News from LabRulezGCMS Library - Week 44, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 28th October 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!

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This week we bring you applications by Agilent Technologies, Thermo Fisher Scientific, and Shimadzu!

1. Shimadzu: Analysis of Major Psychoactive Compounds in Nutmeg Using GC-MS/MS

• Application

Abstract

Nutmeg is a spice used in a variety of recipes that can be easily purchased by anyone. Among younger people, however, excessive consumption of nutmeg powder for recreational purposes is increasing, causing hallucinogenic effects. However, there are few reports on toxic or comatose-fatal blood levels and their changes over time in cases of nutmeg poisoning. Therefore, an analytical method using GC-MS/MS was devised and applied to a case of nutmeg poisoning in order to determine the blood concentrations of the main psychoactive substances (safrole, myristicin, and elemicin) in nutmeg and their change over time. The limit of detection (LOD) and limit of quantification (LOQ) of the constructed method were 0.14 to 0.16 ng/mL and 0.5 ng/mL (the lowest point of the calibration curve), respectively. Calibration curves showed good linearity, with R2 = 0.996 to 0.997 for all substances in the range of 0.5 to 300 ng/mL. The accuracy for QC (low 1 ng/mL, medium 120 ng/mL, and high 240 ng/mL) and LOQ (0.5 ng/mL) was %RSD 2.4 to 11 % for diurnal variation (n = 5) and %RSD 1.5 to 11 % for diurnal variation (6 days). A systematic error of -2.6 to 2.1 % was obtained.

Introduction

Nutmeg, the dried seed of Myristica fragrans, has been used as a spice and for medicinal purposes all over the world since ancient times and is widely sold at low prices. Because nutmeg contains safrole, myristicin, and elemicin (Fig. 1) as the major psychoactive compounds, they are sometimes intentionally consumed in large amounts to induce hallucinations or intoxication^8)-10). In addition, intoxication by unintentional misuse of nutmeg has recently become a problem. In addition to hallucinogenic effects, too much nutmeg is associated with clinical symptoms such as nausea, vomiting, abdominal pain, agitation, drowsiness, dizziness, tachycardia, blurred vision, dry mouth, and flushing^{5), 9), 11)-14)}. However, the majority of nutmeg overdose cases are mild and unlikely to be fatal^{14), 15)}. Symptoms of nutmeg poisoning usually begin 2 to 8 hours after ingestion^{11), 15), 16)} and subside within a few days^{3), 5), 9), 11), 13), 15)-17)}. Only two deaths worldwide have been linked to the consumption of nutmeg^{15), 18)}.

In a recent study, biological samples were collected from volunteers who ingested nutmeg powder to identify metabolites of major psychoactive substances^19)-23). However, although many cases of nutmeg poisoning have been reported to date, there have been no reports evaluating the blood levels and half-lives of major psychoactive substances, such as safrole, myristicin, and elemicin, during poisoning. Therefore, we developed an analytical method for three psychoactive substances using GC-MS/MS, measured the blood levels of these main substances in patients with nutmeg poisoning, and evaluated their changes over time.

Conclusion

Using a MonoSpin® extraction kit in combination with a GC–MS/MS system, a simple method was devised to detect and quantify safrole, myristicin, and elemicin in human serum. This method was validated and applied successfully to a case of nutmeg poisoning. For this patient, the method quantified the time-course changes and half-life of safrole, myristicin, and elemicin in serum. It is believed that this method will help to provide additional blood-concentration data for nutmeg poisoning cases as well as more accurate toxicokinetic parameters.

2. Agilent Technologies: Analysis of 37 Fatty Acid Methyl Esters on the Agilent 8890 GC Using FID and LUMA Detectors

• Application

Introduction

The analysis of fatty acid methyl esters (FAMEs) is used to characterize lipids in foods, including oils, meats, seeds, and other products. The fatty acid composition of fats is a complex mixture of saturated, monounsaturated, and polyunsaturated compounds with various carbon chain lengths.¹ Because the roles of fatty acids in the body vary depending on their structure, it is necessary to conduct detailed compositional analyses of the fatty acids contained in foods. The analysis of fatty acid composition in food is standard in many governmental, quality control (QC), and contract research laboratories worldwide.

The nutrition labels on food products include much of this information, detailing food composition to help consumers make informed choices.³ Gas chromatography-flame ionization detection (GC-FID) is a commonly used method for analyzing the fatty acid composition in foods. In this application brief, an analysis of a neat 37-component FAME mix standard was conducted using an Agilent 8890 GC system equipped with an FID and LUMA vacuum ultraviolet (VUV) detector. For comparison, several branded oils were also purchased and analyzed.

Conclusion

These results show the advantages of using the LUMA detector coupled with an Agilent 8890 GC system and FID for FAMEs testing. By combining the robustness of the FID and the UV spectral power of the LUMA, users can be confident in their results.

3. Thermo Fisher Scientific: Dual injection for Hydrocarbon Oil Index (HOI) determination in water and soil with helium carrier gas conservation

• Application

Goal

The aim of this application note is to demonstrate the performance of a high-throughput and cost-effective method for the determination of the Hydrocarbon Oil Index (HOI) also known as Total Petroleum Hydrocarbon (TPH), in water and soil samples by using a dual injection configuration and conserving helium gas.

Introduction

Petroleum products are complex mixtures of hundreds of hydrocarbon compounds, ranging from light, volatile, short-chained organic compounds to heavy, long-chained, branched compounds. Petroleum hydrocarbons can enter the environment through industrial accidents, spills, or leaks, and as by-products from commercial or private uses. Contamination of water and soil is a growing concern as lighter TPH fractions float in water and form thin surface films, whereas the heavier fractions accumulate in the sediment at the bottom of the water, affecting bottom-feeding fish and organisms. TPH released in soil can evaporate into the air, dissolve into the groundwater, and move away from the spillage area, contaminating the drinking water supplies, or remain bound to the soil particles for a long period, thus reducing the usability of land for development.

To protect public health from toxic effects due to TPH exposure, many European countries and the United States have made the determination of the content of mineral oils and petroleum products in water and soils a compulsory requirement for quality certifications. Because there are so many petroleum products, it is not practical to measure each one individually, therefore the total amount of all hydrocarbons found in a sample of soil, water, or air is usually monitored.¹

The United States Environmental Protection Agency (U.S. EPA), the International Organization for Standardization (ISO), as well as the Italian Institute of Environmental Protection and Research (ISPRA) have published several methods (U.S. EPA 8015 D,² ISO 16703:2011,³ ISO 14039:2004,⁴ ISO 9377:2000⁵, ISPRA Doc. N. 46/14,⁶ ISPRA Doc. n. 04/11⁷) that can be considered when analyzing TPH in water and soil using gas chromatography
coupled to flame ionization detection.

The Hydrocarbon Oil Index (HOI) represents the total amount of compounds that can be extracted from the sample (potable water, surface water, and wastewater) with a non-polar solvent. The extracted compounds must not absorb on Florisil™ and must elute between n-decane (C10) and n-tetracontane (C40) when analyzed by GC on a non-polar column. Such fraction includes heating oils, diesel fuels, kerosene, lubricants, and transmission fluids.

In this work, the Thermo Scientific™ AI/AS 1610 autosampler in the Gemini configuration for simultaneous dual injections combined with the Thermo Scientific™ HeSaver-H₂ Safer™ carrier gas saving technology was employed to increase the sample throughput and double the productivity while reducing helium consumption and cost per analysis. Method compliance in terms of sensitivity, recovery (C40/C20 ratio), linearity and precision were evaluated for quantitative assessment of the HOI in water and soil samples.

Conclusions

• The Hydrocarbon Oil Index analysis in water and soil is a routine test for environmental laboratories. Robust solutions offering time- and cost-saving opportunities are key to maintain laboratory efficiency and face increasing workloads.
• The TRACE 1610 GC with a dual channel SSL-FID and the AS 1610 autosampler in the Gemini high-throughput configuration can double the number of samples through simultaneous injections, while Chromeleon CDS allows easy management of instrument control, data processing, and reporting for both channels.
• The system performance exceeds the regulatory requirements in terms of recovery, repeatability, linearity, and limit of quantitation, well below the minimum acceptable hydrocarbon contamination.
• The system robustness helps minimize maintenance for extended instrument uptime with consistent results over longer sequences.
• The innovative HeSaver-H² Safer technology used on both channels provides a significant reduction of the helium gas consumption, also during sample analysis, extending 4.5-fold the cylinder lifetime and providing a significant cost savings to the laboratory.