• Title/Summary/Keyword: quantitative GC analysis

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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 and Conservation of Historic Textiles - Theory and Practice - (섬유 문화재의 분석과 보존처리 - 이론과 실제 -)

  • Oh, Joon-Suk
    • Journal of the Korean Society of Costume
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    • v.58 no.5
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    • pp.211-231
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    • 2008
  • To conserve historic textiles, analyses of textile materials, pollutants and deterioration are prerequisite steps. Based upon analytical results, guides for conservation of historic textiles are established. In analyses of textile materials, pollutants and deterioration, there are chemical methods(burning, solubility and staining), physical methods(microscopy and density) and instrumental analysis(Fourier Transform Infrared Spectroscopy (FT-IR), Fourier Transform Raman Spectroscopy(FT-Raman), Gas Chromatography(GC), Mass Spectroscopy(MS), X-Ray Fluorescence (EDXRF, WDXRF), Energy Dispersive Spectroscopy(EDS), and X-Ray Diffraction(XRD), Tensile Testing Machine etc.). Combination of qualitative and quantitative analyses makes accurate diagnosis of textile condition possible. As examples of analyses and conservation of historic textiles, Chuninsan(19 century) similar to sunshade with handing down historic textile and golden decorative skirt(17 century) with excavated costume are taken.

Quantitative and Comparative Analysis of Urinary Steroid Levels upon Treatment of an Anti-Diabetic Drug, CKD-501 using Gas Chromatography-Mass Spectrometry

  • Sadanala, Krishna Chaitanya;Jung, Byung-Hwa;Jang, In-Jin;Chung, Bong-Chul
    • Journal of Pharmaceutical Investigation
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    • v.41 no.1
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    • pp.37-43
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    • 2011
  • Urinary steroid levels were investigated in the treatment of CKD-501, a new anti-diabetic drug candidate. CKD-501 was administered orally at the dosage of 1, 2, 4 mg/day for 7 days to normal men (n=18). Urine was collected before, during and after stopping the drug administration and the urinary level of androgen, estrogen, progestin and corticoids were quantified using GC-MS (gas chromatography-mass spectrometry). Only urinary corticosteroid and an androgen, DHEA levels among all the analyzed steroids, have been found to increase progressively, reaching significant levels on the last day of drug treatment and later declined after the drug treatment is withdrawn. Therefore, it was thought that an increase in the urinary corticoid and DHEA levels could be a characteristic of CKD-501, since it prominently acts on the glucose sensitivity and suppresses the triglyceride levels. In conclusion, it was found that CKD-501, an anti-diabetic drug candidate, affects the glucocorticoid and DHEA levels and it plays a crucial role in glucose homeostasis.

Quantitative Analysis of Isoflavones and Lignans in Sea Vegetables Consumed in Korea Using Isotope Dilution Gas Chromatography-Mass Spectrometry

  • Lee, Young-Joo;Adlercreutz, Herman;Kwon, Hoon-Jeong
    • Food Science and Biotechnology
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    • v.15 no.1
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    • pp.102-106
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    • 2006
  • The phytoestrogens including isoflavones (genistein, daidzein, biochanin A, formononetin, and glycitein), coumestrol, and lignans (secoisolariciresinol, matairesinol, and anhydrosecoisolariciresinol) were quantified in edible sea vegetables from Korea. Sea vegetable samples were collected based on domestic consumption data. After hydrolysis of phytoestrogen glycosides in prepared samples, aglycones of phytoestrogens were extracted with diethyl ether and analyzed with isotope dilution gas chromatography-mass spectrometry in selected ion monitoring mode (ID-GC-MS-SIM). Total samples included 19 samples representing eight species. Most of the samples showed rather low concentrations, ranging from not determinated to $79.2\;{\mu}g/kg$ for isoflavones and from 106.4 to $694.8\;{\mu}g/kg$ for lignans. The daily intake of phytoestrogen from sea vegetables, estimated from the present data and domestic consumption data, was about $0.13\;{\mu}g/day$ for isoflavones and $2.0\;{\mu}g/day$ for lignans. When we compared these results with those from legumes, sea vegetables would not be considered the major source of phytoestrogens in the Korean diet.

Quantitative Analysis of Tiropramide in Human Blood by Gas Chromatography with Nitrogen-Phosphorus Detector

  • Kwon, Oh-Seung;Park, Young-Jin;Ryu, Jae-Chun;Chung, Youn-Bok
    • Archives of Pharmacal Research
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    • v.26 no.5
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    • pp.416-420
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    • 2003
  • The analytical method of antispasmodic agent tiropramide {$(\pm)\alpha$-(benzoylamino)-4-[2-(diethylamino)ethoxy]-N,N-dipropylbenzenepropanamide hydrochloride} was developed by gas chromatography/nitrogen-phosphorus detector (GC/NPD) in human plasma. Two kinds of tiropramide tablets were orally administered to volunteers by Latin square crossover design, and blood was withdrawn as designed schedule. The plasma of 1 mL was loaded on Sep-pak $C_{18}$ cartridge and eluted with methanol after washing with 30% methanol. The residue dissolved in 100 $\mu$L of methanol after evaporation was analyzed by GC/NPD. Precision (CV%) of intra-day was located within 2.6% and accuracy was less than 9.7%. Inter-day precision was below 8.7% and accuracy was relatively good as less than 14%. Plasma samples obtained from human volunteers were analyzed for the determination of tiropramide concentration by using this method. The method was sensitive, rapid and suitable enough to be applied for pharmacokinetic and bioequivalence studies of tiropramide in human volunteers.

Gas Chromatography Residue Analysis of Bifenthrin in Pears Treated with 2% Wettable Powder

  • Choi, Jeong-Heui;Liu, Xue;Kim, Hee-Kwon;Shim, Jae-Han
    • Toxicological Research
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    • v.25 no.1
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    • pp.41-45
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    • 2009
  • This study was conducted to monitor the level of bifenthrin residues in pear sprayed with 2% bifenthrin wettable powder (WP) at the recommended rate at four different schedules prior to harvest. The target analyte was extracted with acetone, partitioned into dichloromethane, and then purified by florisil chromatographic column. The residue determination was performed on a DB-5 capillary column using GC with electron capture detector (ECD). Linearity of this method was quite good ($r^2$ = 0.9951) in the concentration ranged from 0.2 mg/kg to 10 mg/kg. Recovery test was carried out at two concentration levels, 0.2 mg/kg and 1.0 mg/kg, in three replicates, and their rates were from 82.9% to 107.2%. No quantitative bifenthrin was detected in pear of all kinds of treatments including the treatment sprayed 4 times until 7 days before harvest. This sensitive and selective method can be used to monitor the trace residual amounts of bifenthrin in pear in a quite low concentration level.

Analysis of Essential Oils Extracted from Fresh and Shade-dried Leaves of Synurus deltoides (Arr.) Nakai (신선 및 건조된 수리취의 정유 성분 분석)

  • Choi, Hyang-Sook
    • The Korean Journal of Food And Nutrition
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    • v.34 no.2
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    • pp.224-232
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    • 2021
  • This study investigated the volatile flavor composition of essential oils extracted from Synurus deltoides (Arr.) Nakai. The essential oils extracted from the aerial parts of plants by the hydrodistillation extraction method were analyzed by gas chromatography (GC) and GC-mass spectrometry. Ninety-six (98.76%) volatile flavor compounds were identified in the essential oil extracted from fresh leaves of S. deltoides (Arr.) Nakai. The major compounds were 6,10,14-trimethyl-2-pentadecanone (19.91%) and phytol (12.38%). Ninety-seven (97.81%) volatile flavor compounds were identified in the essential oil extracted from shade-dried leaves of S. deltoides (Arr.) Nakai. The major compounds were phytol (51.71%), di(6-methylhept-2-yl) phthalate (7.66%), and 6,10,14-trimethyl-2-pentadecanone (4.23%). Quantitative variations of 6,10,14-trimethyl-2-pentadecanone, phytol and di(6-methylhept-2-yl) phthalate according to different state of S. deltoides (Arr.) Nakai can serve as a quality index of essential oils used in the food industry.

Impurity profiling and chemometric analysis of methamphetamine seizures in Korea

  • Shin, Dong Won;Ko, Beom Jun;Cheong, Jae Chul;Lee, Wonho;Kim, Suhkmann;Kim, Jin Young
    • Analytical Science and Technology
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    • v.33 no.2
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    • pp.98-107
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    • 2020
  • Methamphetamine (MA) is currently the most abused illicit drug in Korea. MA is produced by chemical synthesis, and the final target drug that is produced contains small amounts of the precursor chemicals, intermediates, and by-products. To identify and quantify these trace compounds in MA seizures, a practical and feasible approach for conducting chromatographic fingerprinting with a suite of traditional chemometric methods and recently introduced machine learning approaches was examined. This was achieved using gas chromatography (GC) coupled with a flame ionization detector (FID) and mass spectrometry (MS). Following appropriate examination of all the peaks in 71 samples, 166 impurities were selected as the characteristic components. Unsupervised (principal component analysis (PCA), hierarchical cluster analysis (HCA), and K-means clustering) and supervised (partial least squares-discriminant analysis (PLS-DA), orthogonal partial least squares-discriminant analysis (OPLS-DA), support vector machines (SVM), and deep neural network (DNN) with Keras) chemometric techniques were employed for classifying the 71 MA seizures. The results of the PCA, HCA, K-means clustering, PLS-DA, OPLS-DA, SVM, and DNN methods for quality evaluation were in good agreement. However, the tested MA seizures possessed distinct features, such as chirality, cutting agents, and boiling points. The study indicated that the established qualitative and semi-quantitative methods will be practical and useful analytical tools for characterizing trace compounds in illicit MA seizures. Moreover, they will provide a statistical basis for identifying the synthesis route, sources of supply, trafficking routes, and connections between seizures, which will support drug law enforcement agencies in their effort to eliminate organized MA crime.

Study of the Presence of Residual Hexane in Olive Oils (유통 올리브유의 잔류 헥산에 대한 연구)

  • Kim, Nam-Sook;Lee, Jeung-Hee;Heo, Ok-Soon;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.10
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    • pp.1405-1411
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    • 2006
  • The presence and content of residual hexane in the olive oils were studied. Total 41 olive oils of imported and domestic brands, which were labeled as extra virgin and refined (mixed), were collected from the market. For analysis, electronic nose and headspace SPME-GC/MS were used. Electronic nose equipped with 12 metal oxide sensors was used for the discrimination of odor pattern of olive oils against the different concentrations of hexane. From the results, it is assumed that the contents of residual hexane in the collected olive oils were below 5 ppm. For Qualitative and quantitative analysis of hexane, polydimethylsiloxane (PDMS) fiber was employed for SPME-GC/MS. In the results, the peak of residual hexane was detected in 8 samples from 41 olive oils. But the detected level was no more than 1 ppm that is under the regulation limit (5 ppm) by Korea Food Additive Code.

Quantitative Analysis and Qualification of Amitrole Using LC/ESI-MS (LC/ESI-MS를 이용한 아미트롤의 정성확인 및 정량분석)

  • Park, Chan-Koo;Eo, Soo-Mi;Kim, Min-Young;Sohn, Jong-Ryeul;Mo, Sae-Young
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.117-129
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    • 2004
  • Amitrole in environment, difficult to be analyzed by GC or GC/MS due to high polarity and low volatility, was analyzed by LC/ESI/MS in the study. Maximum peak intensity of amitrole in LC/MS/ESI mass spectrum is m/z 85 of protonated molecular ion $(M+H)^+$ with 30V of cone voltage at SIR mode. It was confirmed that ratios between main ion of amitrole, 85 of protonated molecular ion, and m/z 58 fragmented ion of amitrole, had increased corresponding with the increment of cone voltage from 20V to 70V. The isotope molecular weight of amitrole was $86([M+H])^+$ at LC/MS analysis and the mass spectrum ratio between 85 mass and 86 mass was not different by the change of concentration but similar to theoretical ratio(less than 10% standard deviation).The linearity of standard calibration curve under same condition with sample treatment method had $y=1.09354e^6X+26947.2$ and $r^2=0.99$. Recovery rates in water and soil samples were 77.64~83.44% and 71.11~79.44%, respectively. Reliability of the analysis was performed with 5 repeated measurements at each level of standard concentration and the result showed that relative standard deviation was less than 10%; therefore, the extraction and analysis method in the study suggested that it would be reliable to measure amitrole in water and soil media.