• Title/Summary/Keyword: Detection concentration

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Changes of Endogenous Steroids Profile After Oral Administration of Danazol (Danazol의 경구투여에 따른 내인성 스테로이드들의 변화)

  • Choi, Man Ho;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.11 no.5
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    • pp.353-359
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    • 1998
  • Danazol, one of the IOC banned substances, is a synthetic steroid which stimulates the synthesis of cellular protein with multiple and diverse biologic effects. To confirm the androgenic effects of danazol, levels of eight endogenous steroids and its major metabolite in human urine were simultaneously analyzed by selected ion monitoring (SIM) of GC/MS after oral administration. The recovery range of this method was 71.59%~93.56% and the RSD values of precision and accuracy test were 1.87%~10.48% and 1.32%~11.25%, respectively. The limits of detection of most of the drugs were $0.01{\sim}0.05{\mu}g/mL$ and calibration was carried out using urine spiked with each endogenous steroid and ethisterone standard at a concentration of 0.1, 0.5, 1.0, 10, 20 and $50{\mu}g/mL$ and with $10{\mu}g/mL$ of internal standard. Correlation coefficients varied between 0.963 and 0.991. The endogenous steroid profiling is one of valuatle tool for decteation of anabolic steroids.

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Determination of benzene, toluene, ethylbenzene and o-xylene in bottled waters by headspace solid-phase microextraction and gas chromatography/mass spectrometry (HS-SPME-GC/MS를 이용한 먹는 샘물 중 벤젠, 톨루엔, 에칠벤젠, 자일렌의 정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.119-126
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    • 2011
  • Abstract: The amount of benzene, toluene, ethylbenzene, and o-xylene (BTEX) in 30 kinds of bottled waters purchased from market and 9 kinds of tap waters from home were determined using headspace solid phase microextraction (HS-SPME). The sample was stirred at 1200 RPM G for 4 min using a magnetic bar with $100\;{\mu}m$ PDMS as adsorbent for BTEX. Then it was desorbed from the fiber for 1 min at room temperature. Quantitation was achieved using standard calibration method. The limit of detection was determined as benzene 0.39 (${\pm}0.04$) ng/mL, toluene 0.08 (${\pm}0.04$) ng/mL, ethylbenzene 0.04 (${\pm}0.01$) ng/mL, and o-xylene 0.05 (${\pm}0.02$) ng/mL. Benzene and o-xylene were not detected in any samples, but toluene was detected in 11 samples, and ethylbenzene was detected just in 3 samples among 30 investigated bottled waters. The concentration range of investigated materials for toluene and o-xylene were $0.24({\pm}0.09)\sim2.95\;({\pm}0.08)\;ng/mL$, $0.08({\pm}0.06)\sim0.93({\pm}0.10)\;ng/mL$, respectively.

Independent and Additive Interaction Between Tumor Necrosis Factor β +252 Polymorphisms and Chronic Hepatitis B and C Virus Infection on Risk and Prognosis of Hepatocellular Carcinoma: a Case-Control Study

  • Jeng, Jen-Eing;Wu, Hui-Fang;Tsai, Meng-Feng;Tsai, Huey-Ru;Chuang, Lea-Yea;Lin, Zu-Yau;Hsieh, Min-Yuh;Chen, Shinn-Chern;Chuang, Wan-Lung;Wang, Liang-Yen;Yu, Ming-Lung;Dai, Chia-Yen;Tsai, Jung-Fa
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.23
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    • pp.10209-10215
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    • 2015
  • To assess the contribution of tumor necrosis factor $(TNF){\beta}$ +252 polymorphisms to risk and prognosis of hepatocellular carcinoma (HCC), we enrolled 150 pairs of sex- and age-matched patients with HCC, patients with cirrhosis alone, and unrelated healthy controls. $TNF{\beta}$ +252 genotypes were determined by polymerase chain reaction with restriction fragment length polymorphism. Multivariate analysis indicated that $TNF{\beta}$ G/G genotype [odds ratio (OR), 3.64; 95%CI, 1.49-8.91], hepatitis B surface antigen (OR, 16.38; 95%CI, 8.30-32.33), and antibodies to hepatitis C virus (HCV) (OR, 39.11; 95%CI, 14.83-103.14) were independent risk factors for HCC. There was an additive interaction between $TNF{\beta}$ G/G genotype and chronic hepatitis B virus (HBV)/HCV infection (synergy index=1.15). Multivariate analysis indicated that factors associated with $TNF{\beta}$ G/G genotype included cirrhosis with Child-Pugh C (OR, 4.06; 95%CI, 1.34-12.29), thrombocytopenia (OR, 6.55; 95%CI, 1.46-29.43), and higher serum ${\alpha}$-fetoprotein concentration (OR, 2.53; 95%CI, 1.14-5.62). Patients with $TNF{\beta}$ G/G genotype had poor cumulative survival (p=0.005). Cox proportional hazard model indicated that $TNF{\beta}$ G/G genotype was a biomarker for poor HCC survival (hazard ratio, 1.70; 95%CI, 1.07-2.69). In conclusion, there are independent and additive effects between $TNF{\beta}$ G/G genotype and chronic HBV/HCV infection on risk for HCC. It is a biomarker for poor HCC survival. Carriage of this genotype correlates with disease severity and advanced hepatic fibrosis, which may contribute to a higher risk and poor survival of HCC. Chronic HBV/HCV infected subjects with this genotype should receive more intensive surveillance for early detection of HCC.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Pentoxifylline in Human Serum (체내동태 연구를 위한 혈청 중 펜톡시필린의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Yoo, Hee-Doo;Lee, Hwa-Jeong;Moon, Jai-Dong;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.2
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    • pp.89-95
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    • 2006
  • A selective and sensitive reversed-phase HPLC method for the determination of pentoxifylline in human serum was developed, validated, and applied to the pharmacokinetic study of pentoxifylline. Pentoxifylline and internal standard, chloramphenicol, were extracted from the serum by liquid-liquid extraction with dichloromethane and analyzed on a Luna CI8(2) column with the mobile phase of acetonitrile-0.034 M phosphoric acid (25:75, v/v, adjusted to pH 4.0 with 10 M NaOH). Detection wavelength of 273 nm and flow rate of 0.8 mL/min were used. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of the serum was 10 ng/mL, which was sensitive enough for pharmacokinetic studies of pentoxifylline. The overall accuracy of the quality control samples ranged from 89.3 to 92.7% for pentoxifylline with overall precision (% C.V.) being 4.1-9.2%. The relative mean recovery of pentoxifylline for human serum was 105.8%. Stability (stock solution, short and long-term) studies showed that pentoxifylline was not stable during storage. But three freeze-thaw cycles and extracted serum samples were stable. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of pentoxifylline in human serum samples for the pharmacokinetic studies of orally administered $Trental^{\circledR}$ tablet (400 mg pentoxifylline), demonstrating the suitability of the method.

Sensitivity of Sclerotium cepivorum Causing Garlic White Rot Isolated from Taeahn, Seosan and Goheung Areas to Fungicides (서산, 태안 및 고흥 지역에서 마늘 흑색썩음병을 일으키는 Sclerotium cepivorum의 살균제 감수성 조사)

  • Kim, Hyung Jo;Choi, Woobong;Kim, Heung Tae
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.133-139
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    • 2013
  • To investigate the sensitivity of Sclerotium cepivorum causing garlic white rot to 5 fungicides, including prochloraz, tebuconazole, flutolanil, iminoctadine and isoprothiolane, 147 isolates isolated from infected garlics from 2008 to 2009 through a single sclerotium isolation were screened. While each mean value of $EC_{50}$ (effective concentration reducing mycelial growth by 50%) of S. cepivorum isolates collected in 2008 to each fungicide was 0.054, 0.012, 23.189, 0.901, and $21.362{\mu}g\;mL^{-1}$, that of 2009 isolates were 0.030, 0.020, 10.367, 1.684, $33.406{\mu}g\;mL^{-1}$. There was a difference in mean value of $EC_{50}$ of S. cepivorum according to regions isolated. $EC_{50}$ values of S. cepivorum isolated in Goheung to flutolanil and isoprothiolane were 14.468 and $24.653{\mu}g\;mL^{-1}$, respectively, which was lower than those of Seosan and Taeahn. Isolates from Taeahn showed the lowest $EC_{50}$ value to prochloraz as $0.008{\mu}g\;mL^{-1}$. In addition, we could not find any resistant isolates to fungicides tested. The $EC_{50}$ values in this study will be used in a fungicide resistance monitoring program to determine whether shifts in sensitivity to fungicides included into different groups are occurring in S. cepivorum populations.

Field Performance Evaluation of Candidate Samplers for National Reference Method for PM2.5 (PM2.5 국가기준측정장비 선정을 위한 비교 측정 연구)

  • Lee, Yong Hwan;Park, Jin Su;Oh, Jun;Choi, Jin Soo;Kim, Hyun Jae;Ahn, Joon Young;Hong, You Deog;Hong, Ji Hyung;Han, Jin Seok;Lee, Gangwoong
    • Journal of Korean Society for Atmospheric Environment
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    • v.31 no.2
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    • pp.157-163
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    • 2015
  • To establish National Reference Method (NRM) for $PM_{2.5}$, operational performance of 5 different commercial gravimetric-based $PM_{2.5}$ measuring instruments was assessed at Bulkwang monitoring station from January 23, 2014 to February 28, 2014. First, physical properties, design, and functional performance of the instruments were assessed. Evaluation was carried out to determine whether operating method for the instruments and levels of QA/QC activities meet the data quality objectives (DQOs). To verify whether DQOs were satisfied, reproducibility of QA/QC procedures, accuracy, relative sensitivity, limit of detection, margin of error, and coefficient of determination of the instruments were also evaluated. Results of flow rate measurement of 15 candidate instruments indicated that all the instruments met performance criteria with accuracy deviation of 4.0% and reproducibility of 0.6%. Comparison of final $PM_{2.5}$ mass concentrations showed that the coefficient of determination ($R^2$) values were greater than or equal to 0.9995, and concentration gradient ranged from 0.97 to 1.03. All the instruments satisfied criteria for NRM with the estimated precision of 1.47~2.60%, accuracy of -1.90~3.00%, and absolute accuracy of 1.02~3.12%. This study found that one particular type of measuring instrument was proved to be excellent, with overall evaluation criteria satisfied.

A Study on the Concentration Distribution of Airborne Heavy Metals in Major Industrial Complexes in Korea (국내 주요 산업단지 대기 중 중금속농도 분포에 관한 연구)

  • Kang, Byung-Wook;Kim, Min-Ji;Baek, Kyung-Min;Seo, Young-Kyo;Lee, Hak Sung;Kim, Jong-Ho;Han, Jin-Seok;Baek, Sung-Ok
    • Journal of Korean Society for Atmospheric Environment
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    • v.34 no.2
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    • pp.269-280
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    • 2018
  • This paper reports the results of field evaluation to determine the levels of heavy metals in major industrial complexes in Korea over a seven year period (2007~2013). The measurement of heavy metal was conducted using quartz fiber filter sampling and ICP-AES analysis. In order to validate the analytical performance of these methods, studies were also carried out to investigate data quality control(QC) parameters, such as the method detection limit (MDL), repeatability, and recovery efficiencies. The average concentrations of total suspended particulates (TSP) for the nine industrial complexes in Korea were $104{\sim}169{\mu}g/m^3$, which was higher than other industrial complexes and urban areas. The Sihwa and Banwol industrial complexes were shown to be the biggest contributing sources to high TSP emission ($159{\mu}g/m^3$ and $169{\mu}g/m^3$, respectively). The concentrations of heavy metals in TSP were higher in the order of Fe>Cu>Zn, Pb, Mn>Cr, Ni, As and Cd. It was observed that Fe was the highest in the Gwangyang and Pohang steel industrial complexes. The concentrations of Zn and Pb were high in Onsan, Sihwa and Banwol industrial complexes, and this was attributed to the emission from the nonferrous industry. Additionally, Cr and Ni concentrations were high in the Sihwa and Banwol industrial complexes due to plating industry. On the other hand, Ulsan and Onsan industrial complexes showed high Cr and Ni concentrations as a response to the emission of metal industry related to automobile. The correlation analysis revealed the high correlation between Cr and Ni in plating industry from Sihwa and Banwol industrial complexes. Adding to this, components related to coal combustion and road dust showed high correlation in Pohang and Gwangyang industrial complexes. Then Onsan and Ulsan industrial complexes showed high correlation among components related to the nonferrous metals.

Characterization of Leaching Behaviour of Recycled Concrete for Environmental Assessment (용출특성규명을 통한 재생골재 환경성 평가)

  • Kang, S.H.;Lee, S.H.;Kwak, K.S.;Lee, J.Y.;Chung, M.K.
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.3
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    • pp.293-301
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    • 2005
  • We conducted several different leaching experiments for assessing the potential environmental risk when utilizing recycled concrete for stabilizing bridge pier. The methods include continuous batch leaching test (DIN 38414-S4), availability test (NEN 7341), pH-stat test (CEN/TC 292/WG6) and tank diffusion test (NEN 7345). The concentration ranges vary depending on the testing method. Nearly all the trace elements were low, some elements recording under detection limit. The maximum concentrations for trace elements leached throughout the whole tests are (as mg/L); Cd (0.029), Cu (0.437), Pb (0.14), Ni, Zn (0.95), Hg (0.005). Although the testing methods we used in this study are much more rigorous than other commonly adapted method including TCLP and domestic testing method for solid waste, the trace elemental concentrations are under the criteria for hazardous material set by the TCLP and domestic method. The result seems to suggest that applying the recycled concrete on stream water will be accepatable practice as for as trace elements are concerned. However, the influence of inorganics such as Ca, Mg, Ni and $SO_4^{2-}$ on aquatic ecology should be further examined.

Study on Safety Management Plan through Chemical Accident Investigation in PCB Manufacturing Facility Etching Process (PCB 제조시설 에칭공정 화학사고 조사를 통한 안전관리 방안 연구)

  • Park, Choon-Hwa;Kim, Hyun-Sub;Jeon, Byeong-Han;Kim, Duk-Hyun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.4
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    • pp.132-137
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    • 2018
  • Although the number of chemical accidents has been declining since the Chemical Control Act of 2015, there have been repeated occurrences of similar types of accidents at printed circuit board (PCB) manufacturing facilities. These accidents were caused by the overflow of hydrochloric acid and hydrogen peroxide, which are toxic chemicals used in the printed circuit board manufacturing process. An analysis of the $Cl^-$ content to identify the cause of the accident showed that in the mixed route of hydrochloric acid and hydrogen peroxide, which are accidental substances, the $Cl^-$ concentration was 66.85 ppm in the hydrogen peroxide sample. Through reaction experiments, it was confirmed that the deformation of a PVC storage tank and generation of chlorine gas, which is a toxic gas, occurred due to reaction heat occurring up to $50.5^{\circ}C$. This paper proposes a facility safety management plan, including overcharge, overflow prevention, leak detection device, and separation tank design for mixing prevention in printed circuit board manufacturing facility etch process. To prevent the recurrence of accidents of the same type, the necessity of a periodic facility safety inspection and strengthening of the safety education of workers was discussed.

Accurate Analysis of Trace Phthalates and Method Validation in Cosmetics using Gas Chromatography with Mass Spectrometric Detection (화장품에 함유된 미량의 프탈레이트 함량을 정확히 분석하기 위한 가스크로마토그래피-질량분석 시험법 및 그 시험법의 유효성)

  • Kim, Min-Kee;Jeong, Hye-Jin;Cho, Jun-Cheol
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.38 no.1
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    • pp.33-41
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    • 2012
  • An effective, environmentally friendly analytic methods using gas chromatography with mass spectrometric detector (GC-MSD) have been developed for the quantitative analysis of trace phthalate levels in cosmetics such as nail lacquer and hair spray. Since such cosmetics are largely comprised of organic solvents, conventional clean-up methods that have been widely used for phthalate analyses are in adequate. In addition, analysis of trace phthalate levels is notorious for its sensitivity to contamination, which causes high analytical values. A direct sample dilution method using an organic solvent was adopted to the sample preparation process to determine the exact amounts of phthalates and simultaneously avoid the high risk of secondary contamination. The method has many advantages including high accuracy, sensitivity, and simplicity in sample preparation. Dibutyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) were selected for analysis because they have been frequently detected in cosmetics and consistently reported as endocrine disruptors in humans and animals. Internal standard method using two deuterium substitutes (DBP-$d_4$, DEHP-$d_4$) as the internal standard was also used. The results of 'Method validation' showed the capabilities of this method for the routine analysis of phthalates at the ppm level. The recovery ranges were between 95 % and 106.1 %, and relative standards deviations (RSD) were less than 3.9 % in fortified nail lacquer and hair spray samples at the concentration of $25{\mu}g/g$.