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Simultaneous Determination of Cannabidiol, Cannabinol, and ${\Delta}^9-Tetrahydrocannabinol$ in Human Hair by Gas Chromatography-Mass Spectrometry

  • Kim Jin Young;Suh Sung Ill;In Moon Kyo;Paeng Ki-Jung;Chung Bong Chul
    • Archives of Pharmacal Research
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    • v.28 no.9
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    • pp.1086-1091
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    • 2005
  • An analytical method was developed for evaluating the cannabidiol (CBO), cannabinol (CBN), ${\Delta}^9-tetrahydrocannabinol$ $({\Delta}^9-THC)$ level in human hair using gas chromatography-mass spectrometry (GC-MS). Hair samples (50mg) were washed with isopropyl alcohol and cut into small fragments (< 1mm). After adding a deuterated internal standard, the hair samples were incubated in 1.0M NaOH for 10 min at $95^{\circ}C$. The analytes from the resulting hydrolyzed samples were extracted using a mixture of n-hexane-ethyl acetate (75:25, v/v). The extracts were then evaporated, derivatized, and injected into the GC-MS. The recovery ranges of CBD, CBN, and ${\Delta}^9-THC$ at three concentration levels were $37.9-94.5\%$ with good correlation coefficients $(r^2>0.9989)$. The intra-day precision and accuracy ranged from $-9.4\%\;to\;17.7\%$, and the inter-day precision and accuracy ranged from $-15.5\%\;to\;14.5\%$, respectively. The limits of detection (LOD) for CBD, CBN, and ${\Delta}^9-THC$ were 0.005, 0.002, and 0.006 ng/mg, respectively. The applicability of this method of analyzing the hair samples from cannabis abusers was demonstrated.

Analytical Method Development for Determination of Coenzyme Q10 by LC-MS/MS in Related Health Functional Foods (건강기능식품에서 LC-MS/MS를 이용한 코엔자임Q10 분석법 연구)

  • Lee, Jin Hee;Oh, Mihyune
    • Journal of Food Hygiene and Safety
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    • v.34 no.6
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    • pp.519-525
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    • 2019
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we are continuing our research on analytical method development for the items listed in the Korean Health Functional Food Codex. In this study, we have developed a sensitive and selective test method that could simultaneously separate and determine coenzyme Q10 based on liquid chromatographic-tandem mass spectrometry (LC-MS/MS). Calibration curves showed linearity with a correlation coefficient (R2) of > 0.999 and the limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 26.0 ㎍/L and 78.9 ㎍/L, respectively. The recovery results ranged between 98.6-107.0% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high resolution of the coenzyme Q10 and the assay was fully validated as well.

Identification of Impurities in a Sample of Illicitly Synthesized Methamphetamine

  • Kim, Sung-Hong;Kwon, Woo-Jung;Ryoo, Jae-Jung;Ko, Beom-Jun;Suh, Yong-Jun;In, Mun-Kyo
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.285.2-286
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    • 2003
  • Analysis of illicit methamphetamine samples seized in Korea is discussed. The samples are extracted with the small portion of ethyl acetate under neutral conditions and the extracts are analyzed by GC-MS. Several impuritiy peaks are found in each chromatrogram. Eight compunds (1,2-Dimethyl-3-phenylaziridine, amphetamine oxime, ephedrine, N-formylmethamphetamine, N-acetylmethamphetamine, acetylephedrine, 3,4-dimethyl-5-phenyl-2-oxazolidone, methamphetamine dimer) are identified impurities in illicit methamphetamine and the identity of the impurity is conformed synthesis. (omitted)

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Environment, Health and Safety Offices of the Top 30 Research Universities in the U.S.A. - Focused on the Case of Massachusetts Institute of Technology(MIT) (미국 상위 30개 연구 중심 대학들의 실험실 환경보건안전 담당 부서 - MIT 사례를 중심으로)

  • Ahn, Kwangseog;Kang, Dongmug;Shin, Yong Chul;Jun, Young-Hee
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.17 no.3
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    • pp.192-202
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    • 2007
  • Objectives: The objectives of this research are to examine the missions, organization, and programs of the environmental, health and safety(EHS) offices of the major research universities in the U.S.A., particularly the case of Massachusetts Institute of Technology(MIT) EHS Office, and to suggest ways to address the EHS issues of the universities and research institutes in South Korea. Methods: The top 30 research universities in the U.S.A. were selected by the total amounts of research funds they annually received. The web sites of the 30 universities were searched to identify the names of the departments that address environment, health, and/or safety related issues, the missions of those departments, the major programs of those departments, and the number of staff in those departments. Also, a case study was conducted for the Environment Health and Safety Management System and the Environment, Health and Safety Office of the MIT, using literature and web searches and a meeting with the Director of the MIT Environment, Health and Safety Office. Results: All the top 30 research universities in the U.S.A. had designated departments that dealt with EHS issues. Most of them were by the name of or similar to environmental, health and safety. The mission statements of those departments were mostly about improving the safety and health of their community members, improving the environment, and complying to EHS regulations. Most of those departments had an environmental management program, industrial hygiene program, radiation protection program, safety program, and biosafety program as their major programs. The components of the environment, health and safety management system(EHS-MS) of the MIT were examined in detail. In contrast, not many universities in South Korea had designated departments that dealt specifically with EHS issues. Also, the number of fulltime staff for EHS was only 1-2 in most of the Korean universities and their work duties included only general safety, while neglecting other health/environment related issues. Conclusions: Well organized and functioning environmental, health and safety offices were present in all of the top 30 research universities in the U.S.A., whereas similar organizations of the universities in South Korea were virtually non-existent and/or had very limited EHS activities. Therefore, in order to reduce potential risks of accidents and health problems in the Korean universities and research institutions, well established and functioning EHS-MSs and EHS offices are warranted. The case of the EHS-MS and EHS Office in the MIT demonstrate a successful case to follow.

Distributional Characteristics of Volatile Organic Compounds in the Indoor Air of Various Office Environments (다양한 사무실 실내환경에서의 휘발성유기화합물의 농도분포 특성)

  • Baek, Sung-Ok;Jeon, Chan-Gon
    • Journal of Korean Society for Atmospheric Environment
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    • v.30 no.5
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    • pp.477-491
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    • 2014
  • This study was carried out to evaluate the concentration variations of volatile organic compounds (VOCs) in the office environments located in a large urban area with respect to seasonality, smoking status, types of ventilation and heating. Indoor air sampling was undertaken in 37 and 30 offices in Daegu city during summer and winter, respectively. The VOC samples were collected using adsorbent tubes, and were determined by thermal desorption coupled with GC/MS analysis. The analytical method was validated for repeatability, method detection limits (MDL), and duplication precision. A total of 34 VOCs of environmental concern were determined, including 15 aromatics and 19 halogenated hydrocarbons. Average concentrations of BTEX appeared to 1.91 ppb, 22.98 ppb, 3.44 ppb, and 3.70 ppb, respectively. These values were relatively higher levels than those measured at homes and outdoor roadsides reported by other researches. In general, the concentrations of VOCs were higher in winter than summer, in smoking offices than non-smoking offices, in forced ventilation type than natural ventilation type, and in combustion heating than non-combustion heating offices. However, such differences were not always significant at a level of 0.05 by statistical tests (t-test and/or Mann-Whitney test) with some exceptions for BTEX and styrene. This study demonstrated that smoking status, ventilation type and presence of combustion sources indoors could be important factors on the elevated concentrations of some VOCs in the office environment.

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.

Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.161-170
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    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

Regression model for the preparation of calibration curve in the quantitative LC-MS/MS analysis of urinary methamphetamine, amphetamine and 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid using R (소변 중 메트암페타민, 암페타민 및 대마 대사체 LC-MS/MS 정량분석에서 검량선 작성을 위한 R을 활용한 회귀모델 선택)

  • Kim, Jin Young;Shin, Dong Won
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.241-250
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    • 2021
  • Calibration curves are essential in quantitative methods and for improving the accuracy of analyte measurements in biological samples. In this study, a statistical analysis model built in the R language (The R Foundation for Statistical Computing) was used to identify a set of weighting factors and regression models based on a stepwise selection criteria. An LC-MS/MS method was used to detect the presence of urinary methamphetamine, amphetamine, and 11-nor-9-carboxy-Δ9 -tetrahydrocannabinol in a sample set. Weighting factors for the calibration curves were derived by calculating the heteroscedasticity of the measurements, where the presence of heteroscedasticity was determined via variance tests. The optimal regression model and weighting factor were chosen according to the sum of the absolute percentage relative error. Subsequently, the order of the regression model was calculated using a partial variance test. The proposed statistical analysis tool facilitated selection of the optimal calibration model and detection of methamphetamine, amphetamine, and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol in urine. Thus, this study for the selection of weighting and the use of a complex regression equation may provide insights for linear and quadratic regressions in analytical and bioanalytical measurements.

Establishment of Library for the Identification of Corticosteroids in Various Known Sample Types (미지시료에서 부신피질호르몬제의 확인을 위한 라이브러리 구축)

  • Park, Mee-Jung;Hong, Hyo-Jeong;Lee, Sang-Ki
    • YAKHAK HOEJI
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    • v.55 no.4
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    • pp.289-294
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    • 2011
  • Illegal addition of steroids into cosmetics, ointments or drugs have been increased and their careless usage induced detrimental effect on health. We developed simultaneous analytical method using TLC, HPLC and LC/MS for the identification of 40 corticosteroids. 34 corticosteroids were well separated in HPLC with isocratic mode and remaining 6 drugs were also separated with gradient mode. All of the 40 corticosteroids were detected in negative mode in LC/MS. Halcinonide, prednisolone, triamcinolone acetonide and methylprednisolone hemisuccinate were detected in real samples.

A Proposal for Improving the Perception of Differential Concept by Using a Well-Known Table Processor: MS Excel

  • Tolga, Kabaca;Seref, Mirasyedioglu
    • Research in Mathematical Education
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    • v.12 no.3
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    • pp.193-200
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    • 2008
  • In this study, an innovative computer support has been suggested to improve differential perception of the students. Research has been conducted on a calculus class which has 35 students. A semi-structured interview has been reported in the study. By this interview, it was tried to make differential concept more understandable by using Micro Soft Excel component of the well-known MS Office software. By this aim, students have been asked to integrate a simple function by using MS Excel. At the end of the study, it was observed that differential concept made more sense in students' minds than previous.

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