• Title/Summary/Keyword: 내부표준법

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Development of 10 μmol/mol Hydrogen Sulfide Primary Standard Gas for Odor Measurements (악취측정용 10 μmol/mol 황화수소 표준가스 개발)

  • Kim, Yong-Doo;Bae, Hyun-Kil;Kim, Dalho;Oh, Sang-Hyub;Lee, Jin Hong;Lee, Sangil
    • Journal of the Korean Institute of Gas
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    • v.22 no.2
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    • pp.46-51
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    • 2018
  • Hydrogen sulfide from landfill and sewage treatment plant is a major odor component and causes many civil petitions. Rapidly developing industries release hydrogen sulfide, an odorous gas, to the atmosphere. This study aims to develop a $10{\mu}mol/mol$ concentration level hydrogen sulfide primary standard gas for odor measurement. The hydrogen sulfide gas was prepared at a nominal concentration of $10{\mu}mol/mol$ in nitrogen using the gravimetric method described in ISO 6142. Replicate standard gases were produced in 4 aluminium cylinders, and their concentrations were verified by GC-AED. The uncertainty of production was less than 0.50 %, and the variation of the 4 replicates was 0.22 %. The wall adsorption of hydrogen sulfide in cylinders was 0.10 % at 1500 psi, and the concentration was estimated to be long-term stable for one year. The relative expanded uncertainty of the preparation consistency, adsorption and long-term stability of this hydrogen sulfide standard gas was less than 1.05 % (95 % of confidence level, k=2).

A Study on Residual Amounts of Vinyl Chloride/Vinylidene Chloride in Poly(vinyl chloride)/Poly(vinylidene chloride) Food Packaging using Headspace GC/MS (헤드스페이스 GC/MS를 이용한 폴리염화비닐/폴리염화비닐리덴 식품 포장 중 염화비닐/염화비닐리덴 잔류량 연구)

  • Sung, Jun-Hyun;Kwak, In-Shin;Park, Sung-Kwan;Kim, Hyung-Il;Lim, Ho-Soo;Lee, Ju-Young;Byun, Mi-Yun;Kim, So-Hee
    • Korean Journal of Food Science and Technology
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    • v.43 no.1
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    • pp.6-11
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    • 2011
  • Vinyl chloride (VC) and vinylidene chloride (VDC), which may be present in poly(vinyl chloride) (PVC) and poly(vinylidene chloride) (PVDC) food packaging, were analyzed by using a headspace-gas chromatograph (GC)/mass spectrometer (MS) equipped with a PLOT Q column. 1-Chloropropane (1-CP) was used as an internal standard. The determinations of VC and VDC were carried out by monitoring the characteristic ions for each compound: m/z=61, 62, 64 and m/z=61, 96, 98, respectively. The method validated in this study can be suitable for the compliance test of EU regulation. Among 103 food packaging samples, VC and VDC were not detected, except in one PVDC food package. However, the detected level of VDC in the sample was below the EU regulatory specific limitation.

Cooked Odor Components of Sergia Lucens and Its Fermented Product (새우 및 새우젓의 향기성분(香氣成分))

  • Choi, Sung-Hee
    • Korean Journal of Food Science and Technology
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    • v.19 no.2
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    • pp.157-163
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    • 1987
  • Changes in the odor components of Sergia Lucens during fermentation were studied by simultaneous distillation and extraction method. Forty seven components were identified by GC and GC-MS. Major cooked odor components of raw material were alkyl pyrazines and thialdine. Alkyl pyrazines, furfuryl alcohol, isoamyl alcohol and sulfide compounds, such as dimethylsulfide and dimethyltrisulfide increased during the period of fermentation. On the other hand, thialdine content decreased as the period of fermentation was extended. Sensory evaluation of cooked Sergia Lucens odor was carried out by GC-sniff analysis. The odors of GC effluents at the sniffing port were sniffed in order to find out the key compound of cooked Sergia Lucens odor components. The results of the GC-sniff analysis indicated that 2,5-dimethylpyrazine, 2,6-dimethylpyrazine and 2,3-dimethylpyrazine had dried or roast shrimp-like odor and thialdin had dried small sardine-like odor. The result showed that pyrazines and thialdine could play an important role in the formation of cooked Sergia Lucens odor.

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Determination of Haloperidol Serum Levels in Psychiatric Patients with Gas Chromatography-Nitrogen Phosphorus Detection (GC/NPD를 이용한 정신분열증 환자의 혈중 Haloperidol 정량분석)

  • Paik, Man-Jeong;Kang, Bo-Kyoung;Lee, Kyoung-Ok;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.161-166
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    • 1998
  • Analytical method of haloperidol (HAL) in serum which has been widely used in therapy of schizophrenic disorders is developed. Gas chromatography/nitrogen-phosphorus detection (GC/NPD) was used for this study. Bromoperidol was used as an internal standard and diethylether as a solvent of three-step extraction. The extraction yield in this procedure was $67.5{\pm}1.9%$ at 15 ng/mL. A good linear response in the range of 1~40 ng/mL was obtained with correlation coefficient of $r^2=0.999$. Detection limit was 0.5 ng/mL when 2 mL of serum was used. This method was applied for the analysis of HAL in serum of schizophrenic patients. After HAL decanoate (HD) was intaken as intramuscular route, HAL levels were determined at second week and forth week. From the result, the concentration of HAL at forth week appeared to 29.6% lower than those at second week. The present method showed low detection limit and high selectivity. Therefore it can be applied for the trace analysis of HAL in serum and the monitoring.

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Optimized Condition of Genomic DNA Extraction and PCR Methods for GMO Detection in Potato (유전자재조합 감자의 검정을 위한 DNA분리 및 PCR검출의 최적조건 탐색)

  • Shin, Weon-Sun;Kim, Myung-Hee
    • Korean Journal of Food Science and Technology
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    • v.35 no.4
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    • pp.591-597
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    • 2003
  • To compare the quality of genomic DNA extracted from potato for PCR detection, four different methods, such as silica-based membrane method, silica-coated bead method, STE solution treatment, and CTAB-phenol/chloroform method, were evaluated. Also, to remove an excessive carbohydrate from the potato, ${\alpha}$- and ${\beta}$-amylase were used individually and in combination. When used both silica-based membrane method and silica-coated bead method combined with enzymes, the genomic DNAs were extracted from the raw potato with high purity for PCR. However, the silica-coated head method combined with enzyme treatment was the most efficient for extraction of the genomic DNA from the frozen fried potatoes. When applied with STE solution, the highly purified DNA was extracted from the raw potatoes without enzyme treatment in adequate yield for PCR. In cases of processed potatoes, such as frozen-fried potato and fabricated potato chips, CTAB-phenol/chloroform method is mostly feasible for DNA extraction and PCR efficacy at high sensitivity. As the results of PCR amplification, 216bp of PCR product was detected on 2% agarose gel electrophoresis, but any amplicons derived from New leaf and New leaf Y gene was not detected in any sample.

The study on the measurement of formaldehyde in saliva and urine by GC-MS (가스크로마토그래프-질량분석기에 의한 타액 및 뇨 중 포름알데하이드 분석법 연구)

  • Shin, Ho-Sang;Ahn, Hye-Sil
    • Analytical Science and Technology
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    • v.19 no.2
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    • pp.149-154
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    • 2006
  • A gas chromatography-mass spectrometric method was developed for the determination of formaldehyde in urine and saliva. In a 20 mL glass tube, 0.2 mL of urine or saliva was taken. Further, 1.8 mL of 0.1 M HCl, 0.1 mL of 2,000 mg/L 2,4-dinitrophenyl hydrazine and $20{\mu}l$ of 500 mg/L acetone-$d_6$ as internal standard were added in the tube and sealed tightly with cap. The solution was shaken for 20 min at room temperature and extracted using 4 mL of toluene. The extract was concentrated and redissolved with $100{\mu}l$ of acetonitrile, and then measured by gas chromatography-mass spectrometer (selected ion monitoring). The detection limit was 2.0 ng/mL and 0.5 ng/mL in saliva and urine, respectively. The calibration curves showed good linearity with r = 0.997 and 0.998 for saliva and urine, respectively. The method was used to analyze formaldehyde in rat urine after oral exposure. The developed method may be use ful to the monitoring for formaldehyde exposure in human.

Improvement of an Simultaneous Determination for Clenbuterol and Ractopamine in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 clenbuterol과 ractopamine의 동시 분석법 개선)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Young;Kim, Hyung-Soo;Kang, Ilhyun;Do, Jung-Ah;Oh, Jae-Ho;Kwon, Kisung;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.25-33
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    • 2013
  • Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.259-266
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    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

Efficient Application of Westgard Multi-Rules and Quality Control Implementation Improvement (Westgard Multi-Rules의 효율적 적용과 조치사항의 개선)

  • Jung, Heung Soo;Oh, Youn Jung;Bae, Jin Soo;Baek, Jin Young;Hwang, Bo ra;Shin, Yong Hwan
    • The Korean Journal of Nuclear Medicine Technology
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    • v.21 no.1
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    • pp.60-64
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    • 2017
  • Purpose Westgard multi-rules application based on test quality improvement and commercialized international standard has been widely used in quality control. However, it is difficult to applicate the Westgard multi-rules in nuclear medicine in vitro tests due to the larger sample sizes and the simultaneous measurement of quality control material and patient sample. This study investigated the usefulness of Westgard multi-rules application in nuclear medicine in vitro tests. Materials and Methods A total of 282 systematic error multi-rules (22s, 101s) recorded in the samsung medical center computer system from January 2013 to June 2016 along with 117 cases of corrective measure record was analyzed. The Quality control implementation is recorded in Hospital information system were divided into 4 high-level areas including quality control material error, experimental procedural error, Kit lot number management error, and others. To prevent quality control material error, the existing method that each staff used their own method was changed. The staff who in charge of managing the quality control material was designated and daily consumption amount of every test was strictly controlled by one person. To prevent other errors, every test step was standardized so that the entire test procedures are identically implemented. Results The total quality control implementation was 117 cases; As a result, 62 quality control material errors were 62 cases, experimental process errors were 24 cases, Kit lot number control errors were 18 cases, and other errors were 13 cases. The quality control material error was corrected and could be used fresh materials within 2 days after thawing. The cases of systemic error were decreased to causes as quality control material error. The quality control materials were reduced above 10 vials to a monthly average. In addition, these errors of experimental processing and Kit lot number were improved by test standardization. Consequently, the cases of 101s and 22s in systematic error rules decreased at least 2 cases to a monthly average. Conclusion To confirm of systematic error through multi-rules application quickly, it is necessary to base on management of the QC material, target values and standard deviation. Moreover, in the event of a systematic error, it was found important to record measures based on test cause analysis. The experiment results are expected to contribute to internal quality control improvement and prompt and accurate result reporting through error recording and causal analysis based on Westgard multi-rules analysis.

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Functional Brain Mapping Using $H_2^{15}O$ Positron Emission Tomography ( I ): Statistical Parametric Mapping Method ($H_2^{15}O$ 양전자단층촬영술을 이용한 뇌기능 지도 작성(I): 통계적 파라메터 지도작성법)

  • Lee, Dong-Soo;Lee, Jae-Sung;Kim, Kyeong-Min;Chung, June-Key;Lee, Myung-Chul
    • The Korean Journal of Nuclear Medicine
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    • v.32 no.3
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    • pp.225-237
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    • 1998
  • Purpose: We investigated the statistical methods to compose the functional brain map of human working memory and the principal factors that have an effect on the methods for localization. Materials and Methods: Repeated PET scans with successive four tasks, which consist of one control and three different activation tasks, were performed on six right-handed normal volunteers for 2 minutes after bolus injections of 925 MBq $H_2^{15}O$ at the intervals of 30 minutes. Image data were analyzed using SPM96 (Statistical Parametric Mapping) implemented with Matlab (Mathworks Inc., U.S.A.). Images from the same subject were spatially registered and were normalized using linear and nonlinear transformation methods. Significant difference between control and each activation state was estimated at every voxel based on the general linear model. Differences of global counts were removed using analysis of covariance (ANCOVA) with global activity as covariate. Using the mean and variance for each condition which was adjusted using ANCOVA, t-statistics was performed on every voxel To interpret the results more easily, t-values were transformed to the standard Gaussian distribution (Z-score). Results: All the subjects carried out the activation and control tests successfully. Average rate of correct answers was 95%. The numbers of activated blobs were 4 for verbal memory I, 9 for verbal memory II, 9 for visual memory, and 6 for conjunctive activation of these three tasks. The verbal working memory activates predominantly left-sided structures, and the visual memory activates the right hemisphere. Conclusion: We conclude that rCBF PET imaging and statistical parametric mapping method were useful in the localization of the brain regions for verbal and visual working memory.

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