ABSTRACT
In this study, we have synthesized a series of ZSM-11 zeolite catalysts using tetrapropyl ammonium hydroxide as a structure-directing agent through a highly efficient hydrothermal method. The series of catalysts were studied by different techniques such as FT-IR spectroscopy, XRD, FE-SEM, HR-TEM, EDS, pyridine-FT-IR spectroscopy, and BET analysis. We focused on varying reaction time intervals from 18 to 48 hours to investigate the effect on catalytic activities of the synthesized series of catalysts. The percentages of aluminum increased in the framework of zeolites with increasing crystallinity, surface area, external surface area, and acidity in the series of ZSM-11 zeolites by increasing the time from 18 to 48 h. Then, we studied the catalytic activity of a series of ZSM-11 zeolites and found that the ZSM-11 zeolite (48 h) possesses higher catalytic activity towards the synthesis of 1,2,4,5-tetrasubstituted imidazoles under solvent-free conditions. The present protocol scored well with excellent yield, short reaction time, clean reaction profiles, low catalyst loading, and no tedious workup. The catalyst (ZSM-11 zeolite 48 h) was recycled and reused in five runs without any considerable loss of activity and product yield.
ABSTRACT
A novel screening and quantitation method is reported for non-target multiresidue analysis of pesticides using ultra-HPLC-quadrupole-Orbitrap mass spectrometry in spice matrices, including black pepper, cardamom, chili, coriander, cumin, and turmeric. The method involved sequential full-scan (resolution = 70,000), and variable data independent acquisition (vDIA) with nine consecutive fragmentation events (resolution = 17,500). Samples were extracted by the QuEChERS method. The introduction of an SPE-based clean-up step through hydrophilic-lipophilic-balance (HLB) cartridges proved advantageous in minimizing the false negatives. For coriander, cumin, chili, and cardamom, the screening detection limit was largely at 2 ng/g, while it was 5 ng/g for black pepper, and turmeric. When the method was quantitatively validated for 199 pesticides, the limit of quantification (LOQ) was mostly at 10 ng/g (excluding black pepper, and turmeric with LOQ = 20 ng/g) with recoveries within 70-120%, and precision-RSDs <20%. Furthermore, the method allowed the identification of suspected non-target analytes through retrospective search of the accurate mass of the compound-specific precursor and product ions. Compared to LC-MS/MS, the quantitative performance of this Orbitrap-MS method had agreements in residue values between 78-100%.
