scholarly journals Multiresidue Method for Analysis of 240 Pesticides in Soils of Tomato Planting by Ultra Performance Liquid Chromatography Coupled to Mass Spectrometry

2021 ◽  
pp. 34-67
Author(s):  
João Roberto Fortes Mazzei ◽  
Estevão Freire ◽  
Eduardo Gonçalves Serra ◽  
José Ronaldo de Macedo ◽  
Angélica Castanheira de Oliveira ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
Ultra Performance Liquid Chromatography ◽  
Soil Samples ◽  
Good Precision ◽  
Solution Ph ◽  
Ionization Source ◽  
Soil Extracts ◽  
Validation Parameters

In this work, an analytical method for the determination of residues for the pesticides-focus was optimized: Azoxystrobin, Boscalide, Carbendazim, Chloranthranilprole, Clothianidin, Diafentiuron, Difenoconazole, Dimetomorfe, Espinetoram, Espinosade A, Espinosade D, Fenurox, Metalaxyl M, Methoxyfenozide, Tiametoxan in soil derived from tomato planting, in order to compare the levels of contamination of these compounds in soil samples. The modified QuEChERS extraction method and Ultra Performance Liquid Chromatography coupled with Sequential Mass Spectrometry were used, with ionization source by Electronebulization in ESI mode (+/-). The method consisted of extracting 15.0 g of soil with 15 ml of saturated calcium hydroxide solution pH 12.3 and 15 ml of acetonitrile, with a consequent partition in the “salting out” effect through 6.0 g of sulfate of anhydrous magnesium and 1.5 g of sodium chloride. The phases were separated by centrifugation at 3700 rpm for 7 min. The extracts were diluted with MeOH licrossolv® grade and injected in a chromatograph. The method was validated based on the parameters of linearity, LOD, LOQ, precision and accuracy. Linearity between 0.2 and 20.0 µg L-1, determination coefficients greater than 0.99. The LOQ values ​​for the method were 13 µg kg-1 for Spinosad and 7.0 µg kg-1 for the other pesticides. The method showed good precision, with RSD values ​​<20%, and accuracy, with recoveries between 70 and 120% for the vast majority of the analyzed compounds. The analytical curves were prepared with reference white soil extracts, in order to minimize the Matrix Effect. The method was considered adequate for the analysis of pesticide residues in soil, since it satisfies the validation parameters of chromatographic methods (European Commission, 2018). After validation, the method was used to analyze the residues of these pesticides in soil samples from conventional, organic and sustainable tomato plantations. Making it possible to compare the levels of environmental impacts generated. In addition to validating the analytical method for the pesticides-focus of the study, it was also possible to validate 240 more compounds, between authorized and unauthorized for use in tomato planting.

Determination of Residues of Cyantraniliprole and Its Metabolite J9Z38 in Watermelon and Soil Using Ultra-Performance Liquid Chromatography/Mass Spectrometry

2013 ◽  
Vol 96 (6) ◽  
pp. 1448-1452 ◽  
Author(s):  
Xiuqing Hu ◽  
Changpeng Zhang ◽  
Yahong Zhu ◽  
Min Wu ◽  
Xiaoming Cai ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Silica Gel ◽  
Ultra Performance Liquid Chromatography ◽  
Soil Samples ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

Abstract A method was developed for the determination of cyantraniliprole (HGW86) and its metabolite J9Z38 in watermelon and soil by ultra-performance LC (UPLC)/MS/MS. Target compounds were extracted by acetonitrile–water, cleaned up on a silica gel column, and determined by UPLC/MS/MS. Average recoveries of cyantraniliprole and J9Z38 in watermelon and soil at three levels (0.01, 0.1, and 0.5 mg/kg) ranged from 85.71 to 105.74%, with RSDs of 0.90–6.34%. The LOQs for cyantraniliprole and J9Z38 were determined to be 0.00021, 0.00015, 0.0010, and 0.00090 mg/kg in watermelon and soil samples, respectively. This method was used to determine the cyantraniliprole and J9Z38 residues in watermelon and soil samples for studies on their dissipation. The trial results showed that the half-lives of cyantraniliprole obtained after treatments were 1.1 and 4.1 days in watermelon and soil in Zhejiang, and 2.7 and 2.6 days in watermelon and soil in Hunan, respectively. The average levels of cyantraniliprole and J9Z38 residues in watermelon and soil were all &lt;0.01 mg/kg within the 14-day interval after treatment.

Quantitative Determination of Alkaloids from Roots of Hydrastis canadensis L. and Dietary Supplements Using Ultra-Performance Liquid Chromatography with UV Detection

2012 ◽  
Vol 95 (5) ◽  
pp. 1398-1405 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Ikhlas A Khan
Keyword(s):  
Acetic Acid ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Analytical Method ◽  
Ultra Performance Liquid Chromatography ◽  
Uv Detection ◽  
Mass Analyzer ◽  
Ionization Source ◽  
Hydrastis Canadensis ◽  
Acquity Uplc

Abstract Ultra-performance liquid chromatography (UPLC) with UV detection was used for the quantification of alkaloids from roots of Hydrastis canadensis L. (goldenseal) and dietary supplements claiming to contain goldenseal. The analysis was performed on a Waters Acquity UPLC system with an Acquity UPLC BEH Shield RP18 column using gradient elution with ammonium formate and acetonitrile containing formic acid. The chromatographic run time was less than 6 min. The detection wavelength used for β-hydrastine and canadine was 290 nm; for hydrastinine, coptisine, jatrorrhizine, palmatine, and berberine, it was 344 nm. A total of five different extraction solvents, including 100% methanol, 90% methanol, 90% methanol + 1% acetic acid, 90% acetonitrile + 0.1% phosphoric acid, and 100% acetonitrile, were tested for recovery of the major compounds. The samples extracted with the 90% methanol + 1% acetic acid displayed the best recovery (&gt;97%). The analytical method was validated for linearity, repeatability, LOD, and LOQ. The RSDs for intraday and interday experiments were less than 3.5%, and the recovery was 98–103%. UPLC/MS with a quadrupole mass analyzer and electrospray ionization source was used to confirm the identity of seven alkaloids. The analytical method was successfully applied to confirm the identification of seven alkaloids from the roots of H. canadensis, dietary supplements that claimed to contain goldenseal, and possible adulterant species.

Simple high-throughput analytical method using ultra-performance liquid chromatography coupled with tandem mass spectrometry to quantify total 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol in urine

2015 ◽  
Vol 53 (8) ◽  
Author(s):  
Jun-Young Yang ◽  
Hyun-Kyong Ahn ◽  
Si-Won Lee ◽  
You-Jung Han ◽  
Young-Jun Oh ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Throughput ◽  
Tobacco Smoke ◽  
Analytical Method ◽  
Ultra Performance Liquid Chromatography ◽  
Urinary Concentration ◽  
Tandem Mass ◽  
Biomarker Of Exposure

AbstractSince the urinary concentration of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) is a reliable biomarker of exposure to tobacco smoke, we developed a relatively simple high-throughput chromatographic method to quantify total urinary NNAL concentrations in the general population.The high-throughput analytical method was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) to identify and quantify total urinary NNAL concentrations in 10 non-smokers and 15 otherwise healthy smokers.Loss of nitric oxide atAn UPLC-MS/MS analytical method to quantify total urinary NNAL concentrations in smokers that does not require sample derivatization is presented herein. The method could be useful in clarifying the toxicities associated with human exposure to cigarette smoking. However, quantification might be adversely affected by co-eluting interfering compounds or selective ion suppression or enhancement as a result of having only one ion transition to monitor NNAL and NNAL-methyl-

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