Development and inter-laboratory study of a method for quantifying ochratoxin A in pet foods

2017 ◽  
Vol 10 (1) ◽  
pp. 53-61
Author(s):  
T. Wada ◽  
H. Saito ◽  
K. Aoyama ◽  
S. Saito ◽  
M. Shibukawa
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Laboratory Study ◽  
High Performance ◽  
Immunoaffinity Column ◽  
Pet Food ◽  
Aqueous Acetonitrile ◽  
Relative Standard ◽  
The Mean

An analytical method for quantifying ochratoxin A (OTA) in pet foods using high-performance liquid chromatography was developed, and an inter-laboratory study was conducted. OTA was extracted from samples with aqueous acetonitrile. The extract was purified by an immunoaffinity column, OCHRAKING, and analysed by high performance liquid chromatography with fluorescence detection. The limits of quantification by this method were 2 µg/kg for dry and semidry pet food and 1 µg/kg for wet type pet food. The calibration curve showed linearity in the range of 0.5-50 ng/ml (equivalent to 1-100 µg/kg for wet type pet food). The mean recoveries of OTA spiked at 1-5 µg/kg were in the range of 83.0-106% and relative standard deviations of the in-house method validation were 2.6-6.8%. The mean recoveries, repeatability, reproducibility and the Horwitz ratios for OTA from the inter-laboratory validation study were 75.6-83.1%, 3.5-6.1%, 5.0-15.0% and 0.23-0.68, respectively.

Development and inter-laboratory study of a method for quantification of fumonisin B1, B2 and B3 in pet foods

2015 ◽  
Vol 8 (1) ◽  
pp. 55-61 ◽  
Author(s):  
M. Nomura ◽  
T. Ishibashi ◽  
T. Komoriya ◽  
T. Nagahara ◽  
T. Chihara
Keyword(s):  
Liquid Chromatography ◽  
Laboratory Study ◽  
Fumonisin B1 ◽  
Ionization Mass ◽  
Pet Food ◽  
Limit Of Quantification ◽  
Aqueous Acetonitrile ◽  
Esi Ms ◽  
Relative Standard ◽  
The Mean

An analytical method to determine fumonisin B1 (FB1), B2 (FB2) and B3 (FB3) in pet foods using a liquid chromatography-electrospray ionization-mass spectrometer (LC-ESI-MS) was developed, and an inter-laboratory study was conducted in eleven laboratories. FB1, FB2 and FB3 were extracted with aqueous acetonitrile. The extract was purified by a multifunctional column, MultiSep 211 Fum, and analysed by LC-ESI-MS. The limit of quantification of fumonisins was estimated to be 0.2 mg/kg for dry and semi-dry pet foods, and 0.1 mg/kg for wet pet food. The calibration curve showed linearity in the range of 0.1-5 ng of fumonisins (0.02-1.0 μg/ml). The values of the mean recovery for FB1 at 0.1-1.0 mg/kg were 93.3-107% and of the relative standard deviation less than 7.9%. These values were 87.3-102 and 8.6% for FB2 and 90.8-102 and 8.6% for FB3, respectively. The mean recovery, repeatability, reproducibility and the Horwitz ratio for FB1 from the inter-laboratory validation study were 92.9-98.9%, 2.6-4.6%, 6.8-10% and 0.41-0.54, respectively. The values for FB2 were 91.5-94.7%, 2.7-5.9%, 6.8-8.9% and 0.33-0.55, respectively, and the values for FB3 were 90.1-94.3%, 3.3-5.9%, 7.3-9.5% and 0.44-0.57, respectively.

Determination of β -Sitosterol with Chemical Course and Material Applications in Jatropha Seed Oil by High Performance Liquid Chromatography

2012 ◽  
Vol 577 ◽  
pp. 69-72 ◽  
Author(s):  
Shu Yu Liu ◽  
Anaerguli Maihemuti
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Seed Oil ◽  
Reversed Phase ◽  
Analytical Recovery ◽  
Relative Standard ◽  
The Mean ◽  
Jatropha Seed

A simple and rapid high performance liquid chromatography (HPLC) assay was developed to identify and measure theβ-sitosterol with chemical course and material applications in jatropha seed oil. The stigmasterol was isolated with a good selectivity by HPLC employing reversed phase C18 columns. The components were separated by mobile phase of methanol-water (99/1, v/v) and detected at 205nm. The quantitation of the stigmasterol was reproducible and the method relative standard deviation is 1.1%. The mean analytical recovery was 96.2%.

scholarly journals Determination of Aflatoxins and Ochratoxin a in Animal Liver Using HPLC-FD Method with Immunoaffinity Column Clean-Up

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Biljana Stojanovska-Dimzoska ◽  
Elizabeta Dimitrieska-Stojkovic ◽  
Zehra Hajrulai-Musliu ◽  
Risto Uzunov ◽  
Aleksandra Angeleska ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Immunoaffinity Column ◽  
Acceptable Range ◽  
Animal Liver ◽  
Relative Standard ◽  
Validation Parameters ◽  
The Mean ◽  
Concentration Levels

Abstract Analytical methods based on immunoaffinity column clean-up and quantitative determination with liquid chromatography-fluorescence detection were used to determine aflatoxins and ochratoxin A in liver samples. The validation of the procedures was performed. The linearity of the methods was checked, and a good coefficient of correlation was found for all aflatoxins and OTA as well. The LOD and LOQ were acceptable: 0.003 µg/kg and 0.009 µg/kg for AFB1; 0.001 µg/kg and 0.005 µg/kg for AFB2; 0.006 µg/kg and 0.020 µg/kg for AFG1; 0.007 µg/kg and 0.022 µg/kg for AFG2; 0.08 µg/kg and 0.27 µg/kg for OTA. The results for the repeatability estimated by the relative standard deviation (RSDr) were satisfactory and the obtained values were in the acceptable range (1.97–14.41% for all aflatoxins and 3.76-8.31% for OTA) at three proposed concentration levels. RSDR values showed acceptable correlation between two analysts for all four aflatoxins and OTA. The RSDR values were as followed: 2.37% and 5.60% for AFB1, 6.71% and 8.78% for AFB2, 4.40% and 7.00% for AFG1 and 10.30% and 13.91% for AFG2 (for the first and second analyst, respectively). The RSDR values for OTA were 4.91% and 3.15% (1 µg/kg); 3.76% and 4.12% (5 µg/kg) and 8.31% and 8.21% (10 µg/kg). The mean recovery for total aflatoxins and OTA were 78.10% and 93.34%, respectively. All validation parameters were in accordance to European legislation. They indicate that the proposed analytical procedures are suitable and they could be methods of choice for the determination of aflatoxins and OTA in liver samples.

scholarly journals Analysis of ochratoxin A in malt beverage samples using dispersive liquid–liquid microextraction coupled with liquid chromatography-fluorescence detection

2013 ◽  
Vol 31 (No. 5) ◽  
pp. 520-525 ◽  
Author(s):  
M. Maham ◽  
V. Kiarostami ◽  
S. Waqif-Husain ◽  
R. Karami-Osboo ◽  
M. Mirabolfathy
Keyword(s):  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Fluorescence Detection ◽  
High Performance ◽  
Optimum Conditions ◽  
Beverage Samples ◽  
Extraction Solvent ◽  
Relative Standard ◽  
The Mean ◽  
Liquid Microextraction

A simple and economic procedure based on dispersive liquid–liquid microextraction has been applied to extract and pre-concentrate trace levels of ochratoxin A (OTA) in malt beverage prior to analysis using high performance liquid chromatography with fluorescence detection. The method was based on the formation of fine droplets of a water-immiscible extraction solvent in the sample solution using a water-miscible disperser solvent. The influences of various parameters such as the type and volume of extraction and disperser solvents, centrifuging time, sonication time, and salt concentration on the extraction efficiency of ochratoxin A were investigated. Under optimum conditions, the relative standard deviations for five replicates of 2 ng/ml of OTA were 3.4% as within-day and 6.2% as between-day precisions. The detection limit (S/N = 3) was 0.1 ng/ml and the mean recoveries of OTA from malt beverage samples at spiking levels of 0.5, 2, and 4 ng/ml were in the range of 104–108.2%.

scholarly journals Ochratoxin A determination in beer by immunoaffinity column clean-up and high-performance liquid chromatography

2003 ◽  
Vol 23 ◽  
pp. 58-61 ◽  
Author(s):  
Guilherme Prado ◽  
Marize Silva Oliveira ◽  
Eliana Pinheiro Carvalho ◽  
Luiz Carlos Oliveira Lima ◽  
Thais Veloso ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Ochratoxin A ◽  
High Performance ◽  
Immunoaffinity Column

Determination of Ochratoxin A in Pig Kidneys by Immunoaffinity Cleanup and Ultra-High Performance Liquid Chromatography

2015 ◽  
Vol 98 (6) ◽  
pp. 1566-1570 ◽  
Author(s):  
YaLi Hou ◽  
Jinhui Zhou ◽  
YuPing Li ◽  
JiangHua Xie ◽  
Li Zhou ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Ochratoxin A ◽  
High Performance ◽  
Accurate Method ◽  
Immunoaffinity Column ◽  
Trace Level ◽  
Pig Kidney ◽  
Identification And Quantification

Abstract An accurate method was developed for determining ochratoxin A (OTA) in pig kidney using an immunoaffinity column for cleanup and ultra-HPLC/MS/MS for identification and quantification. Mean recoveries of OTA from kidney samples fortified at 0.10–5 μg/kg levels ranged from 74 to 92%, with RSDs of 4.6–7.5%. The LOD was estimated to be 0.03 μg/kg and the LOQ was 0.10 μg/kg based on an S/N in kidney of 3:1 and 10:1, respectively. The developed method was used for the determination of OTA in pig kidney. A survey of the OTA content of pig kidneys slaughtered in Chongqing, China, revealed that 35 out of 40 analyzed samples were contaminated; the OTA concentration in kidney ranged from trace level (0.03–0.1) to 0.323 μg/kg. This method was shown to be useful for accurately evaluating the intake of OTA from pig kidneys.

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