• Title/Summary/Keyword: GC/MS spectrometry

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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
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    • v.57 no.2
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    • pp.87-94
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    • 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.

Growth promotion and root development of Nicotiana tabacum L. by plant growth promoting fungi (PGPF) (식물 생장 촉진 진균에 의한 담배의 생장 촉진과 뿌리 발달)

  • Hong, Eunhye;Lee, Jinok;Kim, Sujung;Nie, Hualin;Kim, Young-Nam;Kim, Jiseong;Kim, Sunhyung
    • Journal of Plant Biotechnology
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    • v.47 no.4
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    • pp.337-344
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    • 2020
  • Plant growth-promoting microorganisms promote plant growth by supplying nutrients to roots and interacting with the intrinsic factors in plants through volatile organic compounds (VOCs). In this study, we evaluated the effect of UOS, plant growth-promoting fungi (PGPF) isolated from previous study, on the growth of Nicotiana tabacum L. var Xanthi nc. Phylogenetic analysis and GC-MS were used to identify the fungal species and the VOCs emitted by the UOS, respectively. The fresh weight of UOS-treated Nicotiana tabacum L. was 3.8 and 4.2-fold higher than that of the control groups grown in vertical and I-plates, respectively. Moreover, in the UOS-treated plants, the length of the primary root was half and the number of lateral roots were twice compared to those in control plants. The UOS was identified as Phoma sp. by studying spore and mycelial morphology and using phylogenetic analysis. GC-MS revealed that the VOC emitted by the UOS was hexamethylcyclotrisiloxane (D3). These results suggest that the UOS of Phoma sp. influences plant growth and root development through D3. We expect this UOS and its VOC, D3 to be utilized in the future to increase growth and enhance yield for other plants.

Determination of Capsaicin and Dihydrocapsaicin in Various Species of Red Peppers and Their Powdered Products in Market by GC-MS Analysis (GC-MS 분석에 의한 고추 품종별 및 시판고춧가루의 capsaicin 및 dihydrocapsaicin 함량조사)

  • Yu, Jong-Ok;Choi, Won-Seok;Lee, Ung-Soo
    • Food Engineering Progress
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    • v.13 no.1
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    • pp.38-43
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    • 2009
  • In this research, the contents of capsaicin and dihydrocapsaicin in various species of red pepper produced in the Goesan-gun County were determined by GC-MS. Further, the contents of capsaicin and dihydrocapsaicin in powdered red pepper products with very hot, hot, normal and mild taste were analyzed to present the degree of hot taste in their products based on contents of capsaicin. The contents of capsaicin in each species of red pepper were from 25.18 mg%(Daetong) to 123.62 mg%(Cheongyang). In the powdered red pepper sold in the market, the contents (mg%) of capsaicin in very hot, hot, normal and mild taste products were 101.98, 67.63, 37.74, and 14.73, respectively. Based on this result, the classification of hot taste by contents of capsaicin was presented in the 7 grades. Namely, the products currently sold in the market were classified into very hot, hot, normal and mild taste. In this research, the degree of hot taste was classified based on contents of capsaicin into 1st grade over 120 mg%, 2nd grade in 100-120 mg%, 3rd grade in 80-100 mg%, 4th grade in 60-80 mg%, 5th grade in 40-60 mg%, 6th grade in 20-40 mg% and 7th grade below 20 mg%. Thus, it is expected that the problem which arises when preparing the products such as kimchi, gochujang and seasoning sauces by using powdered red pepper, namely, the inconsistency of hot taste can be improved and maintained.

Studies on Potato Glycoalkaloid Determination by Acid-hydrolysis Method (산 가수분해 방법에 의한 감자 glycoalkaloid성분의 정량성 검토)

  • Yoon, Kyung-Soon;Byun, Gwang-In
    • Journal of the Korean Society of Food Culture
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    • v.24 no.1
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    • pp.84-89
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    • 2009
  • This paper was conducted to evaluate aglycones and carbohydrates produced by acid hydrolysis of three potato glycoalkaloids [(PGA); ${\alpha}$-chaconine, ${\alpha}$-solanine, and demissine] in potatoes. Standard solanidine and demissidine were dissolved in 1N HCl and then heated at $100^{\circ}C$ for 10-120 min. Solanidine was rapidly decomposed during acid hydrolysis and one peak that was identified as solantherene ($M^+$=379) by GC-MS was detected. The transformation solanidine to solanthrene was approximately 50% complete after 10 min, approximately 90% complete after 60 min and 100% complete after 120 min. Demissidine was hydrolyzed using the same method that was used to hydrolyze the solanidine. However, demissidine produced only one peak upon GC-MS ($M^+$=399) analysis and was found to be very stable at increased temperatures. Acidy hydrolysis of ${\alpha}$-chaconine, ${\alpha}$-solanine and demissine resulted in the decomposition of ${\alpha}$-chaconine and ${\alpha}$-solanine to solanidine and solanthrene, respectively. Therefore, this hydrolysis method should not be utilized to produce PGA combining with solanidine as aglycone. The individual carbohydrates produced by the two PGAs by hydrolysis were very stable at increased temperatures; therefore, it was possible to quantify these PGAs based on calculation of the individual carbohydrate content. Conversely, because demissidine produced by the hydrolysis of demissine was extremely stable at increased temperatures, it was possible to quantify the PGA based on the aglycone produced by hydrolysis.

The measurement of dicamba in soil and plants (토양 및 식물 중 디캄바 측정법에 대한 연구)

  • Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.480-487
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    • 2009
  • The herbicide dicamba (2-methoxy-3,6-dichlorobenzoic acid) in soil and plants was determined by gas chromatography-mass spectrometry (GC/MS). The samples were extracted with diethyl ether at pH 2, and washed with 0.1 N HCl, and then dried. The dried residue was derivatized in 1 mL of 10% $H_2SO_4$-MeOH for 2 hr at $80^{\circ}C$. The reaction mixture was neutralized with 4 mL of sodium bicarbonate solution and reextracted with 5 mL of diethyl ether. After the extract was concentrated, dicamba was determined by GC/MS-SIM mode. There was good linearity above 0.999 in the ranges of the $1.0{\sim}100{\mu}g/kg$. Total 42 sample including 32 soil samples and 10 plants samples were analyzed by developed method. Dicamba was detected in the concentration range of $2.9-123.9{\mu}g/kg$ in 15 samples among 32 soil samples and in the concentration range of $43-33,252{\mu}g/kg$ in 5 samples among 10 plants samples. A cause of the wither and die of the pine trees is suspected to spray dicamba around or directly to them.

Analysis of Mineral and Volatile Flavor Compounds in Pimpinella brachycarpa N. by ICP-AES and SDE, HS-SPME-GC/MS (ICP-AES와 SDE, HS-SPME-GC/MS를 이용한 참나물의 무기성분과 향기성분)

  • Chang, Kyung-Mi;Chung, Mi-Sook;Kim, Mi-Kyung;Kim, Gun-Hee
    • Journal of the Korean Society of Food Culture
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    • v.22 no.2
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    • pp.246-253
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    • 2007
  • Mineral and volatile flavor compounds of Pimpinella brochycarpa N., a perennial Korean medicinal plant of the Umbelliferae family, were analyzed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and simultaneous steam distillation extract (SDE)-gas chromatography mass spectrometry (GC/MS), head space solid phase micro-extraction (HS-SPME)-GC/MS. Mineral contents of the stalks and leaves were compared and the flavor patterns of the fresh and the shady air-dried samples were obtained by the electronic nose (EN) with 6 metal oxide sensors. Principal component analysis (PCA) was carried out using the data obtained from EN. The 1st principal values of the fresh samples have + values and the shady air-dried have - values. The essential oil extracted from the fresh and the shady air-dried by SDE method contain 58 and 31 flavor compounds. When HS-SPME method with CAR/PDMS fiber and PDMS fiber were used, 34 and 21 flavor compounds. The principal volatile components of Pimpinella brachycarpa N. were ${\alpha}$-selinene, germacrene D, and myrcene.

The review on standard method of microplastics in soil and groundwater (토양, 지하수 중 미세플라스틱 분석법에 관한 고찰)

  • JongBeom Kwon;Hyeonhee Choi;Sunhwa Park
    • Analytical Science and Technology
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    • v.37 no.3
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    • pp.174-188
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    • 2024
  • This review summarized research trends regarding sample collection methods, pretreatment method, and types of analysis devices for microplastics (MPs) in soil and groundwater matrices. Soil sampling considers the selection of sampling location, depth, and volume. The typically sampling depth is within 15 cm (topsoil), and about 1 kg of mixed each sample. Among spot sampling and continuous flow sampling, groundwater sampling mainly used a continuous flow sampling, with collection rates 2 to 6 L/min in the range of 300~1,000 L, and followed by immediate on-situ filtration. Pretreatment method, applied to soil and groundwater, consist of organic digestion and density separation. In the organic digestion method, H2O2 is recommended among H2O2, acidic, alkaline, and enzymatic method. NaCl is primarily used as a reagent in density separation. However, depending on the density of MPs, other regents can be selectively used like ZnCl2, ZnBr2, and etc. Representative analysis device includes Fourier Transform Infrared (FTIR) and Raman spectroscopy for non-destructive analysis and Pyrolysis Gas Chromatography Mass Spectrometry (Py-GC/MS) for destructive analysis. µ-FTIR and Raman can count MPs of larger than 10 and 1 ㎛, and analyze MPs materials. However, it is need to sufficiently remove interference, like organic matter, in spectroscopic analysis using essential pretreatment method. Py-GC/MS is being continuously researched because it doesn't require complex pretreatment method and allows quantitative analysis of specific materials.

Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Lee, Jeong-Min;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Geon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.2
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    • pp.117-124
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    • 2008
  • A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

Changes of Flavor Compounds in Persimmon Leaves(Diospyros kaki folium) during Growth (감잎의 성장시기별 향기성분의 변화)

  • 김종국;강우원;김귀영;문혜경
    • Journal of the East Asian Society of Dietary Life
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    • v.11 no.6
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    • pp.472-478
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    • 2001
  • This study was conducted to investigate the change in volatile flavor components of persimmon leaves during growth. The flavor components of persimmon leaves were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry(GC/MS). The flavor compounds were collected by simultaneous steam distillation and extraction(SDE) method, and were separated and identified resulting in 126 components, including 23 alcohols, 18 aldehydes, 4 esters. 15 acids, 37 hydrocarbons, 14 ketones, 6 phenols. and 9 others in persimmon leaves. The most abundant components of persimmon leaf were alcohols including iinalool. cis-3-hexanal. 1-$\alpha$ -terpineol. 3.7.11.15-tetramethyl-2-hexadecen-1-ol and aldehydes including trans-2-hexanal. nonanal, 2-decenal and hydrocarbons including 1.1-dimethylethyl cyclohexane, 1-methyl-4-(2-methylpropyl) -benzene. During growth, many other components were formed and dissipated after the 20th of June.

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Analysis of fatty acid methyl ester in bio-liquid by hollow fiber-liquid phase microextraction

  • Choi, Minseon;Lee, Soyoung;Bae, Sunyoung
    • Analytical Science and Technology
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    • v.30 no.4
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    • pp.174-181
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    • 2017
  • Bio-liquid is a liquid by-product of the hydrothermal carbonization (HTC) reaction, converting wet biomass into solid hydrochar, bio-liquid, and bio-gas. Since bio-liquid contains various compounds, it requires efficient sampling method to extract the target compounds from bio-liquid. In this research, fatty acid methyl ester (FAME) in bio-liquid was extracted based on hollow fiber supported liquid phase microextraction (HF-LPME) and determined by Gas Chromatography-Flame Ionization Detector (GC-FID) and Gas Chromatography/Mass Spectrometry (GC/MS). The well-known major components of biodiesel, including methyl myristate, palmitate, methyl palmitoleate, methyl stearate, methyl oleate, and methyl linoleate had been selected as standard materials for FAME analysis using HF-LPME. Physicochemical properties of bio-liquid was measured that the acidity was 3.30 (${\pm}0.01$) and the moisture content was 100.84 (${\pm}3.02$)%. The optimization of HF-LPME method had been investigated by varying the experimental parameters such as extraction solvent, extraction time, stirring speed, and the length of HF at the fixed concentration of NaCl salt. As a result, optimal conditions of HF-LPME for FAMEs were; n-octanol for extraction solvent, 30 min for extraction time, 1200 rpm for stirring speed, 20 mm for the HF length, and 0.5 w/v% for the concentration of NaCl. Validation of HF-LPME was performed with limit of detection (LOD), limit of quantitation (LOQ), dynamic range, reproducibility, and recovery. The results obtained from this study indicated that HF-LPME was suitable for the preconcentration method and the quantitative analysis to characterize FAMEs in bio-liquid generated from food waste via HTC reaction.