scholarly journals DEVELOPMENT OF ANALYTICAL METHOD FOR THE DETERMINATION OF TRIAZOLE AND PYRETROID PESTICDES IN MUSTARD GREENS (Brassicajuncea)

2017 ◽  
Vol 126 (1C) ◽  
pp. 5
Author(s):  
Nguyễn Đăng Giáng Châu

<p><strong>Abstract</strong><strong></strong></p><p>            Triazole and pyrethroid are two of the most commonly used pesticides in vegetable cultivation recently. In this study, a multi-residue analytical method employing gas chromatography – mass spectromety (GC-MS) technique was successfully developed for quantification of two triazole fungicides including propiconaozle and difenoconazole and on pyrethroid insecticide cypermethrin (including 04 isomeres) in mustard greens. The GC-MS running program performed good separation, low detection limit and short analysis time (24 minutes). Target compounds in mustard green sample were ultrasonically extracted in 15 minutes by 60 mL acetone, followed by clean-up steps using solid phase extraction of packed activated carbon column with 40 mL acetone:toluene (v:v, 1:1) for elutions, and florisil cartridge with an elution mixture of 15 mL acetone:n-hexane (v:v, 1:5). The method was validated before applying for a preliminary screening of triazole and pyrethroid residue levels in mustard greens collected in Phu Yen Province, Vietnam.</p><p><strong><em>Keywords:</em></strong> triazole, pyrethroid, residues in vegetables, GC-MS</p>

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Bui Van Hoi ◽  
Cam-Tu Vu ◽  
Lan-Anh Phung-Thi ◽  
Thao Thi Nguyen ◽  
Phuong Thanh Nguyen ◽  
...  

In this study, an analytical method for the simultaneous determination of 7 major pharmaceutical residues in Vietnam, namely, carbamazepine, ciprofloxacin, ofloxacin, ketoprofen, paracetamol, sulfamethoxazole, and trimethoprim, in surface water and hospital wastewater has been developed. The method includes enrichment and clean-up steps by solid phase extraction using mix-mode cation exchange, followed by identification and quantification using an ultrahigh-performance liquid chromatography and tandem mass spectrometry and employing electrospray ionization (UPLC-ESI-MS/MS). Seven target compounds were separated on the reversed phase column and detected in multiple reaction monitoring (MRM) mode within 6 minutes. The present study also optimized the operating parameters of the mass spectrometer to achieve the highest analytical signals for all target compounds. All characteristic parameters of the analytical method were investigated, including linearity range, limit of detection, limit of quantification, precision, and accuracy. The important parameter in UPLC-ESI-MS/MS, matrix effect, was assessed and implemented via preextraction and postextraction spiking experiments. The overall recoveries of all target compounds were in the ranges from 55% to 109% and 56 % to 115% for surface water and hospital wastewater, respectively. Detection limits for surface water and hospital wastewater were 0.005–0.015 µg L−1 and 0.014–0.123 µg L−1, respectively. The sensitivity of the developed method was allowed for determination of target compounds at trace level in environmental water samples. The in-house validation of the developed method was performed by spiking experiment in both the surface water and hospital wastewater matrix. The method was then applied to analyze several surface water and hospital wastewater samples taken from West Lake and some hospitals in Vietnam, where the level of these pharmaceutical product residues was still missed. Sulfamethoxazole was present at a high detection frequency in both surface water (33% of analyzed samples) and hospital wastewater (81% of analyzed samples) samples.


2017 ◽  
Vol 9 (15) ◽  
pp. 2284-2289 ◽  
Author(s):  
F. A. Soares ◽  
S. C. Chiapetta ◽  
W. F. Pacheco

In this paper an analytical method was developed for the determination of some tobacco specific N-nitrosamines (TSNAs) in cigarettes, and applied to cigarettes purchased in the city of Rio de Janeiro/RJ (Brazil).


2017 ◽  
Vol 9 (46) ◽  
pp. 6499-6506 ◽  
Author(s):  
Lanling Chu ◽  
Jianjun Deng ◽  
Xuejun Kang

A sensitive analytical method based on packed-nanofiber solid phase extraction (PFSPE) and high performance liquid chromatography (HPLC) has been developed for determining chloramphenicol (CAP) in milk.


2013 ◽  
Vol 106 ◽  
pp. 363-367 ◽  
Author(s):  
Fábio de Souza Dias ◽  
Josemário Santana Bonsucesso ◽  
Lucylia Suzart Alves ◽  
Domingos Correia da Silva Filho ◽  
Antonio Celso Spínola Costa ◽  
...  

2014 ◽  
Vol 12 (9) ◽  
pp. 928-936 ◽  
Author(s):  
Yassine Kadmi ◽  
Lidia Favier ◽  
Isabelle Soutrel ◽  
Marguerite Lemasle ◽  
Dominique Wolbert

AbstractN-nitrosamines are a new class of emerging nitrogenous drinking water disinfection by-products. These compounds are probably carcinogenic which could seriously affect the safety of drinking water consumers. The aim of this study is to develop a simple, fast, and specific analytical method for the routine determination of low part per trillion levels of N-nitrosamines in waters. An ultra high pressure liquid chromatography coupled with tandem mass spectrometry (UHPLC/MS/MS) method was developed for the qualitative and quantitative analysis of N-nitrosamines in waters. N-nitrosamines were extracted, purified and concentrated from water samples in one step using a solid-phase extraction (SPE). The compounds were detected in multiple reaction monitoring via electrospray ionisation source with positive ionisation mode. To achieve symmetrical peak shapes and a short chromatographic analysis time, the mobile phase consisting of acetonitrile, water and formic acid (60:40:0.1, v/v/v) was used in the experiment. Chromatographic separation of N-nitrosamines was done in less than two minutes. All calibration curves had good linearity (r2≥ 0.9989). The intra- and inter-day precision of the assay ranged from 0.59% to 3.11% and accuracy ranged from 99.66% to 104.1%. The mean recoveries of N-nitrosamines in spiked water were 98%-101%. The reproducability was acceptable with relative standard deviations of less than 3.53%. The proposed method yielded detection limits very low which ranges from 0.04 to 0.16 ng L−1. Finally, the developed analytical method was successfully applied to the analysis of N-nitrosamines in natural water sample


Foods ◽  
2021 ◽  
Vol 10 (9) ◽  
pp. 2090
Author(s):  
Sung-Min Cho ◽  
Han-Sol Lee ◽  
Ji-Su Park ◽  
Su-Jung Lee ◽  
Hye-Sun Shin ◽  
...  

A rapid and simple analytical method for triflumezopyrim, a new class of mesoionic insecticides and commercialized molecules from DuPont, was developed with a modified QuEChERS method. The pH adjustment was used to improve the extraction efficiency of acetonitrile solvent, and dispersive solid-phase extraction was employed for the clean-up process. The five selected food commodities were used to verify the present optimized method, which displayed good linearity with an excellent correlation coefficient (R2 = 0.9992–0.9998) in the 0.003–0.30 mg/kg calibration range. The method limits of detection (LOD) and quantification (LOQ) were determined to be a value of 0.003 and 0.01 mg/kg, respectively. The mean recovery for the triflumezopyrim was in the 89.7–104.3% range. The relative standard deviations were ≤9.8% for intra- (n = 5) and inter-day (n = 15) precisions at concentrations of 0.01, 0.1, and 0.5 mg/kg in the five representative samples. The matrix effect has been calculated to confirm the effect during ionization of the analyte in the UPLC-MS/MS. The matrix effects of the instrumental analysis showed that triflumezopyrim was less susceptible to matrices. The proposed analytical method in this study has effectively improved the accuracy, selectivity, and sensitivity for the determination of triflumezopyrim in agricultural commodities; therefore, it can serve as a reference method for the establishment of maximum residue limits (MRLs).


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