scholarly journals Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry

Agriculture ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 283
Author(s):  
Irina Gabriela Cara ◽  
Denis Topa ◽  
Lucian Raus ◽  
Anca Elena Calistru ◽  
Feodor Filipov ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Residue Analysis ◽  
Soybean Plant ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Solvent Extraction Method ◽  
Soybean Straw

Herbicide residue analysis has gained importance worldwide, mainly for food quality control to minimize potentially adverse impacts on human health. A Gas chromatography-tandem mass spectrometry (GC-MS) method for quantitative analysis of acetochlor and s-metolachlor in maize and soybean straw has been developed, validated and applied to analyze the residues of anilide herbicides. Straw material was dried, homogenized and extracted with a mixture of n-hexane and acetone by an accelerated solvent extraction method. Chromatographic separation of the target analytes was performed on an Agilent 7832 GC equipped with a mass spectrometer detector, a split-splitless injector and an HP-5 MS (5% phenylmethyl siloxane) capillary column (30 m × 0.25 mm × 0.25 µm). Under these parameters, the limit of detection (LOD) values were 0.2 ng g−1 for acetochlor and 0.07 ng g−1 for s-metolachlor, with average recoveries between 86% and 119.7%. The method was validated for acetochlor and s-metolachlor in maize and soybean straw at 0.5 and 0.01 mg kg −1. Furthermore, the final residues of the two herbicides in maize and soybean straw were below the maximum residue limit (MRL) at harvest time. The proposed method is suitable for routine analysis.

Application of Enzyme Digestion and Deconjugation Followed by Quick, Easy, Cheap, Effective, Rugged, Safe Extraction and Liquid Chromatography–Tandem Mass Spectrometry Methodology To Determine Ractopamine Residue in Pork

2018 ◽  
Vol 81 (8) ◽  
pp. 1258-1263 ◽  
Author(s):  
VANESSA GRESSLER ◽  
VIVIAN FEDDERN ◽  
JANE de OLIVEIRA PEIXOTO ◽  
MONICA CORREA LEDUR ◽  
OSMAR ANTONIO DALLA COSTA ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Sequential Analysis ◽  
Limit Of Detection ◽  
Residue Analysis ◽  
Tandem Mass ◽  
Method Performance ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

ABSTRACT A new methodology is proposed for ractopamine residue analysis in pork. It consists of enzyme-mediated digestion and deconjugation steps; modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction; and liquid chromatography–tandem mass spectrometry (LC-MS/MS). In brief, the samples were digested with protease and then deconjugated with β-glucuronidase enzyme; they were then subjected to extraction and cleanup by QuEChERS and underwent sequential analysis by LC-MS/MS. The method performance was evaluated in accordance to the validation guidelines regulated by the Brazilian Ministry of Agriculture and Food Supply. The limit of detection was 0.15 μg/kg and limit of quantification was 0.5 μg/kg. When the method was applied to real samples, ractopamine residue was found in concentrations (up to 7.86 μg/kg) below international recommendation limits up to 10 μg/kg. The method is sensitive, accurate, quick, simple, and suitable for routine analysis; therefore, it is a monitoring tool that may be adopted by laboratories to achieve compliance levels.

scholarly journals Gas Chromatography-Tandem Mass Spectrometry Method for Selective Detection of 2-Nitropropane in Mainstream Cigarette Smoke

2019 ◽  
Vol 28 (7) ◽  
pp. 300-309
Author(s):  
Gala M. Chapman ◽  
Juliana Giraldo Junco ◽  
Roberto Bravo Cardenas ◽  
Clifford H. Watson ◽  
Liza Valentín-Blasini
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Cigarette Smoke ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Standard Deviations ◽  
Mainstream Cigarette Smoke

SummaryAlthough 2-nitropropane is a potentially harmful compound present in cigarette smoke, there are few fully-validated, modern methods to quantitate it in mainstream cigarette smoke. We developed an isotope dilution gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) method for the detection of 2-nitropropane in mainstream cigarette smoke. The vapor fraction of mainstream cigarette smoke was collected in inert polyvinyl fluoride gas sampling bags and extracted with hexanes containing isotopically labeled internal standard, then purified and concentrated via solid-phase extraction using a normal phase silica adsorbent and a 100% dichloromethane eluant. This method is sensitive enough to measure vapor phase 2-nitro-propane concentrations in the nanogram range, with a 19 ng per cigarette method limit of detection. Product variability estimated from the analysis of 15 cigarette products yielded relative standard deviations ranging from 5.4% to 15.7%, and estimates of precision from two quality control products yielded relative standard deviations of 9.49% and 14.9%. Under the Health Canada Intense smoking regimen, 2-nitropropane in machine-generated mainstream smoke from 15 cigarette products ranged from 98.3 to 363 ng per cigarette.

scholarly journals Development and validation of an analysis method for pesticide residues by gas chromatography–tandem mass spectrometry in Daikenchuto

2021 ◽  
Author(s):  
Hirokazu Saegusa ◽  
Hiroshi Nomura ◽  
Masaki Takao ◽  
Takashi Hamaguchi ◽  
Masaru Yoshida ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Pesticide Residues ◽  
Residue Analysis ◽  
Herbal Medicines ◽  
Tandem Mass ◽  
Pesticide Residue Analysis ◽  
Analysis Method ◽  
Chromatography Tandem Mass Spectrometry

AbstractDaikenchuto (DKT) is one of the most widely used “Kampo” in Japan as a representative of herbal medicine. Because DKT is made from a natural product like food, it requires the management of pesticides; therefore, an analysis of residual pesticides in Kampo is required. The World Health Organization (WHO) indicates that pesticide residue analysis by the U.S. Pharmacopeia (USP) is required. USP defines 107 compounds containing organochlorine pesticides and organophosphorus pesticides and their metabolites, which have a high residual risk. Accordingly, to guarantee the safety of herbal medicines according to global standards is a very important issue. In this study, we developed an analytical method for 91 compounds, which are listed in USP, using DKT as the subject. The method could extract pesticides from DKT with acetone, elute pesticides with acetonitrile using a SepPak C18 column (5 g) and with ethyl acetate using a DSC-NH2 column (2 g), and perform simultaneous analyses by gas chromatography–tandem mass spectrometry (GC–MS/MS). This method, which could quantify 88 compounds, was validated according to USP. A pesticide residue analysis method that meets USP requirements enables the analysis of pesticide residues with a high residue risk and contributes to improving the safety of “Kampo” and other herbal medicines.

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