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Pittcon 2020

Pittcon 2020
Conference & Expo

Pittcon
Restek at Pittcon 2019
Booth Giveaway

SHORT COURSES:

MONDAY, MARCH 2
Short Course Office S100C, 08:30 AM–12:00 PM
SC1230: Injection Techniques in Gas Chromatography
Jaap de Zeeuw
Restek Corporation
For more information, email Jaap de Zeeuw.
Read abstract

In gas chromatography, the most important process is to get the sample into the column. If sample transfer is not optimized, the results will not be reliable. The goal of this course is to understand the different injection techniques used, and the process of how to obtain a narrow injection band.

TUESDAY, MARCH 3
Short Course Office S100C, 08:30 AM–12:00 PM
SC1231: Practical Maintenance and Troubleshooting in Gas Chromatography
Jaap de Zeeuw
Restek Corporation
For more information, email Jaap de Zeeuw.
Read abstract

In gas chromatography, 90% of the trouble experienced happens in the injection system. In this course, we will discuss the purpose and impact of its critical parts (consumables), present split and splitless injection, and examine how this impacts a maintenance schedule. At the end, we will discuss a series of practical examples via troubleshooting exercises.

ORAL SESSIONS

SUNDAY, MARCH 1
Room W176A, 3:45 PM–4:05 PM
5-3-7: Comparison of Techniques for Terpene Analysis via Gas Chromatography-Mass Spectrometry (GC-MS)
Colton Myers (presenter)
Restek Corporation
For more information, email Colton Myers.
Read abstract

Terpenes are a class of organic compounds that are comprised of isoprene units based on 5 carbons. These compounds are produced by a variety of plants and generally have a strong odor. Different terpenes, and ratios of terpenes, can be found in different cannabis chemovars. Not only are terpenes identified in cannabis for their aromas and flavors, but they also play a major role in the entourage effect. The entourage effect is believed to be created by the synergistic interaction between cannabinoids, terpenes, and other naturally occurring compounds, which gives each cannabis chemovar its own unique experience. This research was focused on determining the terpene content for cannabis flower; however, hops were used due to legal issues. Comparisons will be shown for headspace (HS)-GC-MS using HS-Syringe, a HS-SPME Arrow-GC-MS, and direct immersion (DI)-SPME Arrow-GC-MS. A simple, robust method will be presented demonstrating a rapid and accurate analysis of terpenes in cannabis flower.

MONDAY, MARCH 2
Room W177, 8:30 AM–8:50 AM
5-16-1: Ultrafast Screening of Controlled Substances in Biofluids via Coated Blade Spray MS/MS and Confirmation via LC-MS/MS
Gary Stidsen (presenter)
Restek Corporation
For more information, email Gary Stidsen.
Read abstract

Coated Blade Spray (CBS) is a technology that combines sample preparation and direct coupling to mass spectrometry (MS) on a single device. CBS is a coated stainless-steel sheet with the shape of a small sword with an ultra-thin SPME coating that permits rapid enrichment of small molecules present in complex samples via free-concentration. As a substrate spray technology, it can generate instrumental signal on a mass spectrometer by supplying a small amount of organic solvent to the coated area of the device, and then applying a strong electrical field to the non-coated area of the device, which in turn generates gaseous ions from the tip of the CBS via electrospray ionization (ESI). In this work, we explore, for the first time, its application towards the determination of several controlled-substances/pain-management drugs in oral fluids. As a proof-of-concept, we investigate its applicability to large (>100 µL) and small (<20 µL) sample volumes of Oral Fluids (OF). Hydrophobic-Lipophilic Balance (HLB) particles were selected as the extraction phase and CBS devices. The optimized CBS-MS/MS method demonstrated outstanding precision (RSD<10 %), LOQs equal to or below 5 ng/mL and excellent linearity (R2 > 0.99) for most of the target molecules (e.g., cocaine, fentanyl, EDDP, fluoxetine) over the range evaluated. Furthermore, it was proven that the methodology could also be applied to small sample volumes such as oral fluid droplets. A comparison between the CBS-MS/MS method and the confirmatory test (via LC-MS/MS) showed good agreement (R2 ≥ 0.95) between both approaches for all analytes.

Room W176C, 2:30 PM–2:50 PM
5-28-4: Rapid Screening and Quantitation of Multiresidue Veterinary Drugs in Bovine Tissue by Direct Interfacing of SPME to MS/MS
Janusz Pawliszyn (presenter)
University of Waterloo
For more information, email Dave Bell.
Read abstract

The widespread use of veterinary drugs in food-producing animals is an issue of growing concern. Most established methods used for screening and quantitation of multiresidue veterinary drugs in complex biological matrices such as tissue require the use of liquid chromatography coupled with mass spectrometry (MS). These methods can be time-consuming, particularly when a large number of samples are to be analyzed. An alternative approach to chromatography is to directly couple the sample to mass spectrometry. Coated blade spray (CBS) is a solid-phase microextraction-based technology that can be interfaced to MS instrumentation for rapid qualitative and quantitative analysis of complex matrices such as biological tissue. In this study, we present, for the first time, the use of CBS-MS/MS for rapid and high-throughput screening/quantitation of 106 veterinary drugs in bovine tissue. The selected drugs represent more than 12 different classes of drugs characterized by varying physical and chemical properties. The fully automated sample preparation allows for total analysis time per sample of 1 min time with screening in both negative and positive ionization modes. Only two internal standards were used for correction, one for negative mode and one for positive mode. Excellent accuracy and precision results were achieved with more than 90% of analytes falling within the 70−120% range of their true concentrations and RSD ≤25% at 0.4X, 0.75X and 1.5X concentration levels, where X is the maximum residue level (MRL) of analyte allowed in tissue. In terms of linearity, the majority of analytes achieved linear correlation coefficients > 0.99 within the evaluated range of concentrations (0.25-2.5X). In terms of LOQs, the method was able to meet both Canadian and U.S. regulatory levels for 106 compounds.

Room W175B, 3:45 PM–4:05 PM
5-22-7: Using Method Translation to Increase Throughput While Maintaining the Same Elution Profile
Linx Waclaski (presenter)
Restek Corporation
For more information, email Linx Waclaski.
Read abstract

Existing methods can be accurately scaled down to smaller, high-efficiency, narrow-bore columns using Restek’s EZGC method translator. With a scaled-down column, a properly translated method, and a GC Accelerator kit (when necessary), you can obtain the same chromatographic separation—often with greater sensitivity—in a fraction of the time without making a capital investment. Real-world examples will be given for semivolatiles, pesticides, and petro applications.

TUESDAY, MARCH 3
Room W178B, 9:45 AM - 10:20 AM
2-28-3: Coated Blade Spray–Mass Spectrometry: A Versatile Tool for Qualitative and Quantitative Analysis
Dave Bell (presenter)
Restek Corporation
For more information, email Dave Bell.
Read abstract

Coated Blade Spray (CBS) is a SPME-based technology that allows for analyte collection and direct-to-MS interface from a single device. Fundamentally, CBS is a coated stainless-steel sheet with the shape of a small sword, which, thanks to its ultra-thin coating, permits rapid enrichment of small molecules present in complex samples and ionization via ESI mechanism. The CBS analytical protocol comprises three simple steps: 1.) Analyte-enrichment, by extracting either from a vessel containing the sample (e.g., beer samples on a 96-well plate), or by implanting the device into the sample (e.g., stabbing animal tissue) for a fixed period of time; 2.) Coating-cleaning, which involves fast removal of any matrix that may be on the coated surface by immersing the CBS device in water for a few seconds (<5s); and 3.) Instrumental analysis, which is performed by applying a few 10 µL of an elution solution (e.g., methanol-water 95:5 with 0.1% formic acid) onto the coated area. After 10s, a high-potential difference (3.75 kV) is applied to the non-coated area of the blade, which results in the generation of ESI from its tip. Herein, we demonstrate how CBS, coupled to high resolution mass spectrometry (HRMS) and tandem mass spectrometry (MS/MS), enables either rapid profiling of aqueous and solid matrices or semiquantitative analysis of target analytes in biofluids and food samples. Similar to other SPME technologies, CBS allows performing sampling remotely, while simplifying the transportation of the sample and keeping a clean “sample-extract” that retains relevant chemical information of the sample. Some examples to be discussed in this presentation include the profiling of tissue and beer samples with a Time-of-Flight MS, and the quantitation of drugs of abuse in several biological fluids, such as saliva and blood, via tandem mass spectrometry.

Room W184D, 11:05 AM–11:25 AM
5-30-8: Sample Recognition via Coated Blade Spray-High Resolution Mass Spectrometry
Nathaly Reyes-Garces (presenter)
Restek Corporation
For more information, email Nathaly Reyes-Garces.
Read abstract

Coated Blade Spray (CBS) is a technology that allows for analyte collection and direct-to-MS interface from a single device. Essentially, CBS is a coated stainless-steel sheet with the shape of a small sword which, thanks to its ultra-thin coating, permits rapid enrichment of small molecules present in complex samples and ionization via ESI mechanism. Herein, we demonstrate as a proof-of-concept how CBS coupled to High Resolution Mass Spectrometry (HRMS) enables rapid profiling of aqueous (i.e., beer) and solid matrices (i.e., animal tissue). Unlike other ambient-ionization technologies, CBS allows you performing sampling remotely, cleaning up the sample and retaining relevant chemical information that facilitates its classification via chemometric tools. Beer samples from different types/manufacturers/world regions were purchased at a local store. Samples (300 µL) were deposited on a 96-well plate and analyte collection was performed in high-throughput configuration (i.e., 96-CBS devices concomitantly) for 5 minutes. The discriminant analysis of principal components (DAPC) in combination with Kernel Principal Component Analysis (KPCA) allowed for adequate classification of each of the beer brands under evaluation. Further, when using 60 principal components (PC), the leave-one-out cross validation (LOOCV) and the Support Vector Machine (SVM) unequivocally identified each of the samples. Likewise, CBS was capable of differentiating different types of meat samples (e.g., lamb, beef, chicken, and pork). The DAPC-KPCA plot showed clear distinction of each meat. By using 60 PC, the LOOCV and SVM lead to a predictability of 94 and 96%, respectively. In a third experiment, CBS was used to differentiate diverse fish samples. The DAPC-KPCA plot showed clear distinction of each species. Similar to the meat samples, by using 60 PC, the LOOCV and SVM lead to a predictability of 94 and 96% of the fish samples, respectively.

Room W176A, 1:30 PM–1:50 PM
5-39-1: Simultaneous Analysis of Ultrashort-chain, Alternative, and Legacy PFAS: Method Development and Application to Water Sample
Shun-Hsin Liang (presenter)
Restek Corporation
For more information, email Shun-Hsin Liang.
Read abstract

Current LC-MS/MS methods for per- and polyfluoroalkyl substances (PFAS) monitoring do not address the analysis of newly trending ultrashort-chain (C2 and C3) compounds due to their insufficient retention on typical reverse-phased (RP) columns. It is of importance to monitor these compounds for their ubiquitous occurrence in aqueous environmental samples. This presentation will discuss the LC-MS/MS method development and evaluation for C2 and C3 PFAS analysis and analytical methodologies for simultaneous chromatographic determination of ultrashort-chain, alternative, and legacy PFAS. A direct injection method was evaluated by precision and accuracy analysis of fortified field water samples including tap water, river water, groundwater, and sewage treatment (effluent) water for ultrashort-chain PFAS analysis. The analysis was performed using a Shimadzu Nexera X2 LC system coupled with a SCIEX Triple Quad 4500 MS/MS. It was shown that C3 compounds, PFPrA and PFPrS, could be analyzed together with alternative and legacy PFAS with this RP methodology. A critical challenge was encountered when C2, trifluoroacetic acid (TFA) was added to the PFAS analyte list using typical reversed-phase column due to its minimum retention on the column. Implementing a unique hybrid HILIC/ion exchange column, a fast and easy LC method was developed for simultaneous analysis of TFA (C2), C3, C4, and C8 PFAS. This method provides convenient setup and high throughput analysis for the lab interested in adding ultrashort-chain compounds to PFAS assay

Room W176B, 1:50 PM–2:10 PM
5-40-2: Analysis of ppm-ppb Levels of Nitrous Oxide (N2O) via GC Using Split, Direct, and Stack Injection
Jaap de Zeeuw (presenter)
Restek Corporation
For more information, email Jaap de Zeeuw.
Read abstract

While N2O is considered a greenhouse gas, it has a variety of beneficial uses in multiple industries. We all know it as “laughing gas,” thus the analysis is commonly done in medical and forensic labs. N2O is soluble in fat and inhibits bacterial growth, which makes it an ideal propellant in cans of whipped cream. It’s also a powerful oxidizer, yet stable at room temperature, so it powers our rockets into space. Analysis of this light gas is often performed in the ppb concentrations in atmospheric samples. So, all the mentioned characteristics make it an easy gas to analyze using gas chromatography. Separation of N2O from permanent gases at room temperature can be attained using several adsorbents. The large surface area of those materials offers enough retention for the light analytes to separate without using sub-ambient temperatures. Here, we will discuss the separation on different column types. Used mostly are the porous polymer type PLOT columns —often a number one choice for this analysis. Porous polymers are very inert and will not irreversibly adsorb components. CO2 and N2O will be separated at 40°C with enough resolution. Also, molecular sieves using carbon or zeolite 5A are very interesting as they offer high retention, and because of this, stacked injections can be applied. This allows low ppm levels of N2O to be measured using TCD. With ECD, it’s possible to analyze low ppb levels

THURSDAY, MARCH 5
Room W176A, 11:05 AM–11:25 AM
5-65-8: Analytical Solutions for the Determination of Pesticides in Cannabis Products
Nathaly Reyes-Garces (presenter)
Restek Corporation
For more information, email Nathaly Reyes-Garces.
Read abstract

The use of cannabis for medicinal and/or recreational purposes has become legal in several states. Regulations that permit the use of different forms of cannabis demand effective and reliable analytical strategies to ensure the safety of cannabis users. Pesticides content is one of the main parameters tested in cannabis and cannabis-derived products due to the risks that these compounds pose for human health. The list of regulated pesticides varies from state to state: Oregon, for instance, set control levels for 59 pesticides whereas California law requests testing for 66 (58 pesticides also regulated by Oregon plus 8 more). The main challenges associated with pesticides testing rely on the broad range of physicochemical properties of these compounds, the low action levels requested by the law, and the complexity and diversity of matrices to be analyzed. The purpose of this work is to present sample preparation and instrumental strategies for the accurate quantitation of the Oregon and California lists of pesticides in cannabis products. Parameters such as sample clean up, extract stability, method linearity, accuracy, precision, and matrix effects were all taken into consideration. Our results evidence that solid phase extraction (SPE) can provide a simple yet effective way to remove interferences from sample extracts. In addition, matrix effects vary significantly from matrix to matrix; hence, adequate chromatographic separation, the use of ion ratios, and internal standards are all important to ensure reliable results.

Room W176C, 3:05 PM–3:25 PM
5-72-5: Understanding the Fundamentals Behind the Operation of Coated Blade Spray-Mass Spectrometry
Dave Bell (presenter)
Restek Corporation
For more information, email Dave Bell.
Read abstract

Coated Blade Spray (CBS) is an SPME-based analytical technology that facilitates collection of analytes of interest from a sample and the direct interface to mass spectrometry systems via a substrate spray ionization. The device comprises a thin-flat sheet with a pointed tip, and it is manufactured of a conductive substrate such as stainless steel. As an SPME device, the substrate is partially coated with an extraction phase comprised of polymeric particles and a binder. The function of the polymeric particles is to enrich the analytes of interest from the sample matrix while collecting the least amount of interferences. As a direct to MS device, the device requires a pre-wetting of the extraction material so to elute the analytes collected on it. Subsequently, a differential potential is applied between the non-coated area of the substrate and the inlet of the MS system generating an electrospray at the tip of the CBS device.

In this work, we present a thorough examination of the fundamental parameters behind the operation of CBS, including the following: analyte extraction (e.g. ,coating chemistry, coating thickness, extraction time), analyte elution (e.g., elution time, elution solvent), and ionization conditions (e.g., applied voltage, distance to the MS inlet). As a proof of concept, plasma and urine samples were selected as matrices under study. A panel of substances with different physicochemical properties was selected as target compounds so to enable a better understanding of each of the steps in the analytical workflow. Our results demonstrated that best extraction times must be selected on the basis of signal-to-noise ratios rather than mere instrumental signal as when compared to SPME coupled to LC-MS. Likewise, the selection of the extraction, elution, and ionization conditions must be done aware of possible synergies among them. Design of the experiments proved to be fundamental to understand best conditions for specific analyte-matrix pair.

RESTEK TECHNICAL POSTERS

TUESDAY, MARCH 3
Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
603-10P: The Analysis of Mycotoxins in CBD Oils by LC-MS/MS
Nathaly Reyes-Garces (presenter)
Restek Corporation
For more information, email Nathaly Reyes-Garces.
Read abstract

Fungi that readily colonize crops such as cannabis are capable of producing secondary metabolites known as mycotoxins that can cause disease and death in humans. The two primary types of mycotoxins associated with cannabis are aflatoxins and ochratoxins. These mycotoxins are produced by the fungal species Aspergillus flavus and Aspergillus parasiticus for aflatoxins, and Penicillium verrucosum as well as Aspergillus ochraceus for ochratoxins. Crops are susceptible to contamination from seed through storage with most effort focused on mitigation during harvest and storage. The thermal stability of mycotoxins presents a particular challenge as the likelihood is high that existing crop contamination will persist and concentrate during processing into oil and extracts causing levels to rise above state limits.

Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
603-11P: The LC-UV Analysis of 19 Cannabinoids of Interest in Commercially Available CBD Products
Nathaly Reyes-Garces (presenter)
Restek Corporation
For more information, email Nathaly Reyes-Garces.
Read abstract

More than 100 cannabinoids have been isolated from cannabis in addition to the five most commonly tested: THC, THCA, CBD, CBDA, and CBN. While methods have been published that show the separation of these major cannabinoids, many do not take into account the possibility of interference from other cannabinoids that may be present. This is most problematic in concentrates where minor cannabinoids can be enriched to detectable levels that were not observed in the flower. Additionally, some terpenes have been shown to absorb UV light at 228 nm, the wavelength that cannabinoids are typically detected at, which can result in an additional source of interference. In this study, the LC-UV separation of 19 cannabinoids of interest was performed while monitoring for the potential impact from minor cannabinoids and terpenes on reported potency values. The method is applied to commercially available CBD products that have recently become suspect due to inaccurate label claims. Alternate methods to decrease the time of analysis and reduce solvent consumption are also discussed.

Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
604-5P: Quantitation of Mycotoxins in Food Matrices Comparing Stable Isotope Dilution Assay with Matrix Matched Calibration Methods
Shun-Hsin Liang (presenter)
Restek Corporation
For more information, email Shun-Hsin Liang.
Read abstract

Mycotoxins are secondary fungal metabolites produced by mold that may be found in food or feed. They can cause severe health problems in humans and animals and can result in significant economic losses. Among the hundreds of toxic mycotoxins, aflatoxins, fumonisins, deoxynivalenol, ochratoxin A, HT-2 toxin, zearalenone, and T-2 toxin are considered as a major concern for corn, wheat, peanuts, and other agricultural products. LC-MS has become the standard and is now widely used for routine mycotoxin analysis or identification. One of the challenges faced by LC-MS techniques is the matrix effect caused by the use of electrospray ionization (ESI). Generally, sample preparation, chromatographic, and calibration techniques are the common strategies for reducing negative effects of matrix effects. Standard addition, matrix matching, and stable isotope dilution assay (SIDA) are all possible calibration solutions. In this work, a quick "dilute-filter-shoot" method was used for sample preparation. A 7-minute LC-MS/MS method using a biphenyl column was developed and verified for quantifying 12 mycotoxins in 4 matrices (corn, peanut butter, brown rice, and corn/wheat mixture). Both SIDA and matrix-matched calibration methods were applied, compared, and evaluated in terms of recovery, efficiency, advantages, and limitations.

WEDNESDAY, MARCH 4
Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
615-6P: Analysis of Acrylamide Using an Aqueous Compatible Reversed-Phase Column by LC-MS/MS Detection
Shun-Hsin Liang (presenter)
Restek Corporation
For more information, email Shun-Hsin Liang.
Read abstract

Acrylamide is a by-product of the Maillard reaction when aldehyde sugars and the amino acid asparagine react at elevated temperatures. Acrylamide can be found in foods such as roasted coffee and starchy foods, such as potato chips, toasted bread, and cereal. Studies on lab mice have shown that excessive ingestion of acrylamide can result in neurological and reproductive side effects. Acrylamide has also been classified as a Category 1B carcinogen, having caused cancer in animal testing. With these risks, regulations have been put in place in the European Union, and a Prop 65 warning was issued in California regarding acrylamide. With health concerns and added regulation, there has been an increase in need for chromatographic determination of acrylamide in foods. Leading LC-based chromatographic methods that quantify acrylamide often suffer from irreproducibility and poor column lifetimes. This results in longer turnaround times, less instrument uptime, and poor data quality. A new method has been developed that addresses both pain points that utilizes a reproducible, retentive, and robust analytical column. The benefits of the new method will be discussed showing examples of difficult matrices, such as coffee and potato products, with particular emphasis on the role of the analytical column on the success of the analytical method.

Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
615-10P: Improving Sample Preparation and Analysis for Organochlorine Pesticides Using an Optimized Extraction and Analysis
Linx Waclaski (presenter)
Restek Corporation
For more information, email Linx Waclaski.
Read abstract

Although organochlorine pesticides have been banned for more than half a century, their persistence in the environment requires environmental monitoring well into the future. Environmental labs are often required to prepare, analyze, and report on large quantities of samples with short notice. In addition to this, the cost of performing the work sometimes exceeds the revenues generated and, therefore, a more cost-effective solution is needed. In this presentation, a methodology is introduced that is designed specifically to reduce the time and cost associated with preparing and analyzing organochlorine pesticide samples. What this means for the laboratory is less time invested in each individual sample, ultimately leading to higher sample throughput, equating to lower overall laboratory costs. In addition to an efficient solid phase extraction method, the use of a GC oven volume reduction is utilized to increase instrument ramping capability, thereby shortening analysis time per sample. Total instrument cycle time is around 10 minutes per sample, with all analytes eluting in close to five minutes using a dual column set-up and micro-ECD detection.

Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
615-8P: Reducing Instrument Downtime for Polychlorinated Biphenyl Analysis Using an Optimized Graphitized Carbon Black Cartridge
Jaap de Zeeuw (presenter)
Restek Corporation
For more information, email Jaap de Zeeuw.
Read abstract

Some of the most commonly encountered problems experienced by those analyzing environmental samples for polychlorinated biphenyl are instrument downtime and shortened calibration periods, both due to the deleterious effects of coextracted matrix components that are introduced into the analytical instrument during sample injection. In addition to this, chromatographic interferences complicating identification and quantification have also made life difficult for environmental analysts. Although there are cleanup options such as Florisil, silica gel, and alumina, these normal phase solutions often do not adequately remove the less polar and high molecular weight compounds that are responsible for diminishing instrumental performance and sample path inertness. In this presentation, a cartridge is introduced that is designed specifically to be utilized exactly like the commonly employed Florisil cartridge, but to a much superior effect for highly pigmented and inlet degrading samples. What this means for the analyst is calibration curves that can be maintained longer and reduced instrument maintenance, ultimately leading to higher sample throughput.

Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
615-9P: Evaluation of Capillary Columns for the Analysis of Volatile Organic Compounds Using Computer Modeling Software
Colton Myers (presenter)
Restek Corporation
For more information, email Colton Myers.
Read abstract

With an ever-expanding target list and many different stationary phases available, choosing the correct column can be difficult. Every stationary phase has limitations, whether it’s temperature, stability, or selectivity. With the advent of new revisions to the method target, coelutions of analytes that share common ions is almost certain to be a problem. The first columns used for analyzing volatiles were based on diphenyl/dimethyl polysiloxane stationary phases. The main advantage of these polymers are their resistance to oxidative breakdown and their low bleed compared to cyanopropylphenyl polysiloxane (i.e., 624) phases. The disadvantage is the incomplete resolution of the early eluting compounds, poor overall selectivity of halogenated-aromatics, and branched aromatics. Modeling software allows precise evaluations of selectivity specific to the users compound list and chosen stationary phase. It is possible to predict retention times and optimized chromatographic methods without the need to analyze compound sets under many different empirical conditions. The program allows users to adjust stationary phase type, film thickness, temperature, column length, column internal diameter, and flow. This program will be used to examine the most commonly used stationary phases for the analysis of volatiles and demonstrate advantages of each phase under a given set of conditions.

THURSDAY, MARCH 5
Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
625-13P: Optimizing GC-MS and GC-MS/MS Analysis of 3-MCPD and Glycidyl Esters
Linx Waclaski (presenter)
Restek Corporation
For more information, email Linx Waclaski.
Read abstract

3-MCPD and glycidyl esters in edible oils are contaminants that are formed through refining processes, and several of these substances have been classified as possible human carcinogens. Methods, which are similar to one another, have been developed by ISO, AOCS, and DGF for analyzing these contaminants. While the methods cover extraction and derivatization techniques in detail, very little attention is paid to the GC-MS methods. With emerging automated systems, it is important to simplify and speed up the method by optimizing the parameters to include switching to split injection. The initial optimization of the temperature program led to an 8-minute decrease in the analysis time, and additional time can be saved by utilizing free method development software. The employment of split injection resulted in better peak shape and achieved limits of detection that were comparable to splitless injection. Further evaluation of split injection revealed that the same performance is achieved regardless of inlet temperature resulting in greater flexibility for different inlet configurations.

Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
625-14P: A Robust Column for the Analysis of Benzene and Toluene in Motor and Aviation Fuel Containing Ethanol per ASTM D3606-17
Jaap de Zeeuw (presenter)
Restek Corporation
For more information, email Jaap de Zeeuw.
Read abstract

Laboratories facing the challenge of quantifying both benzene and toluene in finished motor and aviation fuel containing ethanol must use the modified ASTM D-3606-17 method mandated by the US EPA. This column set prevents the coelution of benzene with ethanol, thus assuring accurate quantification of benzene. Toluene quantitation is straightforward in that there are no coelution issues. The scope of the method for quantifying benzene is 0.1% to 5% by volume, and the toluene range is 2% to 20% by volume. With the addition of butanol blended fuel slowly entering the market, this same packed column set with a slight modification of the GC oven parameters, which also uses methyl ethyl ketone (MEK) as the internal standard, can be used for the analysis of ethanol-free gasoline containing butanol blend with no concerns of inconsistent retention times and/or coelutions of critical components. This packed column set will satisfy both Part A and Part B of the D 3606-17 method.

Back of 4500-4600 Aisle, Expo Floor, 10:00 AM–12:00 PM
629-8P: Application of Large Volume SPME Fibers
Colton Myers (presenter)
Restek Corporation
For more information, email Colton Myers.
Read abstract

Traditional SPME fiber technology has remained virtually unchanged over the last three decades and is subject to the following major drawbacks: limited mechanical stability and small phase volumes. A large volume fiber (i.e., SPME Arrow) has been developed to overcome these shortcomings. When compared to a traditional SPME fiber, the Arrow’s increased diameter (1.1 mm vs. 0.5 mm) and length (20 mm vs. 10 mm) result in a larger sorption phase surface area (up to 6x) and volume (up to 20x) as well as an increase in mechanical robustness. The following presentation will provide side-by-side applications of traditional SPME fibers and SPME Arrows for acrylamide in potato chips/coffee; polycyclic aromatic hydrocarbons (PAHs) in drinking water; and residual solvents in cannabis extracts.

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