• Analytical Science and Technology
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• v.24 no.3
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• pp.183-192
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• 2011

This study was done for the determination and excretion profile of superdrol and its metabolites in human urine using both liquid chromatography with electrospray ionization mass spectrometry and gas chromatography with mass spectrometry after trimethylsilylation. Superdrol and its two metabolites were detected in human urine after administration of superdrol to healthy volunteers. The intra-day recovery ranged 89.7-113.2%, accuracy ranged 91.8-113.8% and reproducibility ranged 0.2-6.8% and inter-day recovery ranged 89.3-104.1%, accuracy ranged 95.2-103.0%, reproducibility ranged 0.7-7.8%. We found that superdrol M1 was a hydration at C-3 and superdrol M2 was a hydroxylation at D-ring. Superdrol and two metabolites were excreted as their glucuronided fractions. The glucuro-/sulfa-conjugated ratio of superdrol, superdrol M1 and superdrol M2 were 0.02, 0.02, 0.01, respectively. The excretion studies showed that superdrol and two metabolites were reached 4.3 h after oral administration and superdrol and superdrol M1 were detected until 48 h in human urine.

• Environmental Analysis Health and Toxicology
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• v.15 no.3
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• pp.107-113
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• 2000

Chlorophenoxy acids are one of the most useful classes of chlorinated herbicides. Specially 2, 4-D and 2, 4, 5-T were known to endocrine distruptors. In this study, these pesticides in water samples were extracted by liquid-liquid extration at acidic conditions and then derivatization of acidic group was carried out various esterifications using by CH$_3$I/Acetone -K$_2$CO$_3$, H$_2$SO$_4$/MeOH or TFAA/TFE. That result, Sensitivities of TFE derivatized 2, 4-D and 2, 4, 5-T are prior to the others. The recoveries of 2, 4-D and 2, 4, 5-T were 98% and 82% respectively using diethyl ether as an extracting solvent.

• Journal of the Korean Society of Food Science and Nutrition
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• v.26 no.2
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• pp.209-213
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• 1997

Since Houttuynia cordata is well known as a medicinal herb, due to its antibacterial activity on various microorganisms, present investigation was performed to identify the flavor compounds for volatile essential oil. Volatile essential oil was collected by simultaneous distillation-extraction(SDE), and then the oil components were separated on HP-5 capilliary column$(25m{\times}0.25mm\; i.d.)$ and identified those components by GC-MS. Fifty two compounds were isolated from the volatile essential oil of Houttuynia cordata and forty four were positively identified by GC-MS. The volatile compounds were composed mainly of terpenoids(25 classes), aldehydes(7 classes), alcohols(4 classes), ketones(3 classes), acids(1 class) and miscellaneous compounds(4 classes). Of these, the major compounds were ${\beta}-myrcene$, ${\beta}-ocimene$, decanal, 2-undecanone and geranyl propionate.

• Bulletin of the Korean Chemical Society
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• v.25 no.2
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• pp.271-279
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• 2004

The aroma component of Hallabong peel has been characterized by GC-MS with two different extraction techniques: solid-phase trapping solvent extraction (SPTE) and headspace solid-phase microextraction (HSSPME). Aroma components emitted from Hallabong peel were compared with those of other citrus varieties: lemon, orange and grapefruit by SPTE and GC-MS. d-Limonene (96.98%) in Hallabong was the main component, and relatively higher peaks of cis- ${\beta}$-ocimene, valencene and -farnesene were observed. Other volatile aromas, such as sabinene, isothujol and ${\delta}$-elemene were observed as small peaks. Also, principal components analysis was employed to distinguish citrus aromas based on their chromatographic data. For HSSPME, the fiber efficiency was evaluated by comparing the partition coefficient ($K_{gs}$Kgs) between the HS gaseous phase and HS-SPME fiber coating, and the relative concentration factors (CF) of the five characteristic compounds of the four citrus varieties. 50/30 ${\mu}$m DVB/CAR/PDMS fiber was verified as the best choice among the four fibers evaluated for all the samples.

• Mass Spectrometry Letters
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• v.14 no.2
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• pp.25-35
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• 2023

Plants are a traditional source of many chemicals used as biochemical, flavors, food, color, and pharmaceuticals in various countries, especially India. Most herbal medicines and their derivatives are often made from crude extracts containing a complex mixture of various phytochemical chemical components (secondary metabolites of the plants). This study aimed to identify bioactive compounds from the different parts of the plant from the ethanolic extract of Gymnema sylvestre, Senna auriculata, and Cissus quadrangularis (leaves, flower, stem) by gas chromatography-mass spectroscopy (GC-MS). The gas chromatography - mass spectrometry analysis revealed the presence of various compounds like 3,4-dimethylcyclohexanol, hexanoic acid, D-mannose, and N-decanoic acid. Hence, the Gymnema sylvestre, Senna auriculata, and Cissus quadrangularis may have chemopreventive, anti-cancer, anti-microbial activity, antioxidant, anti-diabetic activity, anti-inflammatory, and antifungal due to the presence of secondary metabolites in the ethanolic extract. These phytochemicals are supported for traditional use in a variety of diseases.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.312-315
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• 2014

The present study demonstrated the development and validation of the method for the quantification of phenol in food using gas chromatography coupled with mass spectrometry (GC-MS). After spiking of internal standard (Phenol-$d_5$) to food, those samples were extracted with organic solvent mixture (acetone : dichloromethane = 1 : 1, v/v) using ultra sonic extractor and cleaned by gel permeation chromatography (GPC) technique. The amount of phenol was determined by GC/MS. To validate the developed method, we evaluated parameters were the selectivity, linearity, accuracy, precision, and recovery. To demonstrate the selectivity of the method, blank samples of rice, corn, and fish(mackerel) were prepared and subjected to GC-MS analysis. To verify the linearity of the method, six different standard concentrations of phenol at 0.01, 0.05, 0.1, 0.5, 1 and 2.5 mg/kg were evaluated. The correlation coefficient ($r^2$) of calibration curve was 0.9999. The recovery rate for phenol standard calculated by internal standard method were 82.2~101.5% for samples fortified with 0.25, 0.50, and 1.0 mg/kg, respectively. Also the repeatability and reproducibility for validation of precision were 0.2~5.5%. According to the result of the validation, this established method was suitable for AOAC guideline. The limit of detection (LOD) for phenol analysis were 0.03~0.1 mg/kg, and the limit of quantification (LOQ) were 0.1~0.3 mg/kg. Therefore, we established the optimal analysis method for determination of phenol in food using GPC and GC/MS.

• Bulletin of the Korean Chemical Society
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• v.23 no.3
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• pp.488-496
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• 2002

SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba /SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv to 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air.

• Proceedings of KOSOMES biannual meeting
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• 2006.11a
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• pp.169-174
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• 2006

A distinctive difference of hydrocarbon in crude oil and petroleum products exists. Depending on the origin where it comes from, crude oil shows its own unique pattern which is different from petroleum products containing characteristics according to their operating process and production period. A process of mixing behavior in a tank containing residual amounts of oil draws its own pattern when analysis is conducted. The analytical process described above is named oil fingerprint method. This study investigates an effectiveness of the method for comparing data sets produced by conventional gas chromatography with mass spectrometer (GC/MS) and comprehensive two-dimensional gas chromatography (GC X GC) which is known as powerful new technology for chemical analysis.

• Analytical Science and Technology
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• v.36 no.5
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• pp.205-215
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• 2023

In the present study, an analytical method was proposed for detecting trifluralin in aquatic products at trace concentrations. The method employed QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) and gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) as the sample preparation and measurement, respectively. The effect of the aqueous phase volume used in the QuEChERS was demonstrated, and the ratio of 10:10 (mL) between water and acetonitrile phase was used for 5 g of sample. Besides, dSPE using C18 and primary-secondary amine (PSA) was applied to remove the potential interferences from the food matrices, indicating no remarkable analyte loss. The linear range was built up from 0.50 ㎍ L^-1 to 3.0 ㎍ L^-1 (R² = 0.9993). Other criteria, i.e., repeatability (RSD_r = 0.86-1.96 %), reproducibility (RSD_R = 1.09-2.01 %), and recovery (over 90 %), were in accordance with Appendix F of AOAC (2016) for method performance. Although no trifluralin was detected for the commercial samples (fish, shrimp, and breaded shrimp), the spiked samples performed favorable recoveries and precision.

• Korean Journal of Food Science and Technology
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• v.28 no.4
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• pp.772-778
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• 1996

In order to investigate changes of flavor during food sterilization in retortable pluches, a model food system consisting of 50% chicken breast meat, 1% salt and 49% chicken stock was analyzed before and after retorting using GC and GC-MS. In the analysis of the volatile components collected by the nitrogen purge and trap technique before and after retorting, a total of 53 peaks were observed on chromatograms and 42 peaks were identified. Among the 42 peaks identified were 17 caused by aldehydes, 9 by hydrocarbons, 8 by alcohols, 6 by ketones, 1 by furan and 1 by terpene. Analysis of the data obtained from our model food system strongly suggested that the compounds responsible for retort flavor are 2-heptanone, 2-pentyl furan and various ketones.