• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.278-295
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• 2014

Fast and accurate multi-residue pesticides inspecting method needs in Agro-Fishery Products Inspection Center. So, We tried to seek the optimum method using GC-TOF/MS, GC-ECD, GC-NPD after QuEChERS sample preparation. In GC-TOF/MS, 138 kinds of pesticide were spiked at 0.3 and $0.5{\mu}g/g$for the identification and quantification in lettuce sample. Recoveries of 77 pesticides were between 70 and 130% with RSD (relative standard deviation lower than 20% at $0.3{\mu}g/g$. In GC-ECD, NPD, 146 kinds of pesticide were spiked for the identification and quantification in lettuce. Recoveries of 61 species were between 70 and 130% with lower than 20%. These results indicated that GC-TOF/MS, GC-ECD, NPD analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in vegetables.

• Analytical Science and Technology
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• v.25 no.6
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• pp.410-415
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• 2012

In this study, a fundamental study was conducted to establish the method for quantitative analysis and pretreatment of triclosan, one of the chemicals to be used as bactericides, detergents, and sterilizers. The extraction efficiency of triclosan was the highest when it was extracted by soxhlet apparatus with n-hexane, and it showed a satisfactory result when the samples were analyzed with both GC/ECD and GC/MS. To evaluate the reproductivity of the results, each 30 reference samples made with paper filter and cotton wool was prepared in this study. From the results with high extraction effectiveness, low analysis deviation, and good statistical analysis data, the method for the extraction and analysis for triclosan were resonable for the paper and textile samples applied in this study.

• 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.

• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.110-117
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• 2018

The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

• Analytical Science and Technology
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• v.15 no.3
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• pp.185-189
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• 2002

International Olympic Committee (IOC) prohibits the use of cyclofenil for male. To prove whether cyclofenil product was taken or not, the analytical method in urine using GC/MS was established. The extraction recoveries of cyclofenil and its metabolites were higher in the range of pH 5-9. Because the parent drug (cyclofenil) was not excreted in urine, metabolites were detected and theses were used as a criteria of cyclofenil dose. Therefore the metabolites were hydrolyzed, extracted at pH 9.6, derivatized with MSTFA and analyzed by GC/MS.

• 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.

• Mass Spectrometry Letters
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• v.4 no.1
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• pp.18-20
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• 2013

Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

• Journal of the Korean Society of Clothing and Textiles
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• v.33 no.6
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• pp.980-989
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• 2009

Amur cork tree was extracted in methanol with the purpose of investigating the most effective extraction procedure for detecting the chromophore using the GC-MS analysis. Different procedures of waterbath and hotplate extractions were carried out and five different GC-MS instrument parameters including the operating temperatures in the GC capillary column and the MSD scan range were tested for their efficiencies. Berberine was determined by the detection of dihydroberberine at 15.0 min r.t. Hotplate was a better device for extracting amur cork tree than waterbath shaker either with or without presoaking in the room temperature. Water was not an adequate extraction medium for the berberine detection. The most effective GC-MS parameter was Method 4; the initial temperature at $50^{\circ}C$ followed by the temperature increase of $23^{\circ}C$/min until $210^{\circ}C$, then increase of $30^{\circ}C$/min until the final temperature reach at $305^{\circ}C$, then hold for 14 minutes to maintain the total run time 24.12 minutes. The MSD scan range for Method 4 was $35\sim400$m/z.

• Korean Journal of Food Science and Technology
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• v.21 no.6
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• pp.749-754
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• 1989

The essential oil was prepared by a gas co-distillation method from flavedo of Poncirus trifoliata and was analyzed by GC/ retention index (RI) and GC/MS. The essential oil prepared by a gas co-distillation gave a whole fragrance of Poncirus trifoliata. The identification of the flavor components was performed by multi-dimensional analysis using GC/RI and GC/MS. GC/RI and GC/MS were complementary to each other. In applying GC/RI for identification, it was more effective when two columns of different polarities were used. Thirty volatile flavor constituents were identified in Poncirus trifoliata. Limonene, myrcene, ${\beta}-caryophyllene,\;trans-{\beta}-ocimene$, ${\beta}-pinene$, 3-thujene and 7-geranyloxycoumarin were the major constituents and cis-3-hexenyl acetate, n-hexyl acetate, 2-methyl acetophenone, elixene and elemicine had not been reported earlier as citrus components.

• Preventive Nutrition and Food Science
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• v.3 no.2
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• pp.111-118
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• 1998

To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.