• Journal of Food Hygiene and Safety
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• v.38 no.6
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• pp.420-429
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• 2023

GC-MS/MS using liquid-liquid extraction (LLE) and C18 cartridges was used to identify and quantify levels of chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin and permethrin in bulk raw milk. A calibration curve spanning 10 ng/mL to 200 ng/mL was obtained with a satisfactory correlation coefficient of 0.99. The limits of detection (LOD) and limits of quantitation (LOQ) for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in the matrix ranged from 0.06 to 1.81 ng/mL and 0.19 to 6.04 ng/mL, respectively. The recoveries of 5 pesticides from spiked samples at 37.5-125 ng/mL ranged from 86.1 to 102.1%. The measurement of uncertainty of the GC-MS/MS method for these five pesticides was developed based on the analytical process and quantification. An analysis method that is easier and faster than the method specified in the Korean food standards codes for analyzing these five pesticides in raw material milk was developed. Moreover, the analytical method for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in bulk raw milk by GC-MS/MS was established.

• Proceedings of the Korea Contents Association Conference
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• 2015.05a
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• pp.267-268
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• 2015

카카오에 함유되어 있는 향기성분을 열탈착 가스크로마토 질량분석기(TD GC/MS)를 이용하여 실시하였다. 그 결과 hydrocarbone류 10종, alcohol류 3종, aldehyde류 7종, ketone류 3종 및 carboxylic acid류 4종 등 총 27종의 향기성분이 동정되었다. 그 중에서 carboxylic acid류의 향기성분이 55.88%로 가장 많이 함유되어 있었다. 그 다음으로 알데히드류가 13.80%, 케톤 화합물이 11.90% 그리고 모노테르펜 화합물이 11.7% 함유되어 있음을 확인하였다.

• 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 Conservation Science
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• v.32 no.1
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• pp.21-32
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• 2016

Animal glue is a traditional material used extensively as adhesive and binder in mother-of-pearl, wooden structure, traditional painting, etc. Analysis of animal glue is usually performed with IR(infrared spectroscopy) based on the IR absorption of functional group. But, it has a limitation in confirming animal glue when a sample consists of several materials because of overlapping of the absorption band. Py/GC/MS(pyrolysis/gas chromatography/mass spectrometry) is a useful tool in analyzing the constituent of polymeric materials like animal glue by identifying their pyrolysate with very small amount of sample. In this study, confirmation of animal glue in a Dancheong sample was tried with this method. Characteristic pyrolytic compounds of animal glue and tung oil used in Dancheong were identified. Dancheong sample painted with Noerok as a coloring material, animal glue and tung oil was prepared and it was possible to find characteristic peaks of animal glue after thermal degradation and artificial weathering experiment. From this, we found that animal glue can be detected using py/GC/MS in cultural heritage samples consisting of several materials and in different condition. IR was also tried to analyze Dancheong sample and the results were compared with those of py/GC/MS for the detection of animal glue.

• The Korean Journal of Pesticide Science
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• v.9 no.4
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• pp.292-302
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• 2005

Condition of Ion-Trap gas chromatography-mass spectrometry (GC-MS) for rapid screening of 206-pesticides residues in agricultural foodstuffs was optimized. As applying a wide-bore column (10 m${\times}$0.53 mm, DF 0.25 um) connected with a fused silica restrictor (0.6 m${\times}$0.1 mm), a significant retention time reduction was obtained. Additionally, the shape of peaks was sharper and higher than classical GC's and GC-MS's, which allowed lower detection limits. To easily manage many spectral data, both of Electron Ionization(EI) and Chemical Ionization(CI) techniques were adopted in screening procedure. At the following steps, MS-MS technique were used to confirm screened analytes in complicated matrices.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.11 no.3
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• pp.206-211
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• 2001

This article describes identification and quantification of benzene in the casting process. Air samples around the casting process were taken by using personal air sampler attached charcoal tube and desorbed by carbon disulfide. The identification and quantitative analysis of benzene have been performed by GC-MS and GC-FID. Calibration range of standard solutions for benzene was prepared in range from 0.1 to 2 times of TLVs concentrations($1.4{\sim}28{\mu}g/1m{\ell}$ CS2) and the limit of detection was $0.11{\pm}0.002{\mu}g/1m{\ell}$ CS2. Benzene detected in airborne was ranged in 4.0ppb~104.7ppb.

• Analytical Science and Technology
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• v.19 no.1
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• pp.107-114
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• 2006

Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

• Korean Journal of Food Science and Technology
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• v.35 no.4
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• pp.648-652
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• 2003

Precise and rapid method out for distinguishing blended sesame oils through the electronic nose analysis was developed. Sesame oil was blended with corn oil at the ratio of 95 : 5, 90: 10, and 80 : 20 (w/w), respectively. Samples were then analyzed by gas chromatography, SPME-GC/MS, and the electronic nose composed of 12 different metal oxide sensors. Sensitivities $(delta\;R_{gas}/R_{air})$ of sensors from electronic nose were analyzed by principal component analysis (PCA). Proportion of the first principal component was 98.76%.

• 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.

• Analytical Science and Technology
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• v.33 no.1
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• pp.23-32
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• 2020

Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.