Pesticides Analysis in Beans by Gas Chromatography Couplet with Tandem Mass Spectrometry

2021 ◽  
Vol 6 (4) ◽  
Author(s):  
Mizutani G ◽  
◽  
Bustillos O ◽  
Keyword(s):  
Gas Chromatography ◽  
Analytical Method ◽  
Extraction Procedure ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Mineral Salts ◽  
Pesticides Residues ◽  
Solid Liquid ◽  
Validation Of Analytical Method ◽  
Iron And Calcium

Beans are part of the basic diet alimentation for Brazilian population, as they gather proteins, carbohydrates, vitamins, mineral salts, fibers, amino acids and essential nutrients such as iron and calcium, being a complete food that can be compared with the amount of protein that the meat has. Considering the beans world production, in development countries represent almost 50%, being that Myanmar, India and Brazil the top three position. The use of pesticides is widely spread in these countries to reduce agricultural losses due to pests that interfere with grain production. Therefore the risk that could be generated from foods pesticides residues makes their analyses of quantification mandatory. The purpose of this work was to develop an analytical method to quantitatively characterize fungicides pesticides residues, flutriafol, procymidone and tebuconazole that were used to angular spot control, anthracnose, rust and alternaria spot, white mold fungi, present in beans, by means of gas chromatography coupled with a triple quadrupole mass spectrometer. Samples of beans, Phaseolus vulgaris L, types white, black, string and Vigna angularis, type adzuki, had been bought in grains store and supermarkets at metropolitan São Paulo city. The validation of analytical method was explored for sensitivity, selectivity, precision. The extraction procedure was performed in two different forms, QuEChERS, and solid-liquid extraction with low temperature. Through this methodology, reached below the maximum limit allowed by Brazilian law 0.5mgkg-1 for procymidone and 0.1mgkg-1 for flutriafol and tebuconazole. Several samples of four types of beans were tested and all of them had procymidone identified and 7% of samples higher than the law limit.

scholarly journals VALIDATION OF ANALYTICAL METHOD OF 2,5-HEXANEDIONE ON URINE BY GAS CHROMATOGRAPHY

2019 ◽  
pp. 320-324
Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
Kurnia Megawati ◽  
Febrina Amelia Saputri ◽  
Mulyana Mulyana
Keyword(s):  
Gas Chromatography ◽  
Analytical Method ◽  
Gas Flow ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Flame Ionization ◽  
System Suitability ◽  
Study Results ◽  
Validation Parameters ◽  
Validation Of Analytical Method

Objective: The purpose of this study was to obtain a valid analytical method for determining the level of 2,5-hexanedione in the urine of oil industry workers. Methods: Gas Chromatography (GC) was employed to analyze 2,5-hexanedione in the urine. The analysis was done using HP-5 (Crosslinked methyl siloxane) capillary columns 30 m x 0.320 mm long, film thickness 0.25 μm. The temperature of the detector temperature was 300 °C, and the injector temperature was 250 °C. The helium gas flow rate was 2 ml/min. The detector was Flame Ionization Detection (FID). Parameters of system suitability test and validation were obtained. Results: This study results that the method of analysis 2,5-hexanedione in urine by Gas Chromatography (GC) confirm the requirements of the validation method with a linearity was 0.99963, accuracy was in the range of 99.16% to 114.13%, the precision with % coefficient of variation was 1.65% to 5.16%, % coefficient variation of specificity was 0.027%, limit of detection was 0.054 μg/ml and limit of quantification was 0.18 μg/ml. Conclusion: The proposed GC method meets the acceptance criteria of validation parameters and can be applied for routine analysis.

Fractionation of Salad Dressings for Fatty Acid Profile and Soluble Sugar Determination Using the Ultracentrifuge

1994 ◽  
Vol 77 (6) ◽  
pp. 1539-1541 ◽  
Author(s):  
Anasuya S Patel
Keyword(s):  
Gas Chromatography ◽  
Fatty Acid ◽  
Analytical Method ◽  
Sugar Content ◽  
Soluble Sugar ◽  
Extraction Procedure ◽  
Small Samples ◽  
Fatty Acid Profiles ◽  
Ether Extraction ◽  
Aqueous Layer

Abstract An analytical method was developed for fractionating small samples of salad dressing for fatty acid profiles and soluble sugar content by using an ultracentrifuge. The extracted oils were characterized and compared with those obtained by the official AOAC ether extraction procedure. Both methods gave similar results for fatty acid profiles and oil recoveries. The fatty acid profiles were determined by gas chromatography. In addition, the sugar content of the aqueous layer of the centrifuged samples could easily be obtained by refractometry. The proposed method is time and labor efficient and eliminates the use of hazardous and flammable ether.

Optimization and Analysis of Acid Treated Trimethylamine using Surface Response and Gas Chromatography Analytical Methods

2020 ◽  
Vol 16 (5) ◽  
pp. 631-640 ◽  
Author(s):  
Seul-Ki Park ◽  
Fazlurrahman Khan ◽  
Yeon-Jin Cho ◽  
Dong-Lee Hong ◽  
Yu-Mi Jang ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Analytical Method ◽  
Analytical Methods ◽  
Acid Treatment ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Control Group ◽  
Optimum Conditions ◽  
Fish Products ◽  
Naoh Solution

Background: Trimethylamine (TMA) is a nitrogenous base aliphatic organic compound accounting for the odor of rotten fish and it is used as an indicator for analyzing the quality of fish products. Introduction: Extraction procedures and analytical methods including colorimetric and Gas- Chromatography (GC) can quantify the TMA contents of fish products after pre-treatment with basic solutions. However, the extraction procedure and analytical methods for acid-treated samples are not known, despite the majority of fish products being preserved using acid preservatives. Methods: The methodologies used included solid-phase micro-extraction of TMA followed by its quantification by a GC-based analytical method. An analysis of response surface methodology was also conducted to verify the optimum conditions for TMA detection in acid-treated liquid samples affected by factors including trapping time, temperature, and stirring speed. Results: The results obtained from this study showed that the optimum conditions for the best yield of TMA extraction are 20 min of trapping, emission at 55°C, and stirring at 400 rpm. The validation of the developed method was carried out using rotten fish after acid treatment. Acid treatment decreased TMA by up to 73.01%, however, when adding NaOH solution of the same volume to the samples, TMA increased similar to the control group. Conclusion: Here, we report a simple, sensitive, and rapid extraction procedure. A GC-based analytical method was developed for the analysis of TMA from the acid-treated sample. The developed extraction procedure and analytical methods were optimized and validated, which could be helpful for the extraction of TMA without damaging the sample.

scholarly journals Determination of Volatile Fuel Oxygenates in Water by Gas Chromatography–Triple Quadrupole Mass Spectrometry: Effect of Automated Sample Preparation Techniques

Water ◽  
2020 ◽  
Vol 12 (8) ◽  
pp. 2266
Author(s):  
Kai Zhu ◽  
Yucan Liu ◽  
Qing Sun ◽  
Min Zhao ◽  
Lihua Huang
Keyword(s):  
Aromatic Compounds ◽  
Solid Phase ◽  
Detection System ◽  
Extraction Procedure ◽  
Triple Quadrupole ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Ms Detection ◽  
Gasoline Additives

Considering the adverse effects of gasoline additives and aromatic compounds on the quality of the water supply and the ecological environment of the water, a methodology, with short chromatographic separation time (22.5 min) and high separation quality, was optimized for the determination of 11 common gasoline additives and aromatic compounds using gas chromatograph coupled with triple quadrupole mass spectrometer (GC–QqQ–MS/MS) system. The extraction procedure of analytes was performed by headspace solid–phase microextraction (HS–SPME) and purge and trap (P&T), respectively. Both of the two extraction methods provided excellent chromatographic resolution in subsequently GC–QqQ–MS/MS detection system, with the coefficients of linear regression of the calibration curves with HS–SPME and P&T pretreatments were 0.9965~0.9998 and 0.9961~0.9999, respectively, n = 7. The limit of detections (LODs) of these selected oxygenate compounds were discovered to be 0.52~32 ng/L in the P&T–GC–QqQ–MS/MS detection system and 0.11~151 ng/L in the HS–SPME–GC–QqQ–MS/MS detection system. For benzene, toluene, ethylbenzene and xylene isomers (BTEX), the HS–SPME–GC–QqQ–MS/MS system provided outstanding detection performance because of the lower LOD obtained. However, for other selected compounds, the P&T–GC–QqQ–MS/MS system offered lower LODs. The proposed extraction–detection procedure is a simple and sensitive analytical approach for the detection of gasoline additives and aromatic compounds in water.

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