RESUMO
An effective and sensitive analytical method was developed to quantify the most common pesticide residues (difenoconazole, dimethoate, pymetrozine, and chlorantraniliprole) used for brinjal cultivation in Bangladesh. The quantification of the analytes was done using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using a modified QuEChERS method and followed by purification with dispersive solid phase extraction (d-SPE) sorbents (PSA, GCB, and C18). Matrix-matched calibration with a regression coefficient R2 ≥ 0.9964 were used to minimize the brinjal matrix effect. The method was validated in quintuple (n = 5) at five different spiked levels (8-400 µg/kg) having recoveries in the range of 70.3-113.2% with relative standard deviations RSDs ≤6.8%, limits of detection (LOD) and limits of quantification (LOQ) was in the range of 0.15-0.66 µg/kg and 0.4-2.0 µg/kg, respectively, for the four analytes. A total 100 samples (50 samples directly from fields of Jessore district, Bangladesh and 50 samples from local market of Dhaka, Bangladesh) were collected to analyse the pesticides residue. The result showed that pesticides residue was found in both the field and market collected samples, 54% and 38%, respectively. The overall mean residue levels of four pesticides in field samples were significantly higher than those of market samples. Moreover, 20% of the field samples and 10% of the market samples had dimethoate residues, which were the most abundant among the four analytes and it ranged from 0.017 to 0.252 mg/kg. In terms of health risk assessments, dimethoate showed the highest estimated daily intake (EDI) and hazard quotient (HQ) values that are 3.02 × 10-5 mg/kg/day and 1.51%, respectively, in field samples. Till now, there have been no regulations or guidelines for the maximum admissible pesticide residue in Bangladesh. Therefore, the above findings will be an initial step for the regulatory authorities of Bangladesh to implement regulations and guidelines for pesticide usage.
RESUMO
Graphene oxide (GO) was prepared from the graphite electrode of waste dry cells, and the application of the prepared GO as a potential adsorbent for rapid and effective removal of an antibiotic, azithromycin (AZM), has been investigated. The synthesis process of GO is very simple, cost-effective, and eco-friendly. As-prepared GO is characterized by field-emission scanning electron microscopy, energy-dispersive X-ray, transmission electron microscopy, X-ray diffractometry, Fourier transform infrared spectroscopy, elemental analysis, Brunauer-Emmett-Teller sorptometry, and zeta potential analysis. The obtained GO has been employed for removal of the widely used AZM antibiotic from an aqueous solution. The quantitative analysis of AZM before and after adsorption has been carried out by liquid chromatography tandem mass spectrometry. The adsorption of AZM by GO was performed in a batch of experiments where the effects of adsorbent (GO) dose, solution pH, temperature, and contact time were investigated. Under optimum conditions (pH = 7.0, contact time = 15 min, and adsorbent dose = 0.25 g/L), 98.8% AZM was removed from the aqueous solution. The rapid and effective removal of AZM was significantly controlled by the electrostatic attractions and hydrogen bonding on the surface of GO. Adsorption isotherms of AZM onto GO were fitted well with the Freundlich isotherm model, while the kinetic data were fitted perfectly with the pseudo-second order. Therefore, the simple, cost-effective, and eco-friendly synthesis of GO from waste material could be applicable to fabricate an effective and promising low-cost adsorbent for removal of AZM from aqueous media.