Fluorinated-Squaramide Covalent Organic Frameworks for High-Performance and Interference-Free Extraction of Synthetic Cannabinoids.

Synthetic cannabinoids (SCs), one of the largest groups of new psychoactive substances (NPSs), have emerged as a significant public health threat in different regions worldwide. Analyzing SCs in water samples is critical to estimate their consumption and control. However, due to their low background concentration and the coexistence of complex matrix, the selective and effective enrichment of SCs is still challenging. In this study, a series of fluorinated-squaramide-based covalent organic frameworks (COF: FSQ-2, FSQ-3, and FSQ-4) are synthesized, and the as-prepared FSQ-4 exhibits strong affinity to different SCs. The proper pore size (1.4 nm) and pre-located functional groups (hydrogen-bond donors, hydrogen-bond acceptors, and fluorophilic segments) work synergistically for efficient SCs capture. Remarkably, when coupled FSQ-4 with solid-phase microextraction (SPME), trace-level (part per trillion, 10-9 ) determination of 13 SCs can be easily achieved, representing one of the best results among NPS analyses, and the excellent extraction performance can be maintained under various interfering conditions.

UPLC-MS/MS Method for Detection of Etomidate and Its Metabolite Etomidate Acid Quantity in Blood.

OBJECTIVES: To establish a method for the simultaneous quantitative analysis of etomidate and its metabolite etomidate acid in blood, and to discuss its application value in actual cases. METHODS: Acetonitrile precipitate protein method was used, and C18 column was selected. Gradient elution was performed with acetonitrile and 5 mmol/L ammonium acetate within 6 min. Electrospray ionization source in positive ion mode was used. The internal standard etomidate acid-d5 was obtained by etomidate-d5 alkaline hydrolysis reaction. Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used for quantitative analysis. The methodological verification was conducted. RESULTS: Etomidate and etomidate acid in blood showed good linear relationship in the quantitative linear range (r>0.999), with the lower limit of quantification was 2.5 ng/mL and 7.5 ng/mL, respectively. The accuracy, precision, recovery rate, and matrix effect of the method met the professional verification standards. The practical application results showed that etomidate and etomidate acid could be detected in the blood of the abusers, and their mass concentrations ranged from 17.24 to 379.93 ng/mL. CONCLUSIONS: The method established in this study can simultaneously quantify etomidate and etomidate acid in blood, which is simple and convenient to operate with accuracy. It can meet the detection needs of actual cases and provide technical support for law enforcement to crack down on etomidate abuse.

Determination of five endosulfan pesticides in the fish pond water by dispersive liquid-liquid microextraction combined with GC-MS.

A simple and rapid dispersive liquid-liquid microextraction (DLLME) technique coupled with gas chromatography-ion trap mass spectrometry (GC-MS) was developed for the extraction and analysis of five endosulfan pesticides from the fish pond water. In this work, different parameters affecting the extraction process such as the type and volume of extraction solvent, type and volume of disperser solvent, and extraction time were studied and optimized. Under optimized conditions, the enrichment factor ranged from 189 to 269 and the relative recovery ranged from 88.5% to 94.9%. The linear range was 2.0-80.0 µg/L; the limits of detection and quantitation were in the range 0.04-1.06 µg/L and 0.12-3.53 µg/L, respectively. The relative standard deviations were in the range 0.94%-2.08% (n = 5). The obtained results show that DLLME combined with GC-MS is a fast and simple method for the determination of endosulfan pesticides in fish pond water.