Novel Applications of Microextraction Techniques Focused on Biological and Forensic Analyses

In recent years, major attention has been focused on microextraction procedures that allow high recovery of target analytes, regardless of the complexity of the sample matrices. The most used techniques included liquid-liquid extraction (LLE), solid-phase extraction (SPE), solid-phase microextraction (SPME), dispersive liquid-liquid microextraction (DLLME), microextraction by packed sorbent (MEPS), and fabric-phase sorptive extraction (FPSE). These techniques manifest a rapid development of sample preparation techniques in different fields, such as biological, environmental, food sciences, natural products, forensic medicine, and toxicology. In the biological and forensic fields, where a wide variety of drugs with different chemical properties are analyzed, the sample preparation is required to make the sample suitable for the instrumental analysis, which often includes gas chromatography (GC) and liquid chromatography (LC) coupled with mass detectors or tandem mass detectors (MS/MS). In this review, we have focused our attention on the biological and forensic application of these innovative procedures, highlighting the major advantages and results that have been accomplished in laboratory and clinical practice.

High Pressure Processing Impact on Emerging Mycotoxins (ENNA, ENNA1, ENNB, ENNB1) Mitigation in Different Juice and Juice-Milk Matrices

The aim of the present study was to investigate the potential of high-pressure processing (HPP) (600 MPa during 5 min) on emerging mycotoxins, enniatin A (ENNA), enniatin A1 (ENNA1), enniatin B (ENNB), enniatin B1 (ENNB1) reduction in different juice/milk models, and to compare it with the effect of a traditional thermal treatment (HT) (90 °C during 21 s). For this purpose, different juice models (orange juice, orange juice/milk beverage, strawberry juice, strawberry juice/milk beverage, grape juice and grape juice/milk beverage) were prepared and spiked individually with ENNA, ENNA1, ENNB and ENNB1 at a concentration of 100 µg/L. After HPP and HT treatments, ENNs were extracted from treated samples and controls employing dispersive liquid-liquid microextraction methodology (DLLME) and determined by liquid chromatography coupled to ion-trap tandem mass spectrometry (HPLC-MS/MS-IT). The results obtained revealed higher reduction percentages (11% to 75.4%) when the samples were treated under HPP technology. Thermal treatment allowed reduction percentages varying from 2.6% to 24.3%, at best, being ENNA1 the only enniatin that was reduced in all juice models. In general, no significant differences (p > 0.05) were observed when the reductions obtained for each enniatin were evaluated according to the kind of juice model, so no matrix effects were observed for most cases. HPP technology can constitute an effective tool in mycotoxins removal from juices.

Fast Dispersive Liquid-Liquid Microextraction Based on Temperature Switching Deep Eutectic Solvent as A Green Extractant

With the development of research, it was found that the dispersive liquid-liquid microextraction (DLLME) was limited by the tedious extraction process and toxic extractant. A thermo-switchable deep eutectic solvent (DES) was applied to the DLLME as a green extractant in this paper. The DES can be dispersed and aggregated by shaking and heating in the water during the extraction process due to the surfactant and thermo-switchable properties, which shortened the extraction time as low as 5 minutes. The feasibility of the developed method was verified using 4 organophosphorus pesticides and 5 pyrethroids as targets in simulated water samples, which showed good precision (RSD%, 0.8-9.7, n=3) and low detection limit (0.16-0.81 µg L−1, S/N = 3) under the optimal extraction conditions. This method was used to detect the pesticide content in four natural rivers in Xi'an, and the recoveries of these spiked samples at three concentrations levels were among 81–113%. This is the first time to combine the toxic-free and thermo-switchable properties of DES in DLLME to proposes a simple, fast, effective, and green pretreatment method.

Dispersive liquid–liquid microextraction of 11-nor-Δ9-tetrahydrocannabinol-carboxylic acid applied to urine testing

Aim: THC-COOH is the major metabolite of Δ9-tetrahydrocannabinol commonly tested in urine to determine cannabis intake. In this study, a method based on dispersive liquid–liquid microextraction was developed for testing THC-COOH in urine. Materials & methods: Hydrolyzed urine specimens were extracted via dispersive liquid–liquid microextraction with acetonitrile (disperser solvent) and chloroform (extraction solvent). Derivatization was performed with N,O-Bis(trimethylsilyl)trifluoroacetamide with 1% trichloro(chloromethyl)silane. Analysis was performed by GC–MS/MS. Results: The method showed acceptable linearity (5–500 ng/ml), imprecision (<10.5%) and bias (<4.9%). Limits of detection and quantitation were 1 and 5 ng/ml, respectively. Twenty-four authentic samples were analyzed, with 22 samples being positive for THC-COOH. Conclusion: The proposed method is more environmentally friendly and provided good sensitivity, selectivity and reproducibility.

Vortex-assisted dispersive liquid-liquid microextraction based on the solidification of sedimentary deep eutectic solvents for the determination of triazine and phenylurea herbicides in milk samples

The vortex-assisted dispersive liquid-liquid microextraction based on the solidification of sedimentary deep eutectic solvents was developed and applied to the extraction of triazine and phenylurea herbicides in milk samples. In...