scholarly journals Development and validation of a method for detection and quantification of ochratoxin A in green coffee using liquid chromatography coupled to mass spectrometry

2012 ◽  
Vol 32 (4) ◽  
pp. 775-782 ◽  
Author(s):  
Raquel Duarte da Costa Cunha Bandeira ◽  
Thaís Matsue Uekane ◽  
Carolina Passos da Cunha ◽  
Valnei Smarçaro da Cunha ◽  
Janaína Marques Rodrigues ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Green Coffee ◽  
Intermediate Precision ◽  
Future Production ◽  
Relative Standard ◽  
Mycotoxin Analysis ◽  
Development And Validation ◽  
Detection And Quantification

A method using Liquid Chromatography Tanden Mass Spectrometry (LC-MS/MS) with matrix-matched calibration curve was developed and validated for determining ochratoxin A (OTA) in green coffee. Linearity was found between 3.0 and 23.0 ng.g-1. Mean recoveries ranged between 90.45% and 108.81%; the relative standard deviation under repeatability and intermediate precision conditions ranged from 5.39% to 9.94% and from 2.20% to 14.34%, respectively. The limits of detection and quantification were 1.2 ng.g-1 and 3.0 ng.g-¹, respectively. The method developed was suitable and contributed to the field of mycotoxin analysis, and it will be used for future production of the Certified Reference Material (CRM) for OTA in coffee.

scholarly journals Detection of Five Mycotoxins in Different Food Matrices in the Malaysian Market by Using Validated Liquid Chromatography Electrospray Ionization Triple Quadrupole Mass Spectrometry

Toxins ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 196 ◽  
Author(s):  
Ali Alsharif ◽  
Yeun-Mun Choo ◽  
Guan-Huat Tan
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Wheat Flour ◽  
Food Samples ◽  
Food Contaminants ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Food Matrices

Mycotoxins are common food contaminants which cause poisoning and severe health risks to humans and animals. The present study applied chemometric approach in liquid chromatography-tandem mass spectrometry (LC-MS/MS) optimization for simultaneous determination of mycotoxins, i.e., aflatoxins B1, B2, G1, and G2, and ochratoxin A. The validated quick, easy, cheap, effective, rugged, and safe (QuEChERS)-LC-MS/MS method was used to study the occurrence of mycotoxins in 120 food matrices. The recovery ranges from 81.94% to 101.67% with relative standard deviation (RSD) lesser than 11%. Through the developed method, aflatoxins were detected in raisin, pistachio, peanut, wheat flour, spice, and chili samples with concentration ranges from 0.45 to 16.93 µg/kg. Trace concentration of ochratoxin A was found in wheat flour and peanut samples which ranged from 1.2 to 3.53 µg/kg. Some of the tested food samples contained mycotoxins of above the European legal maximum limit.

Determination of Ochratoxin A in Wine by Immunoaffinity Cleanup and Liquid Chromatography Tandem Mass Spectrometry

2008 ◽  
Vol 71 (5) ◽  
pp. 1038-1042 ◽  
Author(s):  
SHIGEKUNI NOBA ◽  
MASAYUKI OMOTE ◽  
YASUSHI KITAGAWA ◽  
NAOKI MOCHIZUKI
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ochratoxin A ◽  
Tandem Mass ◽  
Immunoaffinity Column ◽  
White Wines ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

A simple and accurate method has been developed for determining ochratoxin A (OTA), using an immunoaffinity column for cleanup and liquid chromatography–tandem mass spectrometry for identification and quantification. Wine samples were diluted with a solution containing polyethylene glycol 8000 and sodium hydrogen carbonate, filtered through a glass microfiber filter, and cleaned up on an immunoaffinity column. OTA was then eluted with methanol–acetic acid (98:2) and analyzed by liquid chromatography–tandem mass spectrometry. The average recoveries of OTA from red and white wines were 95 and 96.7% (spiked OTA level was 0.05 ng/ml) and repeatabilities (relative standard deviation) were 3.8 and 2.4%, respectively. The detection limit was 0.0003 ng/ml based on the signal-to-noise ratio in wine of 3:1. Analysis of 74 samples of domestic and imported wines showed OTA levels ranging from <0.0003 to 0.82 ng/ml, with an incidence of contamination of 92.1% for red wines, and <0.0003 to 0.51 ng/ml, with an incidence of contamination of 77.8% for white wines. These detection rates were higher than those rates of past reports of OTA contamination in wine, due to the high sensitivity of this method. However, all samples analyzed in this study complied with European Union regulations. It is concluded that this method is a useful tool for the quality assurance of wine.

scholarly journals Monitoring Stevioside in Soju by High-Performance Liquid Chromatography and Liquid Chromatography/Mass Spectrometry

2007 ◽  
Vol 90 (5) ◽  
pp. 1365-1372 ◽  
Author(s):  
Fan Ni ◽  
Jeffrey Ammann ◽  
Abdul Mabud
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Single Step ◽  
Intermediate Precision ◽  
Relative Standard ◽  
Validation Parameters ◽  
Concentration Levels

Abstract A method using high-performance liquid chromatography (HPLC) with UV absorption detection was developed to monitor stevioside in soju, a distilled spirits product that is commercially available. The method uses a single-step dilution for sample preparation. It completely eliminates the time-consuming process of solid-phase extraction. A method using HPLC/mass spectrometry was optimized to confirm the identities of stevioside and other related impurities, including rebaudioside A, rebaudioside C, and dulcoside. The method was validated. The validation parameters included range (10.11007.3 ppm), precision, linearity, accuracy, robustness, system suitability, and intermediate precision. Stevioside standard solutions at 6 concentration levels were prepared for the validation work, including the tests for precision, linearity, and accuracy. The solutions were prepared in triplicate for each concentration. The relative standard deviation for the precision test was <3 for all 6 concentration levels. The correlation coefficient for the linearity within the concentration range was determined to be >0.999. The average recovery ranged from 95.7 to 101.1 for the soju samples spiked with stevioside standard. The detection limit for stevioside was estimated at 75 ppb. The method was used to screen several soju samples; no detectable stevioside was found in the samples.

Development and Validation of Multiclass Chiral Pesticide Residues Analysis Method in Tea by QuEChERS Combined Liquid Chromatography Quadruple-Linear Ion Trap Mass Spectrometry

2020 ◽  
Vol 103 (3) ◽  
pp. 865-871
Author(s):  
Hongcheng Liu ◽  
Tao Lin ◽  
Qiwan Li
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Pesticide Residues ◽  
Ion Trap ◽  
Ion Trap Mass Spectrometry ◽  
Linear Ion Trap ◽  
Analysis Method ◽  
Chiral Pesticides ◽  
Relative Standard ◽  
Development And Validation

Abstract Background No single pure enantiomeric pesticide residues was investigated and set regulations for tea quality safety and risk assessment. Objective Due to lack of chiral pesticide analysis method and data, the Maximum residue limits (MRLs) about the chiral pesticides in tea was unknown. Method An analytical method for the determination of chiral pesticide residues by QuEChERS combined chiral liquid chromatography quadruple/linear ion trap mass spectrometry (LC-MS/MS-Qtrap) was developed and applied to the analysis of various teas. Results The mean recoveries for pesticides enantiomers ranged from 75.9% to 112.4%. Reproducibility represented by relative standard deviation percentage was 10% or less. Good linearity was achieved for all enantiomers with determination coefficients (r2) greater than 0.99. The detection of limit (CCα) and quantification of limit (CCβ) were 0.2 ∼1 µg/kg and 0.5∼5 µg/kg, respectively. Conclusions The method was suitable for monitoring the enantiomeric pesticide residues in various teas. Highlights Enantioselective multiclass pesticide residues were determined in various teas by LC-MS/MS-Qtrap, additional Qtrap scan functions greatly enhance the performance of screening, confirmation, and identification of chiral pesticides.

scholarly journals Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS)

Química Nova ◽  
2012 ◽  
Vol 35 (1) ◽  
pp. 66-71 ◽  
Author(s):  
Raquel D. C. C. Bandeira ◽  
Thais M. Uekane ◽  
Carolina P. da Cunha ◽  
Luths R. O. Geaquinto ◽  
Valnei S. Cunha ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Electrospray Mass Spectrometry ◽  
Roasted Coffee ◽  
Esi Ms ◽  
Development And Validation

scholarly journals Monitoring Lipophilic Toxins in Seawater Using Dispersive Liquid—Liquid Microextraction and Liquid Chromatography with Triple Quadrupole Mass Spectrometry

Toxins ◽  
2021 ◽  
Vol 13 (1) ◽  
pp. 57
Author(s):  
Ainhoa Oller-Ruiz ◽  
Natalia Campillo ◽  
Manuel Hernández-Córdoba ◽  
Javier Gilabert ◽  
Pilar Viñas
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Reversed Phase ◽  
Triple Quadrupole ◽  
Relative Standard ◽  
Mar Menor Lagoon ◽  
Lipophilic Toxins ◽  
Seawater Samples ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

The use of dispersive liquid–liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 µL of chloroform were injected into 12 mL of sample. The enriched organic phase, once evaporated and reconstituted in methanol, was analyzed by reversed-phase liquid chromatography with triple-quadrupole tandem mass spectrometry. A central composite design multivariate method was used to optimize the interrelated parameters affecting DLLME efficiency. The absence of any matrix effect in the samples allowed them to be quantified against aqueous standards. The optimized procedure was validated by recovery studies, which provided values in the 82–123% range. The detection limits varied between 0.2 and 5.7 ng L−1, depending on the analyte, and the intraday precision values were in the 0.1–7.5% range in terms of relative standard deviation. Ten water samples taken from different points of the Mar Menor lagoon were analyzed and were found to be free of the studied toxins.

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