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1.
J Chromatogr A ; 1709: 464407, 2023 Oct 25.
Artigo em Inglês | MEDLINE | ID: mdl-37748352

RESUMO

Due to lack of chromogenic groups and fluorescence groups, high boiling point, high polarity, low volatility, and small molecular weight of glyphosate, glufosinate and bentazone, the detection of three analyses were limited in all kinds of food. Herein, a method for the simultaneous determination of glyphosate, glufosinate and bentazone in tea by ion chromatography tandem triple quadrupole mass spectrometry (IC-MS) was developed, which is without organic solvent and complex derivatization. The recoveries of three compounds in different teas (black tea, green tea, white tea) ranged from 80.40 % to 107.00 %, and the intraday precision (n = 6) ranged from 0.57 % to 9.90 %, the daytime precision ranged from 1.00 % to 5.30 %, the quantitative limit (LOQ) ranged from 0.36 to 1.30 µg/L, and the detection limit (LOD) ranged from 0.11 to 0.39 µg/L. Furthermore, the detection limit and quantitative limit of glyphosate, glufosinate and bentazone by this method are lower than other methods in real samples. Meanwhile, the established method was successfully applied to determine the terminal residues of the three analytes in twelve tea samples from commercial market. Therefore, this method can provide reliable technical support for the study of residue status in vegetables and fruits.


Assuntos
Herbicidas , Herbicidas/análise , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida/métodos , Chá/química
2.
J Hazard Mater ; 452: 131176, 2023 06 15.
Artigo em Inglês | MEDLINE | ID: mdl-36948118

RESUMO

Microorganisms have difficulty surviving and performing remediation functions in mixed systems with high concentrations of Pb and Cd. Biochar has the potential to assist microorganism remediation as an excellent adsorbent for heavy metals. In this study, pig manure biochar (PMB) was used to assist phosphorus solubilizing bacteria (PSB) to explore the mineralization protection and biofeedback mechanism of biochar on PSB under mixed stress of 1000 mg/L Pb2+ and 500 mg/L Cd2+. The adsorption results showed that the removal of Pb2+ and Cd2+ by PMB+PSB was 148.77% and 72.27% higher than that by PSB. Meanwhile, the non-bioavailable fraction of Cd2+ and acid-soluble fraction of Pb2+ in PMB+PSB were increased by 9% and 3%, respectively. Mineralogical and microbial secretion results confirm that showed that the acidic soluble fraction and non-bioavailable fraction were mostly Pb/Cd-carbonate and Pb/Cd-phosphate. The pore adsorption and precipitation (carbonate) of biochar were able to reduce the exposure of PSB to Pb/Cd and the background stress concentration, thus stimulating the biological positive feedback effect of PSB and forming a microenvironment in the cell periphery. The vesicle detoxification and extracellular polymeric substance protection mechanism of PSB were improved under biochar protection, and the individual size and activity of PSB cells were enhanced. Besides, citric acid release from PSB (28.85% increase) accelerated the dissolution of unstable Cd-carbonate, thereby releasing a large amount of Cd2+ to compete with Pb2+ for PO43-. Thus, the protection of biochar and the positive feedback effect of PSB could reduce the biotoxicity of Cd2+ in the stress system by preferentially forming a stable Cd-phosphate. In addition, the excellent electrical conductivity and organic material adsorption of biochar increased the extracellular electron transport rate of microorganisms, which further accelerated the mineralization and immobilization of Pb2+ and Cd2+, so as to ensure the repair effect of PSB on heavy metals.


Assuntos
Metais Pesados , Poluentes do Solo , Animais , Suínos , Fosfatos , Cádmio/análise , Chumbo , Transporte de Elétrons , Elétrons , Matriz Extracelular de Substâncias Poliméricas/química , Poluentes do Solo/análise , Solo , Carvão Vegetal , Fósforo , Metais Pesados/análise , Bactérias
3.
J Chromatogr Sci ; 61(1): 38-55, 2022 Dec 29.
Artigo em Inglês | MEDLINE | ID: mdl-35373835

RESUMO

The aim of this study was to establish a comprehensive strategy based on liquid chromatography coupled with mass spectrometry to potently identify as many compounds of Chinese patent medicine as possible. Ultrahigh performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q/TOF-MS) was used to qualitatively analyze the Chinese patent medicine Xiao'er Chiqiao Qingre Granules (XCQG), which is recorded in the Chinese Pharmacopoeia. A novel strategy, including targeted, semi-targeted and non-targeted identification, was built to explore the compounds based on accurate mass, characteristic fragments, retention time of standard substances, databases or literature. Based on the integrated identification, 250 compounds were identified in total, including 7 alcohols, 3 aldehydes, 17 alkaloids, 9 amino acids, 10 coumarins, 30 flavonoids, 29 glycosides, 12 ketones, 7 lignans, 20 organic acids, 12 phenols, 11 phenylpropanoids, 9 quinones, 3 steroids, 26 terpenes, 14 volatile oils and 31 other compounds. A novel strategy for the identification of compounds in traditional Chinese medicine (TCM) was developed with Ultrahigh performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q/TOF-MS). It is also the first systematic study of compounds in XCQG, laying a foundation for further mechanism research of XCQG. More importantly, the strategy shows good application prospect in identifying compounds of TCM.


Assuntos
Medicamentos de Ervas Chinesas , Medicamentos de Ervas Chinesas/química , Cromatografia Líquida de Alta Pressão/métodos , Glicosídeos/análise , Espectrometria de Massas , Medicina Tradicional Chinesa
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