• Title/Summary/Keyword: Gas Chromatography/mass spectrometry

Search Result 983, Processing Time 0.028 seconds

Analysis of Methamphetamine and Amphetamine in Oral Fluid of Eleven Drug Abusers (마약남용자 11명의 타액 중 메스암페타민의 분석)

  • Kim, Eun-Mi;Lee, Ju-Seon;Choi, Hye-Young;Choi, Hwa-Kyung;Chung, Hee-Sun
    • YAKHAK HOEJI
    • /
    • v.52 no.6
    • /
    • pp.419-425
    • /
    • 2008
  • A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

Comparative analysis of the transcriptomes and primary metabolite profiles of adventitious roots of five Panax ginseng cultivars

  • Lee, Yun Sun;Park, Hyun-Seung;Lee, Dong-Kyu;Jayakodi, Murukarthick;Kim, Nam-Hoon;Lee, Sang-Choon;Kundu, Atreyee;Lee, Dong-Yup;Kim, Young Chang;In, Jun Gyo;Kwon, Sung Won;Yang, Tae-Jin
    • Journal of Ginseng Research
    • /
    • v.41 no.1
    • /
    • pp.60-68
    • /
    • 2017
  • Background: Various Panax ginseng cultivars exhibit a range of diversity for morphological and physiological traits. However, there are few studies on diversity of metabolic profiles and genetic background to understand the complex metabolic pathway in ginseng. Methods: To understand the complex metabolic pathway and related genes in ginseng, we tried to conduct integrated analysis of primary metabolite profiles and related gene expression using five ginseng cultivars showing different morphology. We investigated primary metabolite profiles via gas chromatography-mass spectrometry (GC-MS) and analyzed transcriptomes by Illumina sequencing using adventitious roots grown under the same conditions to elucidate the differences in metabolism underlying such genetic diversity. Results: GC-MS analysis revealed that primary metabolite profiling allowed us to classify the five cultivars into three independent groups and the grouping was also explained by eight major primary metabolites as biomarkers. We selected three cultivars (Chunpoong, Cheongsun, and Sunhyang) to represent each group and analyzed their transcriptomes. We inspected 100 unigenes involved in seven primary metabolite biosynthesis pathways and found that 21 unigenes encoding 15 enzymes were differentially expressed among the three cultivars. Integrated analysis of transcriptomes and metabolomes revealed that the ginseng cultivars differ in primary metabolites as well as in the putative genes involved in the complex process of primary metabolic pathways. Conclusion: Our data derived from this integrated analysis provide insights into the underlying complexity of genes and metabolites that co-regulate flux through these pathways in ginseng.

Identification of volatile flavor compounds in Jeju citrus fruits (제주감귤류의 휘발성 향기성분의 확인)

  • Hong, Young Shin;Kim, Kyong Su
    • Food Science and Preservation
    • /
    • v.23 no.7
    • /
    • pp.977-988
    • /
    • 2016
  • The volatile flavor compounds in five Jeju citrus fruit varieties (Cheonhyehyang, Hallabong, Jinjihyang, Hwanggeum hyang and Redhyang) were extracted by simultaneous distillation-extraction (SDE) using solvent mixture of n-pentane and diethyl ether (1:1, v/v) and analyzed by using gas chromatography-mass spectrometry (GC-MS). The number of aroma compounds were identified with : 104 (4,939.77 mg/kg) in Cheonhyehyang, 98 (3,286.38 mg/kg) in Hallabong, 105 (3,317.56 mg/kg) in Jinjihyang, 102 (4,293.39 mg/kg) in Hwanggeumhyang, and 108 (4,049.94 mg/kg) in Redhyang. The detected main volatile compounds were; limonene, sabinene, ${\beta}$-myrcene, ${\alpha}$-pinene, ${\beta}$-pinene, linalool, 4-terpineol, ${\alpha}$-terpineol, (E)-${\beta}$-ocimene and ${\gamma}$-terpinene. Among the identified volatiles compounds, ethyl-benzene, nonanol, 1-p-menthen-9-al, (E)-isocarveol, methyl salicylate, ${\alpha}$-terpinen-7-al, perilla alcohol, and ethyl-dodecanoate were detected in Cheonhyehyang. only Furthermore, ${\beta}$-chamigrene and ${\alpha}$-selinene were in Hallabong only; 3-hydroxybutanal, (E)-2-nonenal, isoborneol, octyl acetate, (E)-2-undecenal, ${\beta}$-ylangene and guaia-6,9-diene in Jinjihyang. ${\rho}$-Cymenene, ${\beta}$-thujone, selina-4,11-diene and (E,E)-2,6-farnesol in Hwanggeumhyang only; and ${\rho}$-cymen-8-ol, bornyl acetate, carvacrol, bicycloelemene, ${\alpha}$-cubebene and 7-epi-${\alpha}$-selinene in Redhyang only. This study confirmed the differences in composition and content of volatile aroma components in five varieties of Jeju citrus fruits.

Method Development and Validation of Strychnine in Blood by Gas Chromatography/Mass Spectrometry Using Solid Phase Extraction and its Application in Real Specimens (SPE 및 GC/MS에 의한 혈액중 스트리크닌의 분석법 개발 및 검출사례)

  • Rhee, Jongsook;Yum, Hyesun;Moon, Sungmin;Lee, Sangki
    • YAKHAK HOEJI
    • /
    • v.57 no.2
    • /
    • pp.87-94
    • /
    • 2013
  • An analytical methodology based on solid-space extraction (SPE) with with Bond Elut Certify cartridge (Varian, 130 mg) has been developed for the qualification and quantitation of strychnine in blood. After the elution layer was evaporated, the residue was reconstituted with methanol for GC/MS. Internal standard was used 10 mg/l dextromethorphan. Strychnine is a potent central nervous stimulant and convulsant, and an alkaloid found in seeds of Strychnos nux-vomica. It was used therapeutically to improve circulation and muscle tone in oral or intramuscular doses of 0.05~8 mg. The fatal dose of strychnine for humans is 50~100 mg. A man was found dead lying curled up the corner of the large room in a roof house after the fire fighter opened a locked door inside to put out the fire. The postmortem blood and gastric contents were analyzed for toxicological testing. Strychnine and brucine were detected using GC/MS first in gastric contents extracts. The contents of strychnine was 0.083 mg/l in heart blood, 0.088 mg/l in peripheral blood and 4.0 mg/kg in gastric contents, respectively. Method validation was carried out in terms of linearity, accuracy, precision (intraday, interday) in blood. The assay is linear over 0.05~10 mg/l ($r^2$=0.999). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.02 mg/l (S/N=3) and 0.07 mg/l (S/N=10), respectively. Accuracy (bias%) of strychnine with 0.1, 1 and 10 mg/l was 12.0% (n=6), 9.3% (n=6) and 6.9% (n=6), respectively. Intraday precision (CV%) of strychnine with, 0.1, 1 and 10 mg/l were 6.4%, 10.4%, 1.2% (n=6), respectively. Interday precision (CV%) of strychnine with 0.1, 1 and 10 mg/l over three days were 24.0%, 18.5%, 13.8% (n=18), respectively. Relative recovery with 0.1, 1 and 10 mg/l (in blood) were 114.9%, 99.3% and 87.4% (n=6), respectively. The described method can be applied in forensic toxicology to determine strychnine in blood samples.

Effects of Riboflavin-photosensitized Oxidation on the Formation of Volatile Compounds in Oleic Acid Model Systems (리보플라빈 광산화에 의한 올레산 모델시스템에서 휘발성 물질 발생연구)

  • Yang, Seung-Ok;Chang, Pahn-Shick;Lee, Jae-Hwan
    • Korean Journal of Food Science and Technology
    • /
    • v.37 no.5
    • /
    • pp.717-722
    • /
    • 2005
  • Formation mechanisms of light-induced volatile compounds were studied using riboflavin-photosensitized oleic acid model systems. Volatile compounds in model systems with 4000 ppm riboflavin at $35^{\circ}C$ under light or in the dark for 39 hr were isolated and identified by a combination of solid phase microextraction (SPME), gas chromatography (GC), and mass spectrometry (MS). Total volatiles in oleic acid with riboflavin under light for 13, 26, and 39 hr increased by 90, 190, and 270%, respectively, compared to those in oleic acid without riboflavin under light. Total volatiles in samples without riboflavin under light or samples with riboflavin in the dark were not significant in tested conditions (p>10.05). Riboflavin did not act as a photosensitizer when it was dispersed in oleic acid. Heptane, octane, heptanal, octanal, nonanal, and 2-nonenal were significantly increased in riboflavin-photosensitized samples compared to those in samples without riboflavin (p<0,05). Light-induced volatile compounds including heptanal and 2-nonenal from oleic acid could be explained using singlet oxygen oxidation, the formation mechanism of which were not understood using triplet oxygen oxidation. These results will help to understand volatile formation in oleic acid containing foods stored under light.

Volatile Components of Flower and Seed of Safflower (홍화꽃 및 홍화씨의 휘발성성분)

  • Choi, Sung-Hee;Im, Sung-Im;Jang, Eun-Young;Cho, Young-Su
    • Korean Journal of Food Science and Technology
    • /
    • v.36 no.2
    • /
    • pp.196-201
    • /
    • 2004
  • Volatile components in flower and seed of safflower were identified. Volatile flavor compounds of safflower (Carthamus tinctorius L.) was extracted by simultaneous steam distillation and extraction method using Likens and Nickerson's extraction apparatus. Concentrated extract was analyzed and identified by gas chromatography and GC-mass spectrometry. Main volatile components in flower were terpene compounds, including p-cymene, limonene, ${\alpha}-phellandrene$, ${\gamma}-terpinene$, camphor, 4-terpineol, selinene, ${\beta}-caryophyllene$, torreyol, ${\beta}-eudesmol$, and 10 acids including 3-methylbutanoic acid, 2-methylbutanoic acid, and acids of $C_{2},\;C_{5}-C_{11}$. Main volatile components in seed and safflower were 20 aldehydes including hexanal (7.17%), (E)-2-heptenal (1.10%), (E,Z)-2,4-decadienal and (E,E)-2,4-decadienal.

Studies on the Effect of Low Winter Temperatures and Harvest Times on the Volatile Aroma Compounds in Green Teas (동절기 저온현상과 채엽시기에 따른 녹차의 향기성분에 대한 연구)

  • Ryu, Kyung-Heon;Lee, Hye-Jin;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
    • /
    • v.44 no.4
    • /
    • pp.383-389
    • /
    • 2012
  • Green tea leaves grown in Jeju island were harvested at different times in 2010 and 2011. Green teas harvested in 2010 experienced higher effective accumulative temperature than green teas harvested in 2011. The free and bound volatile compounds in green tea were analyzed using headspace-solid phase microextraction gas chromatography (GC) and GC-mass spectrometry. All green teas contained the 6 major volatile compounds ${\alpha}$-methylbutanal, pentanal, (E)-2-hexen-1-ol, ${\beta}$-linalool, geraniol and ${\alpha}$-farnesene. After enzyme treatment, (Z)-3-hexen-1-ol, benzaldehyde, (Z)-3-hexenyl acetate, ${\beta}$-linalool and geraniol were increased in all green teas. (Z)-3-hexen-1-ol increased significantly in green tea harvested in 2010, and benzaldehyde increased widely in green tea harvested in 2011. However, the total volatile compounds in green teas harvested in 2011 were remarkably decreased in comparison to harvested in 2010. It was confirmed that free and bound volatile compounds in green tea are affected by low winter temperatures.

Low-Temperature Microencapsulation of Sesame Oil Using Fluidized Bed Granulation (Fluidized bed granulation을 이용한 참기름의 저온 미세캡슐화)

  • Jeong, Chan-Min;Lee, Min-Kyung;Lee, Hyun-Ah;Park, Ji-Yong
    • Korean Journal of Food Science and Technology
    • /
    • v.41 no.1
    • /
    • pp.27-31
    • /
    • 2009
  • Top spray-drying method is frequently utilized for flavor encapsulation, but the top spray-dried products frequently suffer from high losses of volatile flavor as the result of a high processing temperature (150-$300^{\circ}C$). In an effort to solve these problems, a low-temperature fluidized-bed granulating method was utilized to encapsulate the flavor. For the encapsulation of sesame oil, oil-in-water emulsions of sesame oil and a mixture of maltodextrin, modified starch, gum arabic, and gellan gum were bottom-sprayed at milder temperatures (70-$100^{\circ}C$) using a fluidized-bed granulator. Sesame oil extracts from microcapsules were obtained via a simultaneous distillation/extraction technique, and the retention of volatile flavor compounds was analyzed via a gas chromatography-mass spectrometry. The retention of volatile flavors of sesame oil per se, spray-dried and fluidized-bed granulated microcapsules after 3-day-storage at $37^{\circ}C$ were 0.8%, 37.2%, and 42.0%, respectively. In addition, the low-temperature fluidized-bed granulation showed higher encapsulation yield and sensory preferences for the application of commercial products (beef rice porridge), as compared to spray drying.

Antifungal and Insecticidal Activity of Essential Oil from Asarum sieboldii against Wood Contaminant Fungi and Lasioderma serricorne L. (세신 정유추출물의 목재부후균과 궐련벌레에 대한 항진균 및 살충활성)

  • Kang, Soyeong;Chung, Yong Jae;Lim, Jin A
    • Journal of Conservation Science
    • /
    • v.28 no.4
    • /
    • pp.395-401
    • /
    • 2012
  • To investigate bioactive materials for development of natural conservative agent on organic cultural heritage, essential oil from Asarum sieboldii was screened for antifungal and insecticidal activity against 4 wood rotting fungi and adult of Lasioderma serricorne. Antifungal activity of essential oil was tested by using paper disc soaking method. Antifungal activity expressed as $IC_{50}$ value showed $1.50{\sim}2.84{\mu}l/disc$ range and the most significant antifungal activity was observed in Lentinus lepideus. The insecticidal activity of essential oil was examined by topical application method against L. serricorne adults. 50% and 100% of essential oil gave 98.3% and 100% mortality for 24 hours, respectively. The major components of the essential oil were methyl eugenol (56.32%), eucarvone (11.53%), safrole (5.79%), ${\delta}$-3-carene (2.09%), which were identified by gas chromatography-mass spectrometry. From these results, essential oil from A. sieboldii could be useful for conservation of organic cultural heritage against biological deterioration by insect and wood rotting fungi.

The Concentrations and TEQ Levels of PCDFs and PCDDs in Human Adipose Tissue and First Breast Milk of Korean (체지방 조직 및 초유중에 잔류되어 있는 다이옥신 함유도에 관한 연구)

  • Kim, Yunje;Lee, Sun Young;Han, Soon Young;Park, Kui Lea;Kil, Kwang Sup;Yang, Kyu Hwan;Kim, Eun Kyung;Kim, Myungsoo
    • Analytical Science and Technology
    • /
    • v.14 no.6
    • /
    • pp.504-509
    • /
    • 2001
  • The concentrations and TEQ levels of PCDFs/PCDDs in human aipose tissue and first breast milk were analyzed by high resolution gas chromatography/high resolution mass spectrometry. The human adipose tissue samples measured in this study have been collected at hospital in Seoul. The total concentration and TEQ level of PCDFs were showed 5.812 pg/g and 1.485 pgTEQ/g. The total concentration and TEQ level of PCDDs were showed 26.648 pg/g and 1.176 pgTEQ/g, respectively. This paper also reported dioxin levels in 20 breast milks of Korean mothers from hospital in Seoul National University. Total concentration and TEQ levels of PCDFs were showed 7.019 pg/mL and 0.177 pgTEQ/mL, respectively. Total concentrations and TEQ levels of PCDDs were showed 14.224 pg/mL and 0.693 pgTEQ/mL, respectively. According to the contribution of dioxin congeners in samples, PCDDs was higher than PCDFs. And OCDD had the highest concentration.

  • PDF