• Journal of Korean Society of Environmental Engineers
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• v.36 no.6
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• pp.387-395
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• 2014

A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC-MS/MS) has been developed, allowing the simultaneous multi-analyte determination of 11 synthetic fragrances (SFs) in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 10.9%). The extraction efficiencies were above 83% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~4.1 ng/L and 6.6~12.9 ng/L, respectively. The developed method offers the ability to detect 11 SFs at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 11 SFs. The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.

• Mass Spectrometry Letters
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• v.15 no.2
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• pp.79 -94
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• 2024

Over the past few decades, new psychoactive substances (NPS) have become prevailing. With the widespread emergence of NPS, phenethylamines (PEAs) have become one of the groups abused most which PEAs, along with other stimulants, make up the majority of stimulants. When determining the NPS, the methods for screening and confirmation are crucial which assesses the reliability of testimony. In this study, a set of GC/MS methods employing two derivatizing agents for determining 76 target PEAs in urine was established and further applied for authentic sample analysis. Five PEAs (N,N-DMA, PMMA, 4-CA, amphetamine, and methamphetamine) with contents over their LLOQs were detected in thirteen of the twenty tested samples. In order to compare the result from the GC/MS methods with the previously established LC-MS/MS method, Cohen's kappa coefficient and McNemar's test were applied for statistical analysis. Perfect agreement between GC/MS and LC-MS/MS techniques for determining target PEAs is demonstrated by the Kappa coefficient for each of the five detected targets.

• YAKHAK HOEJI
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• v.46 no.2
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• pp.93-97
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• 2002

Methidathion is one of the organophosphorus pesticides commonly used for stamping out harmful pests in farming areas. This paper presents a fatality due to methidathion intoxication and describes the distribution of methidathion in postmortem blood and tissues obtained at autopsy. Qualitative identification of methidathion was achieved by TLC, GC and GC/MS, and quantitative analysis was performed by GC with thermionic specific detector (TSD). The analytes in postmortem specimens were extracted by liquid-liquid extraction (LLE) with ethylether. After the ethylether layer was evaporated, the residue was partitioned into hexane and acetonitrile, and the acetonitrile layer was used for analysis. Tissue specimens were homogenized with 4% perchloric acid and applied for LLE. After extraction, the extracts were reconstituted 100 $\mu\textrm{g}$ pyraclofos (IS, 100 $\mu\textrm{g}$/ml in methanol) for GC and GC/MS analysis. On analysis of postmortem specimens, methidathion was identified and quantitated. The methidathion concentrations were 2.0 $\mu$l/ml in blood, 24.4 $\mu\textrm{g}$/g in liver, 13.9 $\mu\textrm{g}$/g in lung, 21.8 $\mu\textrm{g}$/g in kidney, respectively.

• Journal of Environmental Health Sciences
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• v.35 no.4
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• pp.322-333
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• 2009

In this study, a measurement method was evaluated for the determination of polycyclic aromatic hydrocarbons (PAHs) in the ambient atmosphere. PAHs were sampled by high-volume samplers, and were then analysed with a GC/MS system. Particulate PAHs were collected on $8"{\times}10"$ quartz fiber filter, while vapor phase PAHs were adsorbed on polyurethane foam (PUF). Target compounds included a total of 36 PAHs, which are known to be frequently detected in the urban atmosphere. It was not necessary to clean-up samples before samples were analyzed using GC/MS, and the overall performance of the method was tested by a variety of quality control and quality assurance schemes. It is generally known that the clean-up procedure can negatively affect the recovery of samples. Precision and accuracy was evaluated using SRM provided by US NIST, and the results were generally satisfactory and reliable. However, the GC/MS method appeared not to be adequate for 6-rings PAHs, such as coronene, due to its lower sensitivity. In addition, collection efficiencies for low molecular compounds, such as 2-rings PAHs, were poor because of the lower retention volume of the PUF adsorbent. As a result, it was concluded that the method based on high-volume sampling and GC/MS analysis can give very reliable data by simultaneous sampling of both particulate and vapor phases for 3-rings to 5-rings PAHs of environmental concern.

• Journal of Adhesion and Interface
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• v.20 no.3
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• pp.102-109
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• 2019

The material constitution of multi-layered thin film coated on the PET base film was analyzed using ATR FT-IR and pyro GC/MS combination. The cross section of the film was acquired by cracking the film after dipping in liquid nitrogen and was observed using optical microscope. Total thickness of the coated film was $70{\mu}m$ and three layers were observed. Since each layers were too thin to analyze directly except the surface layer, analyzable area of each layers were exposed by using a proper solvent and were investigated using ATR FT-IR and pyro GC/MS. Results shows that three layers were commonly consisted of urethane-acrylate copolymers. Also, inorganic and/or metal inclusions detected by XPS and SEM-EDAX were exhibited by nano size $SiO_2$ particles in layer(1) and aluminum flakes in layer(2).

• Food Science of Animal Resources
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• v.41 no.5
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• pp.816-825
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• 2021

This study aims to validate a fast method of simultaneous analysis of 365 LCamenable and 142 GC-amenable pesticides in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively, operating in multiple reaction monitoring (MRM) acquisition modes. The sample preparation was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction. Key method performance parameters investigated were specificity, linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The method was validated at two spiking levels (10 and 50 ㎍/kg), and good recoveries (70%-120%) and relative standard deviations (RSDs) (≤20) were achieved for 92.9% of LC-amenable and 86.6% of GC-amenable pesticide residues. The LOQs were ≤10 ㎍/kg for 94.2% of LC-amenable and 92.3% of GC-amenable pesticides. The validated method was further applied to 100 egg samples from caged hens, and none of the pesticides was quantified.

• Analytical Science and Technology
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• v.16 no.6
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• pp.438-442
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• 2003

The fungicides, used for grape growth and remained in the wine products from domestic and foreign countries such as vinclozolin, dichlofluanid, penconazole, procymidone were quantitatively analyzed after solid-phase extraction using a GC/MS-SIM method. The results obtained were as follows: for all the samples, the content of procymidone was in the range from 2.2 to $76.1{\mu}g/L$, recoveries 81.3-93.1 %, and standard deviation 1.4-3.4 %.

• Journal of Food Hygiene and Safety
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• v.10 no.4
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• pp.239-247
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• 1995

Analytical method for saccharin in foods was developed using gas chromatography/mass spectrometry(GC/MS). Methylation with diazomethane, acetylation with MBTFA, and silylation with MSTFA and MTBSTFA were compared. Methylation of saccharin produced N-methylated saccharin as the major product and O-methylated saccharin as the minor one. Silylation of saccharin with MSTFA and MTBSTFA reasulted in the formation of the correponding O-silylated products, respectively. The derivatization of saccharin was optimized with MSTFA. The ions at m/z 240, 255, and 166 were monitored to characterize saccharin.

• Korean Journal of Food Science and Technology
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• v.45 no.5
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• pp.537-544
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• 2013

This study was performed to establish method of simultaneous determination of fructose, glucose, and sucrose in honey and commercial vitamin drinks by GC and GC/MS. Optimum chromatographic separation of trimethylsilyl-oxime (TMSO) derivatives by GC was achieved on a DB-5 column. Calibration curves for fructose, glucose and sucrose TMSO derivatives by GC were linear in the range of 50-5000 ${\mu}g/mL$, and their $r^2$ values were 0.9999, The limit of detection and limit of quantification of fructose, glucose, and sucrose were 0.68, 0.47, and 0.53 ${\mu}g/mL$, respectively, and 2.27, 1.58, and 1.77 ${\mu}g/mL$, respectively. Average recoveries of fructose, glucose, and sucrose were 100.5, 101.0, and 99.7%, respectively. When the method was applied to 12 honey samples, the average concentrations of fructose, glucose and sucrose were $42.58{\pm}1.97%$, $27.74{\pm}1.16%$, and $0.79{\pm}0.52%$, respectively. The F/G ratio was $1.53{\pm}0.07$. For fructose and glucose contents, results from the GC analysis were similar to those from the HPLC analysis, but the sucrose content was different for each analysis method. We suggest that the GC method is more suitable than other official analytical methods for simultaneous determination of fructose, glucose, and sucrose in honey.

• Bulletin of the Korean Chemical Society
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• v.30 no.10
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• pp.2287-2293
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• 2009

Gas Chromatography-Mass Spectrometry (GC-MS) fingerprint analysis, Principle Components Analysis (PCA), and Hierarchical Cluster Analysis (HCA) were introduced for quality assessment of Curcuma longa L. (C. longa). The GC-MS fingerprint method was developed and validated by analyzing 33 batches of samples of C. longa from different geographic locations. 18 chromatographic peaks were selected as characteristic peaks and their relative peak areas (RPA) were calculated for quantitative expression. Two principal components (PCs) were extracted by PCA. C. longa collected from Guizhou and Fujian were separated from other samples by PC1, capturing 71.83% of variance. While, PC2 contributed for their further separation, capturing 11.13% of variance. HCA confirmed the result of PCA analysis. Therefore, GC-MS fingerprint study with chemometric techniques provides a very flexible and reliable method for quality assessment of C. longa.