Furfural analysis of aqueous and oily foodstuffs using a single modified paper for combined headspace extraction, derivatization and paper spray mass spectrometry.

Furfurals, including 2-furaldehyde, 5-methylfurfural and 5-hydroxymethylfurfural, widely exist in carbohydrate-rich daily foods, and may have toxic effects on humans. Here, a new headspace extraction-paper spray mass spectrometry (HSPS-MS/MS) method was established for furfural detection, in which the extraction and derivatization of volatiles with pre-loaded derivatization agent on paper tips is combined with paper spray mass spectrometry for detection. By this simple and cheap approach, interference of non-volatile matrix compounds is prevented, and the derivatization agent improves electrospray-type ionization efficiency, thus increasing selectivity and sensitivity.

Ultrafast, Selective, and Highly Sensitive Nonchromatographic Analysis of Fourteen Cannabinoids in Cannabis Extracts, Δ8-Tetrahydrocannabinol Synthetic Mixtures, and Edibles by Cyclic Ion Mobility Spectrometry-Mass Spectrometry.

The diversity of cannabinoid isomers and complexity of Cannabis products pose significant challenges for analytical methodologies. In this study, we developed a method to analyze 14 different cannabinoid isomers in diverse samples within milliseconds by leveraging the unique adduct-forming behavior of silver ions in advanced cyclic ion mobility spectrometry-mass spectrometry. The developed method achieved the separation of isomers from four groups of cannabinoids: Δ3-tetrahydrocannabinol (THC) (), Δ8-THC (), Δ9-THC (), cannabidiol (CBD) (), Δ8-iso-THC (), and Δ(4)8-iso-THC () (all MW = 314); 9α-hydroxyhexahydrocannabinol (), 9β-hydroxyhexahydrocannabinol (), and 8-hydroxy-iso-THC () (all MW = 332); tetrahydrocannabinolic acid (THCA) () and cannabidiolic acid (CBDA) () (both MW = 358); Δ8-tetrahydrocannabivarin (THCV) (), Δ8-iso-THCV (), and Δ9-THCV () (all MW = 286).

Comprehensive cannabinoid profiling of acid-treated CBD samples and Δ-THC-infused edibles.

Δ-Tetrahydrocannabinol (Δ-THC) is increasingly popular as a controversial substitute for Δ-tetrahydrocannabinol (Δ-THC) in cannabinoid-infused edibles. Δ-THC is prepared from cannabidiol (CBD) by treatment with acids. Side products including Δ-THC and other isomers that might end up in Δ-THC edibles are less studied.

Bifunctional Ti-modified paper for selective extraction or removal of phospholipids and paper spray mass spectrometry for bioanalysis in urine and plasma.

Background: Phospholipids (PLs) are major constituents of cell membranes, play important roles in cell proliferation and death, as well as in signal transduction, and therefore are relevant biomarkers for different pathologies. On the other hand, when the analysis of small compounds, such as therapeutics in blood is desired, then phospholipids are part of the matrix and cause serious interference during analysis. Currently, both the analysis and removal of PLs from biological samples are limited by extensive sample preparation and instrumental separation.

Boronate affinity paper spray mass spectrometry for determination of elevated levels of catecholamines in urine.

The analysis of catecholamines, such as dopamine, epinephrine and norepinephrine in urine can be used in the diagnosis of certain pathologies, such as hormone-producing tumors. Here, a fast and simple quantitative boronate affinity paper spray tandem mass spectrometric (PS-MS/MS) method is established, which can improve selectivity and reduce ion suppression without needing any instrumental chromatography. We use here the property of boronic acids, which can selectively bind ortho-diol-containing compounds under alkaline conditions.

Semiquantitative Screening of THC Analogues by Silica Gel TLC with an Ag(I) Retention Zone and Chromogenic Smartphone Detection.

With the ever-evolving cannabis industry, low-cost and high-throughput analytical methods for cannabinoids are urgently needed. Normally, (potentially) psychoactive cannabinoids, typically represented by Δ9-tetrahydrocannabinol (Δ9-THC), and nonpsychoactive cannabinoids with therapeutic benefits, typically represented by cannabidiol (CBD), are the target analytes. Structurally, the former (tetrahydrocannabinolic acid (THCA), cannabinol (CBN), and THC) have one olefinic double bond and the latter (cannabidiolic acid (CBDA), cannabigerol (CBG), and CBD) have two, which results in different affinities toward Ag(I) ions.

Chromatographic Determination of the Mycotoxin Patulin in 219 Chinese Tea Samples and Implications for Human Health.

Patulin (PAT) is a mycotoxin, with several acute, chronic, and cellular level toxic effects, produced by various fungi. A limit for PAT in food of has been set by authorities to guarantee food safety. Research on PAT in tea has been very limited although tea is the second largest beverage in the world.

Microextraction of -Dyed Wool and Qualitative Analysis of Its Flavones by UHPLC-UV, NMR and MS.

Detailed knowledge on natural dyes is important for agronomy and quality control as well as the fastness, stability, and analysis of dyed textiles. Weld ( L.), which is a source of flavone-based yellow dye, is the focus of this study.

Rapid Distinction and Semiquantitative Analysis of THC and CBD by Silver-Impregnated Paper Spray Mass Spectrometry.

The control over the amount of psychoactive THC (Δ-9-tetrahydrocannabinol) in commercial cannabidiol (CBD) products has to be strict. A fast and simple semiquantitative Ag(I)-impregnated paper spray mass spectrometric method for differentiating between THC and CBD, which show no difference in standard single-stage or tandem MS, was established. Because of a different binding affinity to Ag(I) ions, quasi-molecular Ag(I) adducts [THC + Ag] and [CBD + Ag] at / 421 and 423 give different fragmentation patterns.

Microfluidic Chip-Based Induced Phase Separation Extraction as a Fast and Efficient Miniaturized Sample Preparation Method.

Induced phase separation extraction (IPSE) is an efficient sample clean-up technique that can replace liquid-liquid extraction (LLE). The purpose of this study was to miniaturize IPSE by carrying it out in a microfluidic chip. An IPSE chip was designed and evaluated for its ability to separate and purify samples on a microscale.

A micro-solid phase extraction device to prepare a molecularly imprinted porous monolith in a facile mode for fast protein separation.

A molecularly imprinted polymeric monolith was synthesized in an aqueous environment in 15 min via UV-irradiation. The imprinted monolith was composed of hydroxyethyl methacrylate as monomer, dimethyl amino ethyl methacrylate as functional monomer, methylene bisacrylamide and piperazine diacrylamide as crosslinkers and human serum albumin as template molecule. The synthesis took place in a PDMS-based device (2.

Low-field benchtop NMR spectroscopy: status and prospects in natural product analysis.

Introduction: Since a couple of years, low-field (LF) nuclear magnetic resonance (NMR) spectrometers (40-100 MHz) have re-entered the market. They are used for various purposes including analyses of natural products. Similar to high-field instruments (300-1200 MHz), modern LF instruments can measure multiple nuclei and record two-dimensional (2D) NMR spectra.

Rapid Analysis of Illegal Cationic Dyes in Foods and Surface Waters Using High Temperature Direct Analysis in Real Time High-Resolution Mass Spectrometry.

A high temperature desorption (HTD) direct analysis in real time-high-resolution mass spectrometric (DART-HRMS) method was developed for the rapid analysis of four banned cationic dyes. Rhodamine B is used to dye foods, while malachite green, crystal violet, and methylene blue are added to fishponds as antimicrobials. A simple induced phase separation extraction was used to pretreat samples.

Is Low-field NMR a Complementary Tool to GC-MS in Quality Control of Essential Oils? A Case Study: Patchouli Essential Oil.

High-field NMR is an expensive and important quality control technique. In recent years, cheaper and simpler low-field NMR has become available as a new quality control technique. In this study, 60 MHz H-NMR was compared with GC-MS and refractometry for the detection of adulteration of essential oils, taking patchouli essential oil as a test case.

Biochip Spray: Simplified Coupling of Surface Plasmon Resonance Biosensing and Mass Spectrometry.

A simplified coupling of surface plasmon resonance (SPR) immuno-biosensing with ambient ionization mass spectrometry (MS) was developed. It combines two orthogonal analysis techniques: the biosensing capability of SPR and the chemical identification power of high resolution MS. As a proof-of-principle, deoxynivalenol (DON), an important mycotoxin, was captured using an SPR gold chip containing an antifouling layer and monoclonal antibodies against the toxin and, after washing, the chip could be taken out and analyzed by direct spray MS of the biosensor chip to confirm the identity of DON.

Analysis of Mycotoxins in Beer Using a Portable Nanostructured Imaging Surface Plasmon Resonance Biosensor.

A competitive inhibition immunoassay is described for the mycotoxins deoxynivalenol (DON) and ochratoxin A (OTA) in beer using a portable nanostructured imaging surface plasmon resonance (iSPR) biosensor, also referred to as imaging nanoplasmonics. The toxins were directly and covalently immobilized on a 3-dimensional carboxymethylated dextran (CMD) layer on a nanostructured iSPR chip. The assay is based on competition between the immobilized mycotoxins and free mycotoxins in the solution for binding to specific antibodies.

Chemometric analysis of comprehensive LC×LC-MS data: Resolution of triacylglycerol structural isomers in corn oil.

Comprehensive hyphenated two-dimensional liquid chromatography mass spectrometry (LC×LC-MS) is a very powerful analytical tool achieving high throughput resolution of highly complex natural samples. However, even using this approach there is still the possibility of not resolving some of the analytes of interest. For instance, triacylglycerols (TAGs) structural isomers in oil samples are extremely difficult to separate chromatographically due to their very similar structure and chemical properties.

Critical comparison of mass analyzers for forensic hair analysis by ambient ionization mass spectrometry.

Rationale: Recently, several direct and/or ambient mass spectrometry (MS) approaches have been suggested for drugs of abuse imaging in hair. The use of mass spectrometers with insufficient selectivity could result in false-positive measurements due to isobaric interferences. Different mass analyzers have been evaluated regarding their selectivity and sensitivity for the detection of Δ9-tetrahydrocannabinol (THC) from intact hair samples using direct analysis in real time (DART) ionization.

(Un)targeted Scanning of Locks of Hair for Drugs of Abuse by Direct Analysis in Real Time-High-Resolution Mass Spectrometry.

Forensic hair evidence can be used to obtain retrospective timelines of drug use by analysis of hair segments. However, this is a laborious and time-consuming process, and mass spectrometric (MS) imaging techniques, which show great potential for single-hair targeted analysis, are less useful due to differences in hair growth rate between individual hairs. As an alternative, a fast untargeted analysis method was developed that uses direct analysis in real time-high-resolution mass spectrometry (DART-HRMS) to longitudinally scan intact locks of hair without extensive sample preparation or segmentation.

Evidence based decontamination protocols for the removal of external Δ9-tetrahydrocannabinol (THC) from contaminated hair.

External contamination can cause false positive results in forensic hair testing for drugs of abuse and is therefore a major concern when hair evidence is used in court. Current literature about decontamination strategies is mainly focused on external cocaine contamination and no consensus on the best decontamination procedure for hair samples containing cannabinoids has been reached so far. In this study, different protocols with solvents, both organic as well as aqueous, were tested on blank and drug user hair for their performance on removing external cannabis contamination originating from either smoke or indirect contact with cannabis plant material.

Multiplex surface plasmon resonance biosensing and its transferability towards imaging nanoplasmonics for detection of mycotoxins in barley.

A 6-plex competitive inhibition immunoassay for mycotoxins in barley was developed on a prototype portable nanostructured imaging surface plasmon resonance (iSPR) instrument, also referred to as imaging nanoplasmonics. As a benchmark for the prototype nanoplasmonics instrument, first a double 3-plex assay was developed for the detection of deoxynivalenol (DON), zearalenone (ZEA), T-2 toxin (T-2), ochratoxin A (OTA), fumonisin B1 (FB1) and aflatoxin B1 (AFB1) using a well-established benchtop SPR instrument and two biosensor chips. To this end, ovalbumin (OVA) conjugates of mycotoxins were immobilized on the chip via amine coupling.

Selective on-line detection of boronic acids and derivatives in high-performance liquid chromatography eluates by post-column reaction with alizarin.

An on-line high-performance liquid chromatography (HPLC) method for the rapid and selective detection of boronic acids in complex mixtures was developed. After optimization experiments at an HPLC flow rate of 0.40 mL/min, the HPLC-separated analytes were mixed post-column with a solution of 75 μM alizarin and 0.

Key steps towards the oriented immobilization of antibodies using boronic acids.

Oriented immobilization of antibodies using boronic acids shows a strong potential for improving immunoassay performance but is not yet widely used, possibly because of the difficulties encountered in its implementation. How to choose the boronic acid structure and how should it be attached to the surface? How to choose an antibody that will bind to the boronic acid? Under which conditions should the binding take place for an effective oriented antibody immobilization? How to make sure that the antibody stays on the surface? This tutorial review provides answers to these questions through analysis of the literature and personal suggestions, and thereby intends to facilitate the development of this promising antibody immobilization strategy.

Ultratrace LC-MS/MS analysis of segmented calf hair for retrospective assessment of time of clenbuterol administration in Agriforensics.

In agriforensics, time of administration is often debated when illegal drug residues, such as clenbuterol, are found in frequently traded cattle. In this proof-of-concept work, the feasibility of obtaining retrospective timeline information from segmented calf tail hair analyses has been studied. First, an ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) hair analysis method was adapted to accommodate smaller sample sizes and in-house validated.

Macroscopic and microscopic spatially-resolved analysis of food contaminants and constituents using laser-ablation electrospray ionization mass spectrometry imaging.

Laser-ablation electrospray ionization (LAESI) mass spectrometry imaging (MSI) does not require very flat surfaces, high-precision sample preparation, or the addition of matrix. Because of these features, LAESI-MSI may be the method of choice for spatially-resolved food analysis. In this work, LAESI time-of-flight MSI was investigated for macroscopic and microscopic imaging of pesticides, mycotoxins, and plant metabolites on rose leaves, orange and lemon fruit, ergot bodies, cherry tomatoes, and maize kernels.