OECD-compliant amino acid derivative assay (ADRA) testing and method transfer to UHPLC conditions is presented.
A novel liquid chromatography–tandem mass spectrometry (LC–MS/MS) method with a dual electrospray ionization (ESI) and atmospheric-pressure chemical ionization (APCI) source was developed for analysis of 66 pesticides and 5 mycotoxins regulated by the State of California in medium-chain triglyceride (MCT) oil cannabis tinctures. The limits of quantitation (LOQs) of all of the pesticides and mycotoxins were well below California state action limits of these analytes in cannabis-based non-inhalable or edible products. A total of 62 (out of 66) pesticides and 5 mycotoxins were analyzed using LC–MS/MS with an ESI source, and the remaining 4 pesticides were determined using LC–MS/MS with an APCI source. A simple, fast, and cheap acetonitrile solvent extraction method was used for sample preparation to get good recovery and achieve high throughput for this analysis. For late-eluted analytes, a number of internal standards were used to compensate for ion suppression effects from the hydrophobic matrix.
Errors arising from the DNPH approach commonly used to analyze carbonyl compounds in smoke from heat-not-burn (HNB) tobacco can be avoided by using the approach described in this study.
Displacement chromatography is a viable alternative to elution chromatography, but the biotechnology industry has yet to fully exploit this technique. The authors present results of a pilot-scale ion-exchange displacement process developed for the removal of variants from recombitant human brain-derived neutrotrophic factor.
Separation scientists frequently encounter critical pairs that are difficult to separate in a complex mixture. To save time and expensive solvents, an effective alternative to conventional screening protocols or mathematical peak width reduction is called iterative curve fitting.
The impact of extracolumn dispersion on kinetic plot curves is investigated. A web-based calculator that allows users to make their own kinetic plots with examples of how the tool can be used to troubleshoot underperforming columns and support column selection is discussed.
Commercially available trypsin IMERs can digest proteins with high sequence coverage and robustness, facilitating online multidimensional LC–MS.
Overcoming the challenges of food and beverage analysis with ion chromatography (IC).
Extractable and leachable (E&L) testing for finished pharmaceutical products, bioprocess manufacturing systems, and medical devices is currently a subject of intense interest. The majority of the challenges encountered in analytical workflows are related to the highly complex matrices and relatively low analyte evaluation thresholds seen in E&L studies. This paper provide options for executing E&L testing to supporting regulatory submissions. There are multiple compliant routes possible, and the presented workflows and analytical solutions are only one of multiple successful approaches.
This method for PFAS analysis in milk and infant formula is robust, reliable, and reproducible, with scope to expand the list of PFAS in the future.
A fully automated quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and extract clean-up method is described for analysis of organophosphate pesticides in orange juice. This method uses GC–MS and LC–MS along with an industry standard robotic x,y,z-sampling system.
This article describes a comprehensive study on optimizing ion-pair reversed-phase liquid chromatography for analysing protected and unprotected single-stranded DNA oligonucleotides.
Integrating electric fields into extraction techniques increases sensitivity and selectivity. These approaches are compatible with miniaturized, portable, and many biological samples.
Monoliths are chromatography sorbents cast into columns as a single continuous piece in contrast with regular chromatographic sorbents, which are packed as individual particles. The guest authors compare three such novel sorbents with a conventional particle-packed column.
Commercially available trypsin IMERs can digest proteins with high sequence coverage and robustness, facilitating online multidimensional LC–MS.
Webinar Date/Time: Wednesday, October 18th, 2023 12:30 pm BST 7:30 am EDT 13:30 pm CEST Thursday, October 19th, 2023 12:30pm BST | 7:30am EDT | 13:30pm CEST
Guest author Reg Cross discusses strategies for collecting samples from large masses of material. He also describes the problems associated with acquiring truly representative samples for analysis.
This GC–FID method enables accurate determination of cooling agents, which are flavor compounds commonly used in cigarette tipping paper.
The authors compare their results in analyzing styrene–butadiene block copolymers by gel permeation chromatography with other methods, such as Fourier transform infrared spectroscopy and pyrolysis gas chromatography.
October 4, 2021 at 3pm BST | 10am EST | 4pm CEST Join global industry and regulatory experts as they discuss current hot topics in extractables and leachables (E&L) testing for pharmaceuticals, biopharmaceuticals and medical devices.
Using ion mobility, analytes that have the same molecular mass can be separated by their shape, centers of mass, and collision cross section, but challenges such as ion loss can still occur. A new development in ion mobility separation, high-resolution ion mobility (HRIM), addresses such problems, and is particularly well suited to challenging applications, such as glycosylation monitoring of biological drugs and vitamin D analysis.
Per- and polyfluoralkyl substances (PFAS) are found in our food. Sensitive, precise, and accurate analytical methods are needed to estimate human exposure to these chemicals. A comparative study was performed between two extraction and cleanup methods (solid-phase extraction [SPE] and dispersive SPE) for the analysis of PFAS in apples. Both methods showed excellent sensitivity, precision, and accuracy. dSPE has some benefits over conventional SPE, and vice versa. The advantages and disadvantages of both methods are discussed.
Hydrophilic interaction chromatography–mass spectrometry (HILIC-MS) offers a flexible and efficient alternative to ion-pairing reversed-phase liquid chromatography (IP-RPLC) for oligonucleotide analysis, with column selectivity and mobile phase pH being key factors in optimizing retention and detection.
A column with chemically modified column hardware showed improvements in analytical performance for siRNA compared to a conventional stainless-steel column.
HRIM has emerged as a robust separation strategy for complex chemical analyses due to its ability to improve peak capacity and aid in the separation of isobaric signals.
Pyrolysis–gas chromatography–mass spectrometry has advantages for the analysis of environmental microplastic samples compared to other leading analytical methods, including spectroscopic techniques.
This GC–FID method enables accurate determination of cooling agents, which are flavor compounds commonly used in cigarette tipping paper.
Food contamination from mineral oil saturated hydrocarbons (MOSHs) and mineral oil aromatic hydrocarbons (MOAHs) is problematic and requires a sensitive analytical technique. These contaminants were analyzed using GC×GC with flame ionization detection (FID) and time-of-flight–MS (TOF–MS) parallel dual detection. The method provides enhanced chromatographic separation, along with the full mass spectra information, and overcomes difficult interferences, resulting in reduction of false positives over conventional GC–MS methods.
Improved analysis of pharmaceutical and natural medicine products requires advances in reversed-phase LC stationary phases. We examine two synthesized stationary phases with applicability in quality control and chiral separation for analysis of natural products.
The current challenges and future perspectives of the purification of cannabinoids from cannabis extracts are presented in this review article.