Author


Sue D’Antonio

Latest:

Liquid Chromatography–Time-of-Flight Mass Spectrometry for Cannabinoid Profiling and Quantitation in Hemp Oil Extracts

A primary impediment to cannabinoid research is the fact that materials possessing psychoactive Δ-9-tetrathydrocannabinol are considered Schedule I drugs as defined in the U.S. Controlled Substances Act. An alternative source of cannabinoids may be found in hemp oil extracts. Hemp contains a low percentage of Δ-9-tetrathydrocannabinol (THC) by weight but relatively high amounts of non-psychoactive cannabinoids. The liquid chromatography-time of flight mass spectrometry (LC-TOF) method presented herein allows for the accurate, precise and robust speciation, profiling and quantification of cannabinoids in hemp oil extracts and commercial cannabinoid products for research and development laboratories. The method was determined to chromatographically separate 11 cannabinoids including differentiation of Δ-8-tetrahdrocannabinol and THC with excellent linear dynamic range, specificity and sensitivity.


C. Pezzei

Latest:

Matrix-Assisted Laser Desorption-Ionization Imaging Mass Spectrometry for Direct Tissue Analysis

A summary of the most recent advances in sample preparation, instrumentation, and data-processing techniques for MALDI-IMS


The Editors of LCGC

Latest:

Celebrating 35 Years of LCGC

Leading separation scientists share their perspectives on current challenges in separation science and where the field is heading.


Michael R. Halpenny

Latest:

Analysis of Terpenes in Cannabis Using Headspace Solid-Phase Microextraction and GC–MS

As the legalization of medicinal cannabis continues to sweep across the United States, an urgent need has developed for fast, accurate and efficient analytical testing. In addition to testing for contaminants and potency, there is also interest in the determination of terpene identity and concentration levels present in different strains of cannabis. Terpenes have been shown to have therapeutic uses for treatment of different medical conditions ranging from cancer and inflammation, to anxiety and sleeplessness. It is believed that the combination of terpenes and cannabinoids in cannabis produce a synergistic effect with regards to medical benefits. The traditional testing method for terpenes in plant materials involves a solvent-based extraction followed by GC analysis. In this work, headspace solid phase microextraction (HS-SPME) was used to identify and quantify terpene content in cannabis. The HS-SPME method provided several advantages over solvent extraction in that it provided a cleaner analysis, free of interferences from co-extracted matrix, and was non-destructive to the sample. A cannabis sample of unknown origin was first analyzed qualitatively by HS-SPME and GC-MS. Spectral library matching and retention indices were used to identify 42 different terpenes. Quantitative analysis was then performed for several selected terpenes using spiked samples. Method accuracy was >90%, with reproducibility of


Gordon Fagras

Latest:

Evaluation of Modified QuEChERS for Pesticide Analysis in Cannabis

While systems for growing, production and sale of cannabis and cannabis related products are well established, regulation and enforcement of quality and safety testing have lagged behind. However, state governments and private labs are focusing on product safety testing with special emphasis on pesticide analysis. This is partially the result of various product recalls, media attention and concern from patient advocacy groups. We evaluated a modified QuEChERS LC-MS/MS method for analysis of multiresidue pesticides. The AOAC QuEChERS method was used for a reduced 1.5 g amount of plant material and processed with a universal dSPE formulation. LC-MS/MS analysis used constant polarity switching ESI and monitored at least two transitions per analyte. Matrix-matched calibration was used for quantitation and both method and instrument internal standards were used. Analyte recovery validation was performed according to FDA guidelines by testing three matrices at three fortification levels in triplicate for over 200 pesticides. For the large majority of pesticides, in all three matrices and at all three fortification levels, recovery was between 70-120%.


Jeffrey H. Dahl

Latest:

Evaluation of Modified QuEChERS for Pesticide Analysis in Cannabis

While systems for growing, production and sale of cannabis and cannabis related products are well established, regulation and enforcement of quality and safety testing have lagged behind. However, state governments and private labs are focusing on product safety testing with special emphasis on pesticide analysis. This is partially the result of various product recalls, media attention and concern from patient advocacy groups. We evaluated a modified QuEChERS LC-MS/MS method for analysis of multiresidue pesticides. The AOAC QuEChERS method was used for a reduced 1.5 g amount of plant material and processed with a universal dSPE formulation. LC-MS/MS analysis used constant polarity switching ESI and monitored at least two transitions per analyte. Matrix-matched calibration was used for quantitation and both method and instrument internal standards were used. Analyte recovery validation was performed according to FDA guidelines by testing three matrices at three fortification levels in triplicate for over 200 pesticides. For the large majority of pesticides, in all three matrices and at all three fortification levels, recovery was between 70-120%.


Derek Laine

Latest:

Optimization of Sample Preparation for Pesticide Analysis in Oil-Based Cannabis Products Using LipiFiltr®

This application note outlines the performance benefits achieved with UCT’s LipiFiltr® cleanup cartridge for the analysis of pesticides in oil-based cannabis products using LC–MS/MS analysis.



Douglas A. Duncan

Latest:

Pesticide and Mycotoxin Analysis: Mastering the Complexity of the Cannabis Matrix

Research scientists in the cannabis field are tasked with validating robust methods that can be seamlessly transitioned into production laboratories. Unlike typical disciplines where controls are easily (and legally) obtained through known manufacturers, analytical chemists working for both consumable vendors as well as cannabis laboratories must do their best to develop methods often without such resources at their disposal. As the industry matures and additional regulations are adopted, the evolution of the pesticide testing subsection continues to be vastly different depending on the jurisdiction one does business in. This creates an interesting challenge for commercial scientists tasked with developing methods that will appeal to a majority of their consumers, while also generating unexpected hurdles to said laboratories once the methods are placed into production. Ace Analytical Laboratory, located in Las Vegas, Nevada, has successfully adopted and validated pesticide testing methods for their cannabis laboratories and has gained valuable insight into how to best work with such a difficult matrix. In conjunction with UCT, LLC, an overview of best practices and method development techniques for pesticide testing in cannabis is discussed below and told from a technical perspective.


Thy X. Truong

Latest:

Analysis of Organic Compounds in Water Using Unique Concentration–Injection Techniques for Portable GC–MS

In this study, a simple method was used for extraction and concentration of trace organic compounds in water, followed by injection using a coiled wire filament and GC–MS analysis. Common semivolatile organic compound contaminants at low parts-per-billion levels were detected in less than 10 min.


Nathan L. Porter

Latest:

Analysis of Organic Compounds in Water Using Unique Concentration–Injection Techniques for Portable GC–MS

In this study, a simple method was used for extraction and concentration of trace organic compounds in water, followed by injection using a coiled wire filament and GC–MS analysis. Common semivolatile organic compound contaminants at low parts-per-billion levels were detected in less than 10 min.


Kevin J. Wells-Knecht

Latest:

Testing the Limits of Ion Mobility Mass Spectrometry to Compare a Nonbiological Complex Drug Product and Purported Generics—A Case Study with Copaxone

The analysis of oil samples containing many thousands of constituents best illustrates the benefits of ion mobility MS for complex samples. Here, we test the limits of ion mobility MS to discern differences between batches of Copaxone, a highly complex drug containing billions of peptides, and various purported generic versions of the drug.


Don Betowski

Latest:

The Application of Computational Chemistry to Problems in Mass Spectrometry

With computational chemistry, chemists can now study chemical phenomena by performing computationally intense calculations on computers rather than examining reactions and compounds experimentally. This is especially attractive when the laboratory experiments are time consuming, costly, dangerous, or difficult. Modern computational chemistry tools are capable of determining molecular structures, molecular spectra, and energetics, and of elucidating reaction pathways and chemical reaction products.


Vera Weinstein

Latest:

Testing the Limits of Ion Mobility Mass Spectrometry to Compare a Nonbiological Complex Drug Product and Purported Generics—A Case Study with Copaxone

The analysis of oil samples containing many thousands of constituents best illustrates the benefits of ion mobility MS for complex samples. Here, we test the limits of ion mobility MS to discern differences between batches of Copaxone, a highly complex drug containing billions of peptides, and various purported generic versions of the drug.


Donald H. Aue

Latest:

The Application of Computational Chemistry to Problems in Mass Spectrometry

With computational chemistry, chemists can now study chemical phenomena by performing computationally intense calculations on computers rather than examining reactions and compounds experimentally. This is especially attractive when the laboratory experiments are time consuming, costly, dangerous, or difficult. Modern computational chemistry tools are capable of determining molecular structures, molecular spectra, and energetics, and of elucidating reaction pathways and chemical reaction products.


Arthur Komlosh

Latest:

Testing the Limits of Ion Mobility Mass Spectrometry to Compare a Nonbiological Complex Drug Product and Purported Generics—A Case Study with Copaxone

The analysis of oil samples containing many thousands of constituents best illustrates the benefits of ion mobility MS for complex samples. Here, we test the limits of ion mobility MS to discern differences between batches of Copaxone, a highly complex drug containing billions of peptides, and various purported generic versions of the drug.


Richard Denny

Latest:

Testing the Limits of Ion Mobility Mass Spectrometry to Compare a Nonbiological Complex Drug Product and Purported Generics—A Case Study with Copaxone

The analysis of oil samples containing many thousands of constituents best illustrates the benefits of ion mobility MS for complex samples. Here, we test the limits of ion mobility MS to discern differences between batches of Copaxone, a highly complex drug containing billions of peptides, and various purported generic versions of the drug.


Tal Hasson

Latest:

Testing the Limits of Ion Mobility Mass Spectrometry to Compare a Nonbiological Complex Drug Product and Purported Generics—A Case Study with Copaxone

The analysis of oil samples containing many thousands of constituents best illustrates the benefits of ion mobility MS for complex samples. Here, we test the limits of ion mobility MS to discern differences between batches of Copaxone, a highly complex drug containing billions of peptides, and various purported generic versions of the drug.


Vaclav Kasicka

Latest:

HPLC 2017 Topic Preview: Affinity Capillary Electrophoresis–A Powerful Tool to Investigate Biomolecular Interactions

This is the final instalment of a series of articles exploring current topics in separation science that will be addressed at the HPLC 2017 conference in Prague, Czech Republic, from 18–22 June.


Jo-Ann M. Jablonski

Latest:

Basic Principles for Purification Using Supercritical Fluid Chromatography

Although supercritical fluid chromatography (SFC) is not a new technique, preparative SFC is becoming increasingly more popular with advances in instrumentation, software and chemistry.


Michael J. Y. Jarvis

Latest:

High-Throughput Quantitative Analysis of Vitamin D Using a Multiple Parallel LC–MS System Combined with Integrated On-Line SPE

A newly developed high-throughput method for the quantitation of vitamin D using both multiplexed LC and on-line SPE is discussed.





I.S. Krull

Latest:

Applicability of Hydrogen–Deuterium Exchange in Comparing Conformations of Innovator to Biosimilar Biopharmaceutical Products

Significant recent advances now enable routine usage of HDX-MS for comparing the conformations of biopharmaceutical products.


Milos Novotny

Latest:

HPLC 2017 Topic Preview: Advances in Glycomics in Biology and Medicine

This is the fifth article in a series exploring current topics in separation science that will be addressed at the HPLC 2017 conference in Prague, Czech Republic, from 18–22 June.


Gerhard Liebisch

Latest:

HPLC 2017 Topic Preview: The Role of LC–MS in Lipidomics

This is the sixth instalment of a series of articles exploring current topics in separation science that will be addressed at the HPLC 2017 conference in Prague, Czech Republic, from 18–22 June.


Stefan Krauss

Latest:

Micro-Pillar Array Column Separations for Proteomics of Liver Organoids

A micro-pillar array format for mapping the proteome of human stem cell-derived liver organoids using timsTOF–MS is presented.



Steven Ray Wilson

Latest:

On the Surprising Retention Order of Ketamine Analogs Using a Biphenyl Stationary Phase

An unexpected retention order for ketamine analogs was observed when using a biphenyl stationary phase for liquid chromatography-mass spectrometry (LC–MS).