A QuEChERS-HPLC-MS/MS Method with Matrix Matching Calibration Strategy for Determination of Imidacloprid and Its Metabolites in Procambarus clarkii (Crayfish) Tissues

We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L−1, the limits of quantification were 0.05–2.0 μg·L−1 and the method of quantification was 0.05–2.0 μg·kg−1. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues.

Analysis and Evaluation of 7 Indictor Polychlorinated Biphenyls (PCBs) Residues in Dried Kelp by Gas Chromatography (GC)

In this study, a special method was developed for the determination of 7 kinds of polychlorinated biphenyls (PCBs) residues in dried kelp by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/dichloromethane (1/1, v/v) by ultrasonic extraction. Clean-up methods were used by concentrated sulphuric acid, neutral alumina oxide solid phase extraction cartridge and silica solid phase extraction cartridge. The analytical compounds were quantified by an internal standard method. Under optimal experimental conditions, good linearity was observed in the range of 5~200ng/mL, and the correlation coefficients were 0.9993~0.9998. The limit of quantification (LOQ) for target analytical compounds ranged from 6.0 to 7.5μg/kg. At the spiked levels of 10，20，50 μg/kg，the average recoveries ranged from 81.8% to 105% with the relative standard deviations 3.05%～11.2%. The result showed that the proposed method was accurate and could be used for the determination of the PCBs in dried kelp.

A New Class of β–Pyrrolidino-1,2,3-Triazole Derivatives as β-Adrenergic Receptor Inhibitors: Synthesis, Pharmacological, and Docking Studies

New 1,4-disubstituted β-pyrrolidino-1,2,3-triazoles were synthesized using a reusable copper-iodide-doped neutral alumina catalyst. Synthesis of diversely substituted triazoles and recyclability of CuI catalyst explains the broad scope of this protocol. The synthesized compounds were screened for their antimicrobial and anticancer properties. Most of the compounds showed significant antimicrobial activities against all the tested microorganisms compared to standard drugs. Furthermore, compounds 5a, 5e, 5g, 5h, 5i, and 5j showed moderate to potent activities against A549 and HepG-2 cells. In addition, compounds 5g and 5h displayed potential cytotoxicity activity against A549 cells with IC50 values of 72 ± 3.21 and 58 ± 2.31 µM, respectively. The molecular docking study revealed that some of the synthesized compounds exhibited comparable binding as co-crystalized ligands with the DNA topoisomerase IV and anaplastic lymphoma kinase receptors.

Antiproliferative activity of new 2-glyco-3-nitro-1,2-dihydroquinolines and quinolines synthesized under solventless conditions promoted by neutral alumina

This paper describes the syntheses of new 2-glyco-3-nitro-1,2-dihydroquinolines and 2-glyco-3-nitroquinolines by one-pot aza-Michael–Henry-dehydration reactions using green procedures, as well as the evaluation of their antiproliferative activity.

Amino-functionalized graphene oxide/neutral alumina nanocomposite based solid-phase extraction coupled with ion chromatography-mass spectrometry for the determination of trace haloacetic acids in drinking water

An efficient solid-phase extraction strategy was developed for the extraction and enrichment of ten haloacetic acids from drinking water.

Synthesis of Sulfonyldiazomethanes and Acetyldiazomethanes via an Alumina-Mediated Decarboxylation Strategy

Diazo compounds are widely adopted in organic synthesis due to their carbine characteristics. One of the most interesting diazo compounds is diazolsulfonyl. Here, in the current study, we found that diazolsufonyl compounds could be prepared with moderate to excellent yield through decarboxylation of diazosulfonyl acetates by neutral alumina. We hope that this mild and simple method might inspire wider application of these useful compounds.