLC the optimal system for the separation of phenolic compounds is the ethyl acetate – formic acid – water system (10:2:3). On the chromatogram four spots were found corresponding to the value of Rf and fluorescence in UV-light to flavonoids of the flavone group and phenolic acids (chlorogenic and caffeic acids). For further identification of phenolic compounds using HPLC, eight peaks were found, which in terms of retention time and spectral characteristics correspond to phenologlycosides, chlorogenic acid, caffeic acid derivatives, ferulic acid, umbelliferone.Conclusions . Thus, the dry extract of dandelion herb and large burdock leaf tea contains hydroxycinnamic acids and their derivatives, compounds of coumarin nature, phenologlycosides.


2013 ◽  
Vol 750-752 ◽  
pp. 1852-1854
Author(s):  
Shu Jun Liu ◽  
Kun Feng ◽  
Hao Nan Xu ◽  
Ying Wang

The gasoline combustion dusts was analyzed by accelerated solvent extraction-high performance liquid chromatography(ASE-HPLC) in this paper. The optimum extraction conditions were that extraction time was 30min, temperature was 120°C and the pressure was 100Mpa. It is a efficient extraction method for a laboratory to quickly extract gasoline combustion dust samples.


2020 ◽  
Vol 58 (10) ◽  
pp. 915-921
Author(s):  
Sho Ohkubo ◽  
Yumiko Akamine ◽  
Tadashi Ohkubo ◽  
Yuka Kikuchi ◽  
Masatomo Miura

Abstract Here, we developed a novel high-performance liquid chromatography (HPLC) method for quantification of perampanel in clinical practice and investigated the relationships between the plasma concentrations of perampanel obtained by this HPLC method and the CYP3A4*1G polymorphism. The developed HPLC method was validated based on US Food and Drug Administration. The developed HPLC method could be performed with a plasma volume of only 200 μL and had a limit of quantification (LOQ) of 2.5 ng/mL. The coefficients of variation (CVs) for intra- and inter-day assays were less than 10.4 and 7.2%, respectively, and the accuracy was &lt;2.4% for both assays. A total of 12 patients who received 2 mg perampanel had C0 values ranging from 70.5 to 451 ng/mL, and the CV showed a large variation of 51.4%. No correlations were observed between the dose-adjusted C0 and the CYP3A4*1G polymorphism. This method was superior to previously reported methods in terms of plasma volume and LOQ and was clinically applicable. Perampanel showed high variations in individual plasma concentrations; however, individual differences could not be predicted from analysis of the CYP3A4*1G polymorphism before perampanel administration. Therefore, after beginning perampanel treatment, the dose should be determined based on the observed plasma concentration.


Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.


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