• Title/Summary/Keyword: sample pretreatment

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Determination of Copper in Uniformly-Doped Silicon Thin Films by Isotope-Dilution Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang;Cha, Myeong;Lee, Dong
    • Bulletin of the Korean Chemical Society
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    • v.22 no.2
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    • pp.205-209
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    • 2001
  • Uniformly-doped silicon thin films were fabricated by ion beam sputter deposition. The thin films had four levels of copper dopant concentration ranging between 1 ${\times}$1019 and 1 ${\times}$ 1021 atoms/cm3 . Concentrations of Copper dopants were determined by the isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) to provide certified reference data for the quantitative surface analysis by secondary ion mass spectrometry (SIMS). The copper-doped thin films were dissolved in a mixture of 1 M HF and 3 M HNO3 spiked with appropriate amounts of 65 Cu. For an accurate isotope ratio determination, both the detector dead time and the mass discrimination were appropriately corrected and isobaric interference from SiAr molecular ions was avoided by a careful sample pretreatment. An analyte recovery efficiency was obtained for the Cu spiked samples to evaluate accuracy of the method. Uncertainty of the determined copper concentrations, estimated following the EURACHEM Guide, was less than 4%, and detection limit of this method was 5.58 ${\times}$ 1016 atoms/cm3.

Evaluation of DNA Damage Using Microwave Dielectric Absorption Spectroscopy

  • Hirayama, Makoto;Matuo, Youichirou;Sunagawa, Takeyoshi;Izumi, Yoshinobu
    • Journal of Radiation Protection and Research
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    • v.41 no.4
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    • pp.339-343
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    • 2016
  • Background: Evaluation of deoxyribonucleic acid (DNA)-strand break is important to elucidate the biological effect of ionizing radiations. The conventional methods for DNA-strand break evaluation have been achieved by Agarose gel electrophoresis and others using an electrical property of DNAs. Such kinds of DNA-strand break evaluation systems can estimate DNA-strand break, according to a molecular weight of DNAs. However, the conventional method needs pretreatment of the sample and a relatively long period for analysis. They do not have enough sensitivity to detect the strand break products in the low-dose region. Materials and Methods: The sample is water, methanol and plasmid DNA solution. The plasmid DNA pUC118 was multiplied by using Escherichia coli JM109 competent cells. The resonance frequency and Q-value were measured by means of microwave dielectric absorption spectroscopy. When a sample is located at a center of the electric field, resonance curve of the frequency that existed as a standing wave is disturbed. As a result, the perturbation effect to perform a resonance with different frequency is adopted. Results and Discussion: The resonance frequency shifted to higher frequency with an increase in a concentration of methanol as the model of the biological material, and the Q-value decreased. The absorption peak in microwave power spectrum of the double-strand break plasmid DNA shifted from the non-damaged plasmid DNA. Moreover, the sharpness of absorption peak changed resulting in change in Q-value. We confirmed that a resonance frequency shifted to higher frequency with an increase in concentration of the plasmid DNA. Conclusion: We developed a new technique for an evaluation of DNA damage. In this paper, we report the evaluation method of DNA damage using microwave dielectric absorption spectroscopy.

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

  • Park, Sun-Young;Kang, Bo-Xin;Li, Quing;Kim, Hoon-Sik;Lee, Jun-Gae;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1497-1504
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    • 2009
  • GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

1D Proton NMR Spectroscopic Determination of Ethanol and Ethyl Glucuronide in Human Urine

  • Kim, Siwon;Lee, Minji;Yoon, Dahye;Lee, Dong-Kye;Choi, Hye-Jin;Kim, Suhkmann
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2413-2418
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    • 2013
  • Forensic and legal medicine require reliable data to indicate excessive alcohol consumption. Ethanol is oxidatively metabolized to acetate by alcohol dehydrogenase and non-oxidatively metabolized to ethyl glucuronide (EtG), ethyl sulfate (EtS), phosphatidylethanol, or fatty acid ethyl esters (FAEE). Oxidative metabolism is too rapid to provide biomarkers for the detection of ethanol ingestion. However, the non-oxidative metabolite EtG is a useful biomarker because it is stable, non-volatile, water soluble, highly sensitive, and is detected in body fluid, hair, and tissues. EtG analysis methods such as mass spectroscopy, chromatography, or enzyme-linked immunosorbent assay techniques are currently in use. We suggest that nuclear magnetic resonance (NMR) spectroscopy could be used to monitor ethanol intake. As with current conventional methods, NMR spectroscopy doesn't require complicated pretreatments or sample separation. This method has the advantages of short acquisition time, simple sample preparation, reproducibility, and accuracy. In addition, all proton-containing compounds can be detected. In this study, we performed $^1H$ NMR analyses of urine to monitor the ethanol and EtG. Urinary samples were collected over time from 5 male volunteers. We confirmed that ethanol and EtG signals could be detected with NMR spectroscopy. Ethanol signals increased immediately upon alcohol intake, but decreased sharply over time. In contrast, EtG signal increased and reached a maximum about 9 h later, after which the EtG signal decreased gradually and remained detectable after 20-25 h. Based on these results, we suggest that $^1H$ NMR spectroscopy may be used to identify ethanol non-oxidative metabolites without the need for sample pretreatment.

Quality Characteristics of Dolsan Leaf Mustard according to Various Blanching Conditions and Liquid Chromatography with Photodiode Array and Tandem Mass Spectrometry Analysis (다양한 데침조건에서 돌산갓의 이화학적 특성 및 LC-PDA/MS/MS 분석)

  • Son, Hae-Reon;Oh, Sun-Kyung;Tsukamoto, Chigen;Choi, Myeong-Rak
    • KSBB Journal
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    • v.31 no.1
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    • pp.20-26
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    • 2016
  • This study aims to examine the optimum blanching conditions as a pretreatment condition to improve the storage stability of Dolsan leaf mustard pickle. The effects of the blan- ching temperature and time were investigated at a temperature range of $80-100^{\circ}C$. Sampling was done for 1 month after a 5 days interval. The L value of the Dolsan leaf mustard was found to be the highest at $80^{\circ}C$. The cutting force increased as the blanching temperature increased. The tensile strength decreased at $95^{\circ}C$ and $100^{\circ}C$. In addition, the sensory evaluation scores were the best at $80^{\circ}C$. The storage stability was assessed at various blanching temperatures to increase the sinigrin content during storage. Liquid chromatography with photodiode array and tandem mass spectrometry (LC-PDA/MS/MS) analysis was conducted to identify and quantify the sinigrin content in the Dolsan leaf mustard. Sinigrin as an internal standard was co-injected into each sample solution. The sample was monitored by recording the ultraviolet absorbance at 228 nm and by electrospray ionization (ESI) positive ion mode in the m/z 50-1,500 range. Blanching the sample at $80^{\circ}C$ showed the highest sinigrin concentration during storage among various temperatures and the maximum concentration was 350 ppm at 15 days storage. Study on utilization of vegetable from food processing of leaf mustard and preservation conservation results suggest that blanching at $80^{\circ}C$ is expected to improve the palatability of the pickle.

A Study on the Pretreatment of BaTiOx Ceramics for the Analysis of Ba, Ti and W using Acid Digestion Bomb (가압 산분해법을 이용한 BaTiOx계 세라믹재료 중 Ba, Ti 및 W 분석을 위한 전처리 연구)

  • Park, Kyung-Su;Kim, Sun-Tae;Shim, Eui-Sup;Seo, Min-Jung;Lee, Seoung-Jae
    • Analytical Science and Technology
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    • v.15 no.1
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    • pp.15-19
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    • 2002
  • The pretreatment of tungsten added $BaTiO_x$ ceramics was performed to improve the recovery of Ba, Ti and W. $BaTiO_x$ ceramics were digested with HF : HCl ( 1 : 2 ) mixture in an acid digestion bomb at $220^{\circ}C$ for 3 hrs. The concentration of Ba, Ti and W were determined by ICP-AES. Recoveries of Ba, Ti and W were 99.6%, 99.8% and 99.2%, respectively. And their C.V. values were 1.02%, 0.73% and 1.79%. Using this method, the analytical results of Ba, Ti and W for a real sample were obainted to be 25.9% (w/w), 38.8% (w/w) and 3.31% (w/w), respectively.

Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC (HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구)

  • Oh, Bo Young;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.663-669
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    • 1999
  • For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

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Mean Platelet Volume as a Prognostic Marker in Metastatic Colorectal Cancer Patients Treated with Bevacizumab-Combined Chemotherapy

  • Tunce, Tolga;Ozgun, Alpaslan;Emirzeoglu, Levent;Celik, Serkan;Bilgi, Oguz;Karagoz, Bulent
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.15
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    • pp.6421-6423
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    • 2014
  • Background: Recent studies have revealed a prognostic impact of the MPV (mean platelet volume)/platelet count ratio in terms of survival in advanced non-small cell lung cancer. However, there has been no direct analysis of the survival impact of MPV in patients with mCRC. The aim of the study is to evaluate the pretreatment MPV of patients with metastatic and non-metastatic colorectal cancer (non-mCRC) and also the prognostic significance of pretreatment MPV to progression in mCRC patients treated with bevacizumab-combined chemotherapy. Materials and Methods: Fifty-three metastatic and ninety-five non-metastatic colorectal cancer patients were included into the study. Data on sex, age, lymph node status, MPV, platelet and platecrit (PCT) levels were obtained retrospectively from the patient medical records. Results: The MPV was significantly higher in the patients with mCRC compared to those with non-mCRC ($7.895{\pm}1.060$ versus $7.322{\pm}1.136$, p=0.013). The benefit of bevacizumab on PFS was significantly greater among the patients with low MPV than those with high MPV. The hazard ratio (HR) of disease progression was 0.41 (95%CI, 0.174-0.986; p=0.04). In conclusion, despite the retrospective design and small sample size, MPV can be considered a prognostic factor for mCRC patients treated with bevacizumab-combined chemotherapy.

Two-Step Oxidation of Refractory Gold Concentrates with Different Microbial Communities

  • Wang, Guo-hua;Xie, Jian-ping;Li, Shou-peng;Guo, Yu-jie;Pan, Ying;Wu, Haiyan;Liu, Xin-xing
    • Journal of Microbiology and Biotechnology
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    • v.26 no.11
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    • pp.1871-1880
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    • 2016
  • Bio-oxidation is an effective technology for treatment of refractory gold concentrates. However, the unsatisfactory oxidation rate and long residence time, which cause a lower cyanide leaching rate and gold recovery, are key factors that restrict the application of traditional bio-oxidation technology. In this study, the oxidation rate of refractory gold concentrates and the adaption of microorganisms were analyzed to evaluate a newly developed two-step pretreatment process, which includes a high temperature chemical oxidation step and a subsequent bio-oxidation step. The oxidation rate and recovery rate of gold were improved significantly after the two-step process. The results showed that the highest oxidation rate of sulfide sulfur could reach to 99.01 % with an extreme thermophile microbial community when the pulp density was 5%. Accordingly, the recovery rate of gold was elevated to 92.51%. Meanwhile, the results revealed that moderate thermophiles performed better than acidophilic mesophiles and extreme thermophiles, whose oxidation rates declined drastically when the pulp density was increased to 10% and 15%. The oxidation rates of sulfide sulfur with moderate thermophiles were 93.94% and 65.73% when the pulp density was increased to 10% and 15%, respectively. All these results indicated that the two-step pretreatment increased the oxidation rate of refractory gold concentrates and is a potential technology to pretreat the refractory sample. Meanwhile, owing to the sensitivity of the microbial community under different pulp density levels, the optimization of microbial community in bio-oxidation is necessary in industry.

Combination Pretreatment of Calcium and Vitamin C to Enhance the Firmness of Kimchi Sterilized with High-dose Gamma Irradiation

  • Song, Beom-Seok;Kim, Mi-Jung;Park, Jin-Gyu;Kim, Jae-Hun;Kim, Duk-Jin;Han, Sang-Bae;Shin, Jung-Kue;Byun, Myung-Woo;Lee, Ju-Woon
    • Food Science and Biotechnology
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    • v.17 no.4
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    • pp.751-754
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    • 2008
  • Texture analysis, sensory evaluation, and scanning electronic microscopic (SEM) observation were conducted to evaluate the effects of different calcium salts (calcium lactate, calcium acetate, and calcium chloride) and vitamin C on the textural properties of kimchi, gamma-irradiated at 25 kGy. Increase of the hardness and sensory score were observed in the kimchi pretreated with calcium salt or vitamin C as compared with the untreated and irradiated kimchi. And the hardness and sensory quality of the co-pretreated sample with 0.01% of calcium lactate and 0.3% of vitamin C were the highest after 30 days at $35^{\circ}C$, which indicates that the co-pretreatment is effective in preventing a decrease of the texture and sensory qualities of kimchi by gamma irradiation. Also, this result was supported by the SEM observation.