• Journal of the Korea Academia-Industrial cooperation Society
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• v.16 no.12
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• pp.8836-8843
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• 2015

This study was performed to investigate the antiproliferative activities of supercritical extracts from phalsak(Citrus hassaku Hort ex Tanaka) and yeagam(Citrus iyo Hort. ex Tanaka) against human cervical carcinoma HeLa cells and the chemical compositions of the extracts. The anticancer properties of supercritical extracts were demonstrated using the MTT assay and Hoechst 33342 staining and the compositional analyses were conducted by using gas chromatography-mass spectrometry(GC-MS). The peel extracts of both species exhibited similar antiproliferative effect. The antiproliferative activity of the flesh extracts was not detected up to $400{\mu}g/mL$, whereas peel extracts of phalsak and yeagam reduced cell viability with 87.16% and 92.95% at $400{\mu}g/mL$, respectively. There was a dramatic increase of the apoptotic body formation in the cell treated with peel extracts while no apoptotic body formation detected in the cell treated with flesh extracts at 100, $200{\mu}g/mL$. By GC-MS analysis, 27 and 31 kinds of compounds identified in flesh and peel of phalsak, while 27 and 29 kinds of compounds were identified in flesh and peel of yeagam, respectively. 1,1,4,4-Tetramethyl-2-tetralone(20.86%), alloimperatorin(8.15%), limonene(11.23%), and auraptene(7.29%) were major in peel of phalsak, whereas limonene(22.19%), linalool(11.23%), and ${\gamma}$-sitosterol(9.12%) were major in peel of yeagam.

• Applied Biological Chemistry
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• v.51 no.3
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• pp.238-244
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• 2008

The essential oil was obtained from the aerial part of Caryopteris incana Miq. by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GCMS). The fragrance of the essential oil was fougere and woody. There were sixty-nine constituents in the essential oil: 28 carbohydrates, 22 alcohols, 7 acetates, 7 ketones, 3 aldehydes, and 2 others. Major constituents were 4,6,6-trimethyl [1S-($1{\alpha},2{\beta},5{\alpha}$)]-bicyclo[3.1.1]hept-3-en-2-ol (11.8%), taucadinol (9.4%), myrtenyl acetate (9.2%), pinocarvone (7.0%), 1-hydroxy-1,7-dimethyl-4-isopropyl-2,7-cyclodecadiene (6.3%), ${\delta}$-3-carene (6.2%). By SPME extraction, forty-nine constituents were identified: 22 hydrocarbons, 16 alcohols, 6 acetates, 3 ketones, and 2 ethers. Major constituents of the SPME-extracted sample were ${\delta}$-3-carene (12.6%), (-)-myrtenyl acetate (11.2%), 6,6-dimethyl-2-methylene-bicycol [3.1.1] heptan-3-o1 (10.9%), pinocarvone (9.3%). By HS extraction, ten constituents were identified: 5 hydrocarbons, 2 amines, 1 alcohol, and 2 others. Major constituents of the HS-extracted sample were (Z)-2-fluoro-2-butene (34.9%), ${\delta}$-3-carene (6.9%), 6-(4-chlorophenul)tetrahydro-2-methyl-2H-1,2-oxazine (5.9%). The $IC_{50}$ value (0.011 ${\mu}g/mg$) in MTT assay using HaCaT keratinocyte cell line was lower than those of commercially-selling rosemary and tea tree, suggesting more toxicological studies are needed for commercial use of the essential oil of Caryopteris incana Miq.

• Korean Journal of Clinical Laboratory Science
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• v.50 no.1
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• pp.37-43
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• 2018

Chamaecyparis obtusa (CO) has recently been attracting attention because of its beneficial effects on skin allergies, atopic dermatitis, and skin diseases, such as acne and eczema. In the present study, the extract from CO leaf grown in Jangseong gun, Jeollanam-do, Korea was evaluated for its anti-oxidant, anti-inflammatory, and anti-allergic effects in vitro. The total polyphenol content of the CO leaf extract was $25.89{\pm}0.31mg$ gallic acid equivalents (GAE)/g. Gas-chromatography mass-spectrometry (GC-MS) analysis revealed the presence of six compounds in the CO leaf extract: ${\alpha}-terpinene$ (3.03 mg/g), ${\alpha}-terpineol$ (9.48 mg/g), limonene (5.96 mg/g), borneol (59.78 mg/g), myrcene (4.85 mg/g), and sabinene (11.31 mg/g). The $RC_{50}$ values of the CO leaf extract for $H_2O_2$ and ABTS radical were $5.47{\pm}0.13mg/mL$ and $4.00{\pm}0.01mg/mL$, respectively. In addition, the CO leaf extract showed significant inhibitory effects on lipopolysaccharide-induced nitric oxide production in RAW 264.7 cells and IgE-induced release of ${\beta}-hexosaminidase$ (degranulation) in mast-cell like RBL-2H3 cells. The cell viability assay showed that the CO leaf extract ($100{\sim}800{\mu}g/mL$) did not affect the viability of human normal skin fibroblast CCD-986sk cells significantly. Overall, these results suggest that the CO leaf extract is a potential functional cosmetic ingredient that can exert anti-oxidant, anti-inflammatory, and anti-allergic effects.

• Analytical Science and Technology
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• v.28 no.5
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• pp.323-330
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• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

• Analytical Science and Technology
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• v.24 no.2
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• pp.69-77
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• 2011

Ethylene glycol (EG) is produced commercially in large amounts and is widely used as antifreeze or deicing solution for cars, boats, and aircraft. EG poisoning occurs in suicide attempts and infrequently, either intentionally through misuse or accidental as EG has a sweet taste. EG has in itself a low toxicity, but is in vivo broken down to higher toxic organic acids which are responsible for extensive cellular damage in various tissues caused principally by the metabolites glycolic acid and oxalic acid. The most conclusive analytical method of diagnosing EG poisoning is determination of EG concentration. However, victims are sometimes admitted at a late stage to hospitals or died during emergency treatment like a gastric lavage or found rotten dead, when blood EG concentrations are low or not detected. Therefore, in this study, the identification of EG was not only performed by gas chromatograpyc-mass spectrometry (GC-MS) following derivatization but also further toxicological analyses of metabolites, glycolic acid (GA) and oxalic acid (OA), were performed by ion chromatography in various biological specimens. A ranges of blood concentrations (3 cases) was $10\sim2,400\;{\mu}g/mL$ for EG, $224\sim1,164\;{\mu}g/mL$ for GA and ND $\sim40\;{\mu}g/mL$ for OA, respectively, In other biological specimens (liver, kidney, bile and pleural fluid), a range of concentrations (3 cases) was ND $\sim55,000\;{\mu}g/mL$ for EG, ND $\sim1,124\;{\mu}g/mL$ for GA and ND $\sim60\;{\mu}g/mL$ for OA, respectively. Liver and kidney tissues were recommended specimens including blood because OA, a final metabolite of EG, was identified large amounts in these despite no detectable EG caused by some therapy.

• Analytical Science and Technology
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• v.26 no.4
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• pp.268-275
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• 2013

Many kinds of liquid spray products are used in livelihood activities these days. Spray products can be distinguished by the target to be sprayed (like into the air or on human skin (body)). Because human can be exposed to volatile organic compounds (VOC) emitted from spray products, some considerations on safety or hazard of spray products should be needed. In this study, emission characteristics of VOCs were investigated against 10 types of liquid spray products (6 skin spray and 4 air spray products). The concentrations of benzene and toluene were determined by gas chromatography/mass spectrometry (GC/MS) equipped with a thermal desorber (TD). Their average concentrations from 6 skin spray products exhibited$ 5.64{\pm}1.95$ ($mean{\pm}S.D$) and $8.52{\pm}2.89$ ppb(w), respectively. In contrast, those of 4 air spray samples had $7.30{\pm}1.31$ and $7.19{\pm}1.78$ ppb(w), respectively. If liquid contents in spray samples are completely vaporized in one cubic meter (1 m3) after spraying for 10 seconds, their mean concentrations of skin spray products are $31.7{\pm}8.80$ (benzene) and $50.5{\pm}17.1{\mu}g/Sm^3$ (toluene). In contrast, those of air spray products are $24.0{\pm}4.30$ (benzene) and $23.6{\pm}5.83{\mu}g/Sm^3$ (toluene). The estimated concentration levels of benzene from two types of products (31.7 and $24.0{\mu}/Sm^3$) exceeded the Korean atmospheric environmental guideline ($5{\mu}g/Sm^3$). The results of this study thus suggest that some measures should be made to reduce or suppress the contents of VOC in spray products.

• Clinical and Experimental Reproductive Medicine
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• v.28 no.4
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• pp.279-286
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• 2001

Objective: To elucidate 1) whether there are any differences in the urine concentrations of steroid hormone metabolites between patients with leiomyoma and normal controls 2) the correlation between urinary profiles of steroid hormones and leiomyomas of the uterus according to their type, location, volume, and weight. Materials of Methods : The study population consisted of 37 premenopausal patients with uterine leiomyoma and the control group consisted of 25 premenopausal normal volunteer women without uterine leiomyoma. Confirmation of the existence of uterine leiomyoma was done by ultrasonography and histopathological examination after surgery. The volume of the leiomyoma was estimated by trans-abdominal and/or trans-vaginal ultrasonography. The Leiomyomas were divided into 3 types (subserosal, intramural and submucosal). Seventeen patients had subserosal type of leiomyoma, 10 with the intramural type and 10 with the submucosal type. The locations of the leiomyoma were also divided into 3 groups (fundus, body and isthmus). Seventeen patients showed a fundus location, 10 in body, and 10 in isthmus. We compared urinary profiles of the endogenous steroids between patients with leiomyomas and normal controls, and also investigated the relationship between urinary profiles of the endogenous steroids and leiomyomas according to their type, location, volume and weight by using highly sensitive Gas Chromatography-Mass Spectrometry (GC-MS) system. Results: The mean ages of the patients with leiomyomas and the control group were $43.1{\pm}5.6$ and $40.6{\pm}7.2$ years, the weights were $63.4{\pm}7.3$ and $59.4{\pm}8.1\;kg$, and their heights were $155.4{\pm}4.8$ and $159.3{\pm}4.8\;cm$ respectively. Seventeen patients had subserosal, 10 had intramural, and 10 had submucosal leiomyomas. There were 17 patients with leiomyoma located in fundus, 10 in body and 10 in isthmus. $17{\beta}$-estradiol, 5-AT, 11-keto ET, $11{\beta}$-hydroxy An, $11{\beta}$-hydroxy Et, THS, THA, THE, a-cortolone, a-cortol, $\beta$-cortol, $11{\beta}$-OH Et/$11{\beta}$-OH An and E2/E1 were significantly increased in patients with leiomyoma than in the control group. $17{\beta}$-estradiol was significantly increased in the intramural and the submucosal types than in the subserosal type. There was no significant difference in the concentrations of urinary steroids according to the locations of leiomyomas. There was no significant relationship between the concentration of urinary steroids and the volume of the leiomyomas. $17{\beta}$-estradiol significantly decreased as the weight of uterus increased (r=-0.322, p=0.04). Conclusion: The concentrations of steroid hormone metabolites were generally increased in patients with leiomyoma but were not significantly related to the volume and weight of the leiomyomas. Our study suggests that steroid hormones may be involved in the initiation of leiomyomas but may not be involved in their progression. In addition, the concentrations of steroid hormone metabolites are not related to the leiomyoma type and location.

• Korean Journal of Pharmacognosy
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• v.40 no.3
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• pp.196-204
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• 2009

This study was carried out to investigate the in vivo and in vitro inhibitory effect of a traditional herbal complex (HC) extract prepared from a mixture of four oriental herbs (Dioscorea Rhizoma, Glycine soja Sieb. et Zucc, Bombycis corpus, Fermented Glycine soja) that have been widely used for the treatment and prevention of diabetes mellitus on hyperglycemia. The water extract of HC showed potent inhibitory effect on $\alpha$-glucosidase with $IC_{50}$ value of 1.24 mg/mL. Additionally, the ethanol extract of HC was also found to exhibit significant inhibitory effect against protein tyrosine phosphatase $1{\beta}$ ($PTP1{\beta}$), which is known as a major regulator of both insulin and leptin signaling. In the $PTP1{\beta}$ inhibitory assay, the most active n-hexane fraction obtained from the ethanol extract of HC, was identified as a mixture of fatty acid derivatives by gas chromatography-mass spectrometry (GC-MS). In high-fat diet-low dose streptozotocin (STZ)-induced diabetic rat, the water extract of HC improved the oral glucose intolerance as compared with rosiglitazone. HC also caused a marked decrease of body weight and fasting blood glucose and a significant improvement on glucose tolerance in metabolic syndrome mice model. These findings support that this traditional HC may be useful in the control of blood glucose in diabetes mellitus and metabolic syndrome.

• Journal of Nutrition and Health
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• v.47 no.4
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• pp.221-228
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• 2014

Purpose: Citron seed oil (CSO) has been reported to have high antioxidant activity. However, the composition and other biologically activities of CSO have not been reported. In this study, we confirmed the fatty acid composition of CSO, which may be beneficial to vascular disease and obesity. Methods: We investigated the oil composition of CSO using gas chromatography coupled with mass spectrometry (GC-MS) analysis, and cytotoxicity was confirmed by Cell Counting Kit-8 (CCK-8) assay. Nitric oxide (NO) production in human umbilical vein endothelial cells (HUVECs) was measured using Griess reagent, and lipid accumulation and leptin secretion in 3T3-L1 cells were measured by Oil-Red O staining and commercial ELISA kit, respectively. Results: GC-MS analysis indicated that CSO contains several components, including linoleic acid, oleic acid, palmitic acid, stearic acid, linolenic acid, palmitoleic acid, and arachidic acid. In physiological activity analysis, CSO did not induce cytotoxic effects in HUVECs and 3T3-L1 cells. Further, CSO significantly induced nitric oxide and leptin secretion as well as inhibited lipid accumulation. Conclusion: CSO increased NO release, inhibited lipid accumulation, and induced leptin secretion, suggesting it may be useful for the management of vessels and weight gain. Although further studies are required to investigate the safety and mechanism of action of CSO, our results show that the composition and physiological activity of CSO are sufficient for its use as functional edible oil.

• Journal of the Korean Society of Food Science and Nutrition
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• v.35 no.6
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• pp.738-746
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• 2006

Aroma compounds in four different Byeolmijang made from optional ingredient addition were extracted by SDE (simultaneous steam distillation extraction) and analyzed with GC (gas chromatography) and GC/MS (mass-spectrometry). The major aroma compounds in the four different Byeolmijang during aging were 1-octene-3-ol, hexanal, benzeneacetaldehyde, benzaldehyde, fufural, pyrazine, furan and phenol type compounds. Generally, benzeneacetaldehyde, benzaldehyde, fufural and phenol type compounds were increased during aging. On the other hand, 1-octen-3-ol, hexanal and furan were decreased during aging. Furfural, 2-furanmathanol and benzeneacetaldehyde in Sanghwangjang, 3-methyl-1-butanol, phenol and 1H-indole in Mujang, hexanal, 1-octen-3-ol and 2,4-decadienal in Bizijang and hexanal, tetramethylpyrazine and 2-methoxy-4-vinylphenol in Jigeumjang were identified as major aroma compounds, respectively. Generally, the major aroma compound in four different Byeolmijang with optional ingredient was similar with control and pyrazine, furan and phenol type compounds were decreased to addition with optional ingredient. The major aroma compound in Sanghwangjang with optional ingredient (onion) were 1-hexanol and 2,5-dimethylthiophene and the major aroma compounds were 1,2,4-trithiolane and 2-buthyl-2-octenal in Mujang with optional ingredient (Letinus edodes). Furfural, benzaldehyde, benzeneacetaldehyde, 1,2,4-trithiolane and lenthionine were detected in Bizijang due to the addition of powdered Letinus edodes. Linaool and ${\beta}-lonone$ were detected in Jigeumjang due to the addition of powdered red pepper.