• 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.

• Korean Journal of Veterinary Service
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• v.28 no.3
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• pp.285-294
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• 2005

This study was conducted to investigate the extraction method for the determination of organochlorine, organophosphorus and synthetic pyrethroid pesticide residues in beef fat by gas chromatography-mass selective detector(GC-MSD). Twenty one pesticide residues in fat were determined using a simple and rapid procedure based on solid- phase extraction(SPE) clean-up cartridges with octadecyl $(C_{18})-bonded$ porous silica, florisil, $10\%$ deactivated florisil. a tandem $C_{18}$ and florisil and a tandem $C_{18}$ and $10\%$ deactivated florisil. Solvent-solvent extraction using acetonitrile was not satisfied to eliminate fat interference for pesticide residue analysis by GC-MSD, and the recoveries of the method in fat ranged from 16.2 to $57.3\%$ except DDT$(83.2\%)$. The recoveries of SPE methods using a tandem $C_{18}$ and Florisil was $59.6\~123.8\%$ except fenitrothion $(135.2\%)$. the SPE method was verified the satisfactory performance of pre-treatment for pesticide residues analysis in fat by GC-MSD. The efficiency of florisil deactivated with $10\%$ water has been not proved significantly on recoveries of pesticide residues in fat.

• Mass Spectrometry Letters
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• v.14 no.3
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• pp.104-109
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• 2023

Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

• Mass Spectrometry Letters
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• v.3 no.2
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• pp.29-38
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• 2012

A new approach of volatile compounds analysis is proposed using a linear ion trap Orbitrap mass spectrometer coupled with gas chromatography through an atmospheric pressure photoionization interface. In the proposed GC-HRMS/MS approach, direct chemical composition analysis is made for the precursor ions in high resolution MS spectra and the structural identifications were made through the database search of high quality MS/MS spectra. Successful analysis of a complex perfume sample was demonstrated and compared with GC-EI-Q and GC-EI-TOF. The current approach is complementary to conventional GC-EI-MS analysis and can identify low abundance co-eluting compounds. Toluene co-sprayed as a dopant through API probe significantly enhanced ionization of certain compounds and reduced oxidation during the ionization.

• Bulletin of the Korean Chemical Society
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• v.10 no.2
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• pp.196-200
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• 1989

Some s-triazine herbicides, namely simazine, atrazine, and propazine present as trace components in a complex mixture were analyzed by GC/MS and GC/MS/MS methods. Even though monitoring the molecular ions was the best in terms of sensitivity, adequate analysis could not be done when interfering species were present. When doubly charged ions which appeared at characteristic m/z values were monitored, chromatograms were rather free from interference. More importantly, selected reaction monitoring was found to provide a selective means of detection with general applicability.

• Bulletin of the Korean Chemical Society
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• v.26 no.4
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• pp.575-578
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• 2005

Electrospray ionization mass spectrometry (ESI MS) was used, along with gas chromatography-mass spectrometry (GC-MS), to monitor Paal-Knorr synthesis of 2,5-dimethyl-1-phenylpyrrole by condensation of aniline with 2,5-hexanedione. In addition to 2,5-dimethyl-1-phenylpyrrole observed as a single spot by TLC, unexpected dimer size compounds were observed by GC-MS. Dimers and trimers were observed by ESI MS. ESI tandem mass spectrometry was used to select plausible structures for the dimer. ESI MS with or without liquid chromatographic separation is useful for observing oligomeric byproducts with low volatility produced in organic reactions.

• 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.

• Bulletin of the Korean Chemical Society
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• v.23 no.8
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• pp.1097-1102
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• 2002

The mass spectrometry using an ion trap tandem mass spectrometer has been investigated to find optimum conditions for the analysis of benzo(a)pyrene (3,4-benzpyrene). The applicability to a real soil sample was also investigated to verify the usef ulness of the MS/MS (or collision induced dissociation, CID) analysis. The optimum CID condition was 1.5 and 0.45 for the RF excitation voltage and the q value, respectively. For comparison, CID and EI were applied to the analysis of a soil sample. CID analysis was more sensitive than EI analysis of the soil sample. The limit of detection (LOD) of benzo(a)pyrene was 3.18 ng mL-1 and 0.85 ng mL,-1 for EI and MS/MS analysis, respectively. The precision at the soil sample for EI and CID showed relative standard deviations of 6.1% and 4.1%, respectively, and the concentrations were 168 ㎍ kg-1 and 162 ㎍ kg-1 , respectively.

• Korean Journal of Food Science and Technology
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• v.43 no.5
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• pp.544-552
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• 2011

The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 2003.11a
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• pp.113-118
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• 2003

An investigation has been carried out on collision-induced dissociation (CID) in the development of an analytical protocol for the determination of polycyclic aromatic hydrocarbons (PARs) by ion trap tandem mass spectrometry. Two different considerations were used to choose the optimal CID conditions for complex matrix environmental samples, namely, to determine the highest signal-to-noise (SIN) ratio and the other to eliminate the background interferences originated from complex matrix samples. The PAR content of agricultural soil was measured to estimate overall distribution of PAR in throughout the country, we collected and analyzed 226 soil samples from paddy and upland soil. The average content of total PAR in all samples was 236 ${\mu}g$ $kg^{-1}$, and the range was from 23.3 to 2, 834 ${\mu}g$ $kg^{-1}$. The overall distribution of PAR was found to be closely related to the pollution sources, the size of city and the type of industry.