scholarly journals Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography

Molecules ◽  
2021 ◽  
Vol 26 (22) ◽  
pp. 6914
Author(s):  
Maria Suely Siqueira Ferraz ◽  
Lêda Rita D’Antonino Faroni ◽  
Fernanda Fernandes Heleno ◽  
Adalberto Hipólito de Sousa ◽  
Lucas Henrique Figueiredo Prates ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Agricultural Pests ◽  
Limit Of Quantification ◽  
Headspace Solid Phase Microextraction ◽  
Flame Ionization ◽  
Stored Grains ◽  
Main Component

Bioinsecticides are regarded as important alternatives for controlling agricultural pests. However, few studies have determined the persistence of these compounds in stored grains. This study aimed at optimizing and validating a fast and effective method for extraction and quantification of residues of safrole (the main component of Piper hispidinervum essential oil) in cowpea beans. It also sought to assess the persistence of this substance in the grains treated by contact and fumigation. The proposed method used headspace solid-phase microextraction (HS-SPME) and gas chromatography with a flame ionization detector (GC/FID). Factors such as temperature, extraction time and type of fiber were assessed to maximize the performance of the extraction technique. The performance of the method was appraised via the parameters selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. The LOD and LOQ of safrole were 0.0057 and 0.019 μg kg−1, respectively and the determination coefficient (R2) was >0.99. The relative recovery ranged from 99.26 to 104.85, with a coefficient of variation <15%. The validated method was applied to assess the persistence of safrole residue in grains, where concentrations ranged from 1.095 to 0.052 µg kg−1 (contact) and from 2.16 to 0.12 µg kg −1 (fumigation). The levels measured up from the fifth day represented less than 1% of the initial concentration, proving that safrole have low persistence in cowpea beans, thus being safe for bioinsecticide use. Thus, this work is relevant not only for the extraction method developed, but also for the possible use of a natural insecticide in pest management in stored grains.

scholarly journals Simultaneous Determination of Some Phenothiazine Derivatives in Human Blood by Headspace Solid-Phase Microextraction and Gas Chromatography with Nitrogen-Phosphorus Detection

2008 ◽  
Vol 91 (6) ◽  
pp. 1354-1362 ◽  
Author(s):  
Natsuko Shinmen ◽  
Xiao-Pen Lee ◽  
Takeshi Kumazawa ◽  
Chika Hasegawa ◽  
Yasuhiro Ishiwata ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Whole Blood ◽  
Solid Phase Microextraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Regression Equations ◽  
Phenothiazine Derivatives ◽  
Headspace Solid Phase Microextraction ◽  
Coefficients Of Variation

Abstract Chlorpromazine, levomepromazine, promazine, triflupromazine, and trimeprazine were simultaneously determined in human whole blood and plasma by combining headspace solid-phase microextraction and gas chromatography with nitrogenphosphorus detection. Extraction efficiency for the phenothiazine derivatives was 0.0130.117 for both sample types. Regression equations were linear [correlation coefficient (r) 0.99510.9999] within the range 2.5200 ng/0.5 mL for triflupromazine and trimeprazine, and 6.3200 ng/0.5 mL for chlorpromazine, levomepromazine, and promazine. The limit of detection for each compound was 0.23.9 ng/0.5 mL whole blood and plasma. Intraday and interday coefficients of variation for all phenothiazines in both human samples were commonly &lt;15 and 20, respectively. We also report the determination of levomepromazine in human plasma after oral administration.

scholarly journals Investigation on Furan Levels in Pressure-Cooked Foods

2013 ◽  
Vol 2013 ◽  
pp. 1-4 ◽  
Author(s):  
Adriana P. Arisseto ◽  
Eduardo Vicente ◽  
Maria Cecília F. Toledo
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Cold Storage ◽  
Food Processing ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Limit Of Quantification ◽  
Headspace Solid Phase Microextraction

Furan is a food processing contaminant classified as possibly carcinogenic to humans. As the occurrence of furan has been reported in a variety of foods processed in sealed containers, the objective of this work was to investigate if the contaminant can be found in home-cooked foods prepared in a pressure cooker. For that, several foods including beans, soy beans, whole rice, beef, pork, potato, and cassava were pressure-cooked and analyzed for the furan content by gas chromatography coupled to mass spectrometry preceded by a headspace solid phase microextraction (HS-SPME-GC/MS). Furan was not found above the limit of quantification in the pressure-cooked samples. No furan has either been found in reheated samples after 24 hours under cold storage. Although levels up to 173 μg/kg were already reported for commercial canned/jarred foods, it seems that the cooking in a pressure cooker may not represent a concern in relation to the occurrence of furan in foods.

scholarly journals Determination of Volatile Residual Solvents in Traditional Chinese Medicines by Headspace Solid-Phase Microextraction and Cryogenic Gas Chromatography with Flame Ionization Detection

2003 ◽  
Vol 86 (3) ◽  
pp. 461-466
Author(s):  
Jiemin Liu ◽  
Qunfang Zhou ◽  
Guibin Jiang ◽  
Jingfu Liu ◽  
Jiyan Liu ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Traditional Chinese Medicines ◽  
Flame Ionization Detection ◽  
Chinese Medicines ◽  
Headspace Solid Phase Microextraction ◽  
Residual Solvents ◽  
Flame Ionization

Abstract A method based on headspace solid-phase microextraction and cryogenic gas chromatography with flame ionization detection was developed for the determination of volatile residual solvents in traditional Chinese medicines. A laboratory-made cryogenic chromatographic system was used for the separation of 15 kinds of residual solvents. During the analysis, a 65 μm PDMS/DVB fiber was used to extract the residual solvents, the extraction time was controlled at 0°C for 15 min, and the NaCl content of the sample was maintained at 30%. The limits of detection ranged from 0.08 (for octane) to 5000 μg/L (for ethanol), and the relative standard deviations were &lt;8%. The recoveries from spiked samples ranged from 88 to 112%. Trace levels of residual solvents in several traditional Chinese medicines were effectively identified and quantified.

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