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.

scholarly journals Liquid Chromatography–Tandem Mass Spectrometry for the Simultaneous Determination of Doxorubicin and its Metabolites Doxorubicinol, Doxorubicinone, Doxorubicinolone, and 7-Deoxydoxorubicinone in Mouse Plasma

Molecules ◽  
2020 ◽  
Vol 25 (5) ◽  
pp. 1254 ◽  
Author(s):  
Won-Gu Choi ◽  
Dong Kyun Kim ◽  
Yongho Shin ◽  
Ria Park ◽  
Yong-Yeon Cho ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Tandem Mass ◽  
Mouse Plasma ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Doxorubicin, an anthracycline antitumor antibiotic, acts as a cancer treatment by interfering with the function of DNA. Herein, liquid chromatography-tandem mass spectrometry was for the first time developed and validated for the simultaneous determination of doxorubicin and its major metabolites doxorubicinol, doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The liquid–liquid extraction of a 10 μL mouse plasma sample with chloroform:methanol (4:1, v/v) and use of the selected reaction monitoring mode led to less matrix effect and better sensitivity. The lower limits of quantification levels were 0.5 ng/mL for doxorubicin, 0.1 ng/mL for doxorubicinol, and 0.01 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone. The standard curves were linear over the range of 0.5–200 ng/mL for doxorubicin; 0.1–200 ng/mL for doxorubicinol; and 0.01–50 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The intra and inter-day relative standard deviation and relative errors for doxorubicin and its four metabolites at four quality control concentrations were 0.9–13.6% and –13.0% to 14.9%, respectively. This method was successfully applied to the pharmacokinetic study of doxorubicin and its metabolites after intravenous administration of doxorubicin at a dose of 1.3 mg/kg to female BALB/c nude mice.

Simultaneous Determination of Isopyrazam and Azoxystrobin in Cucumbers by Liquid Chromatography–Tandem Mass Spectrometry

2017 ◽  
Vol 80 (12) ◽  
pp. 2112-2118 ◽  
Author(s):  
Dan Hu ◽  
Xu Xu ◽  
Tian Cai ◽  
Wei-Ying Wang ◽  
Chun-Jie Wu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Matrix Effects ◽  
Fast Method ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

ABSTRACTA rapid and sensitive analytical method based on high-performance liquid chromatography–tandem mass spectrometry was developed and validated for the determination of isopyrazam (IZM) and azoxystrobin (AZT) in cucumbers. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used as the pretreatment procedure. The samples were extracted with acetonitrile and cleaned up with octadecylsilyl silica (C18) and graphite carbon black. The proposed method resulted in satisfactory recovery of IZM and AZT (91.48 to 114.62%), and relative standard deviations were less than 13.1% at fortification concentrations of 1, 20, and 500 μg kg−1 (n = 3). The limits of quantification for IZM and AZT were 0.498 and 0.499 μg kg−1, respectively, which are far below the maximum residue level (0.5 mg kg−1) established for this type of sample. Matrix effects were also evaluated. This study established a sensitive and fast method for the detection of IZM and AZT in cucumber samples.

scholarly journals Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4399
Author(s):  
Dasom Shin ◽  
Hui-Seung Kang ◽  
Hyungsoo Kim ◽  
Guiim Moon
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

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.

Determination of Diflubenzuron Residues in Vegetables by UPLC-MS/MS

2014 ◽  
Vol 852 ◽  
pp. 266-269
Author(s):  
Xiao Fang Wang ◽  
Chun Liang Yang ◽  
Mao Fang Huang ◽  
Ming Yue Wang ◽  
Yu Bing Zha ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

The conditions for detecting residues of diflubenzuron in vegetables by ultra high performance liquid chromatography tandem mass spectrometry were studied. The target was extracted with acetonitrile for 2 min with a homogenizer. The extaction was purifide by a conditioned Florisil SPE cartridge, and then was detected by ultra high-performance liquid chromatography with tandem mass spectrometry. The average recovery was in the range from 87.8 %- 99.2 % at spike levels of 0.1, 1.0 and 10 mg/kg in vegetables, and relative standard deviations was in the range of 4.2 %-8.9 %. The proposed method is fast, simple, sensitive and accurate.

scholarly journals Multiresidue Determination of Quinolone and Fluoroquinolone Antibiotics in Fish and Shrimp by Liquid Chromatography/Tandem Mass Spectrometry

2007 ◽  
Vol 90 (2) ◽  
pp. 604-612 ◽  
Author(s):  
Guy Dufresne ◽  
Andre Fouquet ◽  
Don Forsyth ◽  
Sheryl A Tittlemier
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Tandem Mass ◽  
Fluoroquinolone Antibiotics ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Multiresidue Determination

Abstract A multiresidue method was developed to measure low levels of 8 fluoroquinolones (norfloxacin, ofloxacin, danofloxacin, ciprofloxacin, desethylene ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) and 4 quinolones (oxolinic acid, flumequine, nalidixic acid, and piromidic acid). Method detection limits range from 0.1 ng/g for quinolones to 0.4 ng/g for fluoroquinolones. Average recoveries range from 57 to 96%, depending on analyte and commodity; relative standard deviations are all less than 18%. The drugs are extracted from tissues using a mixture of ethanol and 1% acetic acid, diluted in aqueous HCl, and defatted by extraction with hexane. The compounds are further isolated using cation-exchange solid-phase extraction and measured using liquid chromatography with electrospray tandem mass spectrometry detection. The method has been evaluated and applied to the analysis of salmon, trout, and shrimp. Detectable residues were observed in 10 out of 73 samples, at concentrations ranging from 0.28 to 16 ng/g.

scholarly journals Identification and Quantification of Dimethylamylamine in Geranium by Liquid Chromatography Tandem Mass Spectrometry

2012 ◽  
Vol 7 ◽  
pp. ACI.S9969 ◽  
Author(s):  
J.S. Li ◽  
M. Chen ◽  
Z.C. Li
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Plant Sample ◽  
Tandem Mass ◽  
Esi Ms ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

A sensitive and reliable method of liquid chromatography–electrospray ionization/tandem mass spectrometry (LC-ESI/MS/MS) was developed and validated for determining 1,3-dimethylamylamine (1,3-DMAA) and 1,4-dimethylamylamine (1,4-DMAA) in geranium plants ( Pelargonium graveolens). The sample was extracted with 0.5 M HCl and purified by liquid-liquid partition with hexane. The parameters for reverse-phase (C18) LC and positive ESI/MS/MS were optimized. The matrix effect, specificity, linearity, precision, accuracy and reproducibility of the method were determined and evaluated. The method was linear over a range of 0.10-10.00 ng/mL examined, with R 2 of 0.99 for both 1,3-DMAA and 1,4-DMAA. The recoveries from spiked concentrations between 5.00-40.00 ng/g were 85.1%-104.9% for 1,3-DMAA, with relative standard deviation (RSD) of 2.9%-11.0%, and 82.9%-101.8% for 1,4-DMAA, with RSD of 3.2%–-11.7%. The instrument detection limit was 1-2 pg for both DMAAs. The quantification limit was estimated to be 1-2 ng/g for the plant sample. This method was successfully applied to the quantitative determination of 1,3- and 1,4-DMAA in both geranium plant and geranium oil.

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