Determination of Xylitol in Sugar-Free Gum by GC–MS with Direct Aqueous Injection: A Laboratory Experiment for Chemistry Students

Rajapaksha, Suranga M.; Samarasekara, Dulani; Brown, Jared L.; Howard, L; Gerken, Katherine; Archer, Todd; Lathan, Patty; Mlsna, Todd; Mlsna, Deb

doi:10.1021/acs.jchemed.8b00424

Cited by 5 publications

(2 citation statements)

References 33 publications

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“…Experience of these practical analytical procedures is useful in academia, government, and industry. Laboratory experiments on the use of chromatography (gas and liquid)–mass spectrometry-based methods with applications in the chemical, , environmental, − forensic, biological, and clinical fields are being taught at the universities, but additional training and hands-on experience in these methods should be available in the analytical chemistry and instrumental analysis laboratory courses to provide invaluable skills and experience for undergraduate students.…”

Section: Resultsmentioning

confidence: 99%

Analysis of Pesticides in Plant Foods by QuEChERS and Gas Chromatography–Mass Spectrometry: An Undergraduate Laboratory Experiment

Hengel¹,

Wong

Redman³

et al. 2019

J. Chem. Educ.

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Undergraduate students in an environmental chemistry laboratory course were taught QuEChERS (quick, easy, cheap, effective, rugged, and safe), a sample preparation procedure that is commonly used in pesticide laboratories involving an acetonitrile salt-out extraction of fresh produce samples followed by solid-phase dispersive cleanup using a combination of sorbents. The cleaned extract was solvent exchanged into toluene and analyzed for pesticides by capillary gas chromatography–mass spectrometry in selective ion monitoring mode (GC–MS/SIM). Students utilized QuEChERS to analyze spiked and incurred pesticide residues in several types of plant foods and applied GC–MS/SIM for the simultaneous quantitation and identification of pesticides. Several chemistry, laboratory, and instrumental concepts were demonstrated such as sample preparation, aspects of method validation, and interpretation of chromatographic and mass spectrometric results. This experiment received favorable responses from the students because of the “real-world” applicability of the QuEChERS procedure, the use of GC–MS analysis, and concepts transferred from lecture to the laboratory.

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Section: Resultsmentioning

confidence: 99%

Analysis of Pesticides in Plant Foods by QuEChERS and Gas Chromatography–Mass Spectrometry: An Undergraduate Laboratory Experiment

Hengel¹,

Wong

Redman³

et al. 2019

J. Chem. Educ.

View full text Add to dashboard Cite

show abstract

“…Several experiments utilizing GC–MS to obtain industrial, forensic, and/or environmentally significant data have been successfully implemented by educators to teach undergraduate students about this powerful instrument. Many other experiments have also been published that involve GC–MS analysis of commercial products, such as flavored rapeseed oil, volatile compounds used as fragrance and flavor additives, fatty acids present in commercial cooking oils and fats, caffeine in commercial beverages, xylitol in chewing gum, pesticides extracted from commercial plant foods, hemp fibers, and, perhaps most often, essential oils. , The paper “Analysis of Cannabinoids in Lotions Using High-Performance Liquid Chromatography” by Quiñones et al applies similar concepts, but HPLC was utilized for separation and students went further by creating a calibration curve to allow quantification of cannabinoids present in commercial lotions . In the paper “Chemistry of Cannabis: An Interdisciplinary Course”, Johnston describes the successful development and implementation of a course dedicated to cannabis chemistry .…”

Section: Introductionmentioning

confidence: 99%

Gas Chromatography–Mass Spectrometry Analysis of Cannabis: Undergraduate Organic Chemistry Laboratory Exercise

et al. 2023

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In this laboratory teaching experiment, commercial cannabis oils were analyzed by undergraduate organic chemistry students using gas chromatography–mass spectrometry (GC–MS) to investigate three isomeric cannabinoids commonly found in cannabis products: cannabidiol (CBD), Δ9-tetrahydrocannabinol (Δ9-THC), and Δ8-tetrahydrocannabinol (Δ8-THC). The goal was to introduce GC–MS analysis through the relevant topic of product quality inspection, frequently used in various industries such as pharmaceuticals, cosmetics, etc. and which largely involves analyzing the chemical components of a sample. First, to better understand the cannabinoid analytes, students were taught the differences between these structural isomers, including bond locations, stereochemistry, and functional groupsfactors which pertain to their pharmacology and drug classification. Finally, students were guided through the basics of GC–MS instrumentation and the process of analyzing GC–MS spectra through the characterization of CBD, Δ8-THC, and Δ9-THC present in oil samples.

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Qualitative Analysis of Acetophenone, Naphthalene, and Hexadecane by GC-Triple-Quad-MS Using MRM

Slonecker

Vonderheide

2022

J. Chem. Educ.

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The use of mass spectrometry (MS) is becoming widespread and rather routine in all levels of industry, government, and academia. Coupled with chromatographic methods, this powerful instrumental technique can be used to elucidate the composition of a complex sample and definitively identify constituents while offering the benefits of high-precision quantitative analysis and low detection limits. These attributes, as well as its growing employment, emphasize the need for the undergraduate student to gain practical experience with this instrumental technique. Additionally, it is critical that students observe first-hand the abilities and contrasts of MS analysis versus MS−MS analysis or triple-quadrupole (Q 1 q 2 Q 3 ) multiple reaction monitoring (MRM) analysis. The focus of this experiment was the qualitative analysis of a sample containing three compounds: acetophenone, naphthalene, and hexadecane using a Q 1 q 2 Q 3 GC−MS in single-quad full-scan mode, Q 1 q 2 Q 3 in full-scan mode, and Q 1 q 2 Q 3 in MRM mode. The analytes were specifically chosen to range from extensive fragmentation (molecular ion of low stability) to minimal fragmentation (molecular ion of high stability). Students utilized the MS NIST library to identify the unknown peaks after analysis using the first quadrupole in full-scan mode. They further compared different injection volumes and observed the effect of injection volume on the band shapes and the signal to noise ratio. The students then compiled a table of precursor ion MS peaks from the single-quad full-scan mode. The sample was next analyzed using Q 1 q 2 Q 3 in full-scan mode, and students compiled a table of product ion MS peaks. These were translated to transition ion pairs and compared to instructor-chosen transition ion pairs used in the final MRM analysis. This laboratory exercise allowed the students to use modern instrumentation and analytical techniques to investigate the potential of second stage mass spectrometry, increasing their technical ability and understanding of this critical scientific tool. Moreover, they were able to observe first hand the power of the NIST library for unknown analytes as well as the potential advantages of MRM when selectivity and low detection limits are critical.

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Determination of Xylitol in Sugar-Free Gum by GC–MS with Direct Aqueous Injection: A Laboratory Experiment for Chemistry Students

Cited by 5 publications

References 33 publications

Analysis of Pesticides in Plant Foods by QuEChERS and Gas Chromatography–Mass Spectrometry: An Undergraduate Laboratory Experiment

Analysis of Pesticides in Plant Foods by QuEChERS and Gas Chromatography–Mass Spectrometry: An Undergraduate Laboratory Experiment

Gas Chromatography–Mass Spectrometry Analysis of Cannabis: Undergraduate Organic Chemistry Laboratory Exercise

Qualitative Analysis of Acetophenone, Naphthalene, and Hexadecane by GC-Triple-Quad-MS Using MRM

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