The LS-APGD microplasma has shown potential as a combined atomic and molecular (CAM) ionization source, though to this point it has been solely interfaced with large, laboratory-scale instruments. There are many instances wherein reduced-format, lower operating overhead, analyzers are appropriate. To this end, the LS-APGD has been coupled with an Advion expressionL Compact Mass Spectrometry (CMS) for the analysis of diverse samples. This instrument has been previously travel hardened in accordance to MIL-SPEC-810, demonstrating its suitability for in-field analysis. The coupling of the LS-APGD to this instrument expands its capability for diverse analyses, with early-stage figures of merit presented here. With this new coupling, a thorough optimization of both the instrument ion optics and the LS-APGD operating parameters was necessary as this platform does not have a direct method for collisional dissociation of potentially-deleterious molecular species. Under the optimized conditions, analytical response curves were constructed for Na, Rb, Cs, and Tl, demonstrating detection limits between 17.6–146 ng mL−1 (single ng, absolute). Furthermore, CAM sampling capabilities can be realized upon changing from a 2% HNO3 to a 70 : 30 MeOH : H2O solvent system, providing molecular-level chemical information readily obtained from atomic ionization sources such as the inductively coupled plasma (ICP-MS). Here detection limits between 1–32 nM (single pg, absolute) were obtained for caffeine, acetaminophen, Δ9-tetrahydrocannabidiol, sulfadimethoxine, terfenadine, and reserpine. The unique features of the CAM ionization source on this flexible MS platform hold promise for many operation environments.
USDA-ARS, Cornell University, Michigan State University
Abstract
Processing techniques can disrupt the cotyledon cell walls of raw beans, allowing digestive enzymes greater access to intercellular stores of micronutrients such as iron during digestion. This study evaluated the iron bioavailability of seven bean varieties with different seed coat colors (white, yellow, cranberry, red, black) either boiled or processed into spaghetti pastas formulated from heat treated bean flour as the major ingredient (90% bean flour). Iron bioavailability was significantly (p ≤ 0.05) higher in spaghetti made from white or yellow bean varieties Snowdon, Alpena, Samurai and Canario when compared to boiled beans. Although cotyledon cells were broken and the phytate to iron molar ratios were significantly lower, the iron bioavailability of the cranberry (Etna), red kidney (Red Hawk) and black (Zenith) bean varieties did not improve after processing into spaghetti. Iron bioavailability of bean-based pastas was associated with procyanidin and cinnamtannin compounds that have a negative impact on the absorption of iron.
Analysis was performed by LC/MS using the Advion Interchim Scientific expression® Compact Mass Spectrometer (CMS).
The combination of the Advion Interchim Scientific® expression® CMS puriFlash® flash chromatography technologies speed up the synthesis, purification and characterization of a compound.
Kyungpook National University, Dankook University, Ulsan National Institute of Science and Technology, South Korea; Icahn School of Medicine at Mount Sinai, United States
Abstract
Sphingosine kinase1 (SphK1) is an acetyl-CoA dependent acetyltransferase which acts on cyclooxygenase2 (COX2) in neurons in a model of Alzheimer’s disease (AD). However, the mechanism underlying this activity was unexplored. Here we show that N-acetyl sphingosine (N-AS) is first generated by acetyl-CoA and sphingosine through SphK1. N-AS then acetylates serine 565 (S565) of COX2, and the N-AS-acetylated COX2 induces the production of specialized pro-resolving mediators (SPMs). In a mouse model of AD, microglia show a reduction in N-AS generation, leading to decreased acetyl-S565 COX2 and SPM production. Treatment with N-AS increases acetylated COX2 and N-AS-triggered SPMs in microglia of AD mice, leading to resolution of neuroinflammation, an increase in microglial phagocytosis, and improved memory. Taken together, these results identify a role of N-AS in the dysfunction of microglia in AD.
Mass analysis was carried out using an Advion expression® Compact Mass Spectrometer (CMS).
In this application note, the Advion Interchim Scientific expression® Compact Mass Spectrometer (CMS) with volatile APCI (vAPCI) is used to analyze volatile compounds present during the fermentation of homebrewed beer by Stephanie Rankin Turner of Loughborough University.
The complex flavor of beer is primarily a result of the ingredients used, the brewing method, and conditions during fermentation. The analysis of beer throughout this process can be invaluable. Being one of the most widely consumed beverages worldwide, rapid and reliable analytical techniques are essential to keep up with demand and production.
This note demonstrates the use of the Advion Interchim Scientific expression® CMS with vAPCI for the analysis of volatile compounds from the headspace of homebrew beer and hops. The Venturi-assisted interface of the instrument enabled rapid sampling of volatiles, allowing the changing volatile profile of the homebrew to be observed throughout the fermentation process. This simple method would be suitable for fast quality control during alcoholic beverage production.
National Organization for Drug Control and Research, Cairo University
Abstract
Stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) and normal-phase high-performance thin-layer chromatography (NP-HPTLC) methods have been developed for the determination of palonosetron which is a potent antiemetic drug used with chemotherapy. Forced degradation studies were performed on palonosetron to study its stability behavior. The drug was subjected to acid, base, neutral hydrolysis, oxidation, thermal and photolytic conditions. Mass analysis has been performed to elucidate the oxidative degradants by Advion compact mass spectrometer. HPLC separation was achieved on PerfectChrom 100 C4 (250 × 4.6 mm, 5 μm particle size) column using buffer (20 mM dipotassium hydrogen orthophosphate, adjusted with phosphoric acid to pH 2.5):acetonitrile:methanol (60:30:10, v/v) as the mobile phase with isocratic mode at a flow rate of 1 mL/min using photodiode array detector (PAD) at 210 nm. The method showed adequate sensitivity concerning linearity, accuracy and precision over the range of 0.1–10 μg/mL. Limit of detection (LOD) and limit of quantification (LOQ) were determined to be 0.03 μg/mL and 0.09 μg/mL, respectively. HPTLC separation was carried out on aluminum plates pre-coated with silica gel 60 F254 using methanol:ammonia (10:0.5, v/v) as the mobile phase. CAMAG scanner was operated at 254 nm for the densitometric measurement in the absorbance mode. A polynomial relationship was constructed in concentration range of 0.1–2 μg/band, with LOD and LOQ 0.02 μg/band and 0.06 μg/band, respectively. The cited chromatographic methods were successfully applied to the determination of palonosetron in the presence of its degradation products and additives in the commercially available vials. Method validation was performed as per the ICH guidelines confirming methods robustness to be used in quality control laboratories. Statistical comparisons have been performed between the results of the cited chromatographic methods and those of the official one using Student’s ttest and F test values at 95% confidence interval level, revealing good accuracy and precision.
Authors: Japan Bioindustry Association, Advanced Industrial Science and Technology, Japan
Highlights
Deacetylation of glycopeptide with an esterase prevents base-induced side reactions, b-elimination, and epimerization
An esterase from B. subtilis was utilized for Deacetylation of sugar hydroxyl groups on glycopeptide synthesis
Deacetylation with an esterase and glycosylations with glycosyltransferases were accomplished in one-pot
Abstract
Glycopeptides are fragments of glycoproteins and are important in evaluating the biological roles of carbohydrates in glycoproteins. Fmoc solid-phase peptide synthesis using acetyl-protected glycosylated amino acids is a common strategy for the preparation of glycopeptides, but this approach normally requires chemical de-O-acetylation with a base that β-eliminates sugar residues and epimerizes the peptide backbone. Here we demonstrate a facile new chemoenzymatic synthetic strategy for glycopeptides, using an esterase for the de-O-acetylation of sugar residues and glycosyltransferases for successive sugar elongations at neutral pH.
ESI-MS spectra were collected using an Advion expression Compact Mass Spectrometer (CMS) in negative ion mode.
Learn Mass Spectrometry: For a limited time, access our free curriculum from Dr. Jack Henion, global leader and educator for Mass Spectrometry and LC/MS
Take advantage of this educational opportunity to learn from the master, Dr. Henion, Cornell Emeritus Professor, who will guide you through basic principles to more advanced techniques. This lecture series offers a university-level course, only offered to Advion customers and university students — until now.
This lecture package includes the following modules:
Introduction to Mass Spectrometry
Flow Injection Analysis, ESI and APCI Ionization Techniques
Direct Analysis Probe for Liquids and Solids (ASAP)
Plate Express TLC Plate Reader
Touch Express Open Port Sampling Interface (OPSI)
LC/MS Techniques
Other CMS Applications & Techniques
This course is available for a limited time to aid in at-home learning initiatives and coursework. Professors who aim to teach, undergraduates who desire to further their education, or Ph.D.’s in need of a refresher, our team at Advion is offering this package at no-charge.
Advion’s curriculum package offers viewers a wide range of essentials for teaching and learning mass spectrometry for chemists.
Benzo[d]thiazole is widely used in synthetic and medicinal chemistry, and it is a component of many compounds and drugs that have several different bioactivities. Herein, we describe an elegant pathway for synthesis of methyl 4- and 5-hydroxy-2-amino-benzo[d]thiazole-6-carboxylates as building blocks that can be substituted at four different positions on the bicycle and thus offer the possibility to thoroughly explore the chemical space around the molecule studied as a ligand for the chosen target. A series of 12 new compounds was prepared using the described methods and Williamson ether synthesis.
Martin-Luther-University Halle-Wittenberg, Free University of Berlin
Abstract
Cannabis products have been used in various fields of everyday life for many centuries, and applications in folk medicine and textile production have been well-known for many centuries. For traditional textile production, hemp fibers were extracted from the stems by water retting in stagnant or slow-moving waters.
During this procedure, parts of the plant material‚ among them phytocannabinoids‚ are released into the water. Cannabinol (CBN) is an important degradation product of the predominant phytocannabinoids found in Cannabis species. Thus, it is an excellent indicator for present as well as ancient hemp water retting.
In this study, we developed and validated a simple and fast method for the determination of CBN in sediment samples using high-performance thin-layer chromatography (HPTLC) combined with electrospray ionization mass spectrometry (ESI-MS), thereby testing different extraction and cleanup procedures‚ as well as various sorbents and solvents for planar chromatography.
This method shows a satisfactory overall analytical performance with an average recovery rate of 73%. Our protocol enabled qualitative and quantitative analyses of CBN in samples of a bottom sediment core‚ having been obtained from a small lake in Northern India, where intense local retting of hemp was suggested in the past. The findings correlate with existing records of Cannabis-type pollen. Thus, the method we propose is a helpful tool to track ancient hemp retting activities.
The Advion TLC/CMS system with the expression® Compact Mass Spectrometer (CMS) and Plate Express® TLC Plate Reader was utilized for the elution of compounds from the HPTLC plates.
