• Title/Summary/Keyword: method detection limit

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A New Analytical Method for the $Dy^{3+}$ Ion Using the Luminescence Enhancement by the Treatment of o-Phenanthroline on the TLC Plate (TLC Plate에서의 발광증폭 및 o-Phenanthroline에 의한 Energy Transfer를 이용한 $Dy^{3+}$ 이온의 미량 분석법)

  • Jeong, Hyuk
    • Analytical Science and Technology
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    • v.11 no.5
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    • pp.386-393
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    • 1998
  • A new analytical luminescence method for the $Dy^{3+}$ ion was studied using the luminescence enhancement by the treatment of the o-phenanthroline on the TLC plate. Compared to the specific emission intensities of the ion in water solution, if the ion solution is spotted on the TLC plate, the luminescence intensities were extremely enhanced. There was additional enhancement effect of the luminescence intensities of the ions on the TLC plate, if the ion on the TLC plate is treated with o-phenanthroline. Based on the luminescence enhancement, the detection limit was improved by more than 4 order of magnitude compared to that of solution sample. The dynamic ranges and correlation coefficients of the calibration curves near the detection limit were 102 order and ~0.99, respectively. The energy-transfer mechanism was explained for the theoretical back ground of the luminescence enhancement.

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Effective Concentration Method for Applying PCR to Detect Viruses in Water (수계바이러스검출에 PCR을 이용하기 위한 효과적인 농축기법)

  • 이승훈;김상종
    • Korean Journal of Microbiology
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    • v.35 no.1
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    • pp.41-46
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    • 1999
  • In detecting pathogeuic viruses in water sample, polymerase-chain-reaction (PCR) amplification was uscd. In order lo obtain the intact viral particlc, five concentration techniques were compared and an improved procedure was developed with some modifications. Among them, adsorption-elution~EG precipitation and flocculatio~~iultracentriEugation were more efficient than others with thc detection limit of 10 PFU $ml^{-1}$. By the additional step removing inhibitory compounds for PCR reaction, the purity of the concentrated sample was improved and the detection limit was lowered by one order (to 1 PFU $ml^{-1}$. To examine the availability of the optimized procedure for field surveys, the distributions of enterovirus in Han River were estimated using the novel procedure. Seventy-five percentage (618) of sewagc samples and twenty percentage (2110) of river water samples were positive for enterovirus. These results indicate that adsorption-elutionPEG precipitation by PCR method is useful for the prompt and handy monitoring of viral contaminaiton in water environment and pathogenic viruses are widely distributed in water environments of Seoul.

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Comparison of Blood Lead Concentration Using Graphite Furnace Atomic Absorption Spectrometry (GF-AAs) and Inductively Coupled Plasma-mass Spectrometry (ICP-MS) (흑연로 원자 흡광 광도법과 유도 결합 플라즈마 질량 분석법을 이용한 혈중 납 농도 비교)

  • Kang, Min-Kyung;Kwon, Jung-Yeon;Kim, Byoung-Gwon;Lim, Hyoun-Ju;Seo, Jeong-Wook;Kim, Yu-Mi;Hong, Young-Seoub
    • Journal of Environmental Health Sciences
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    • v.45 no.3
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    • pp.258-266
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    • 2019
  • Objectives: In this study, blood lead was analyzed using graphite furnace atomic absorption spectrometry (GF-AAs) and inductively coupled plasma mass spectrometry (ICP-MS). We tried to examine the difference and consistency of the analytical values and the applicability of the analytical method. Methods: We selected 57 people who agreed to participate in this study. After confirming the linearity of the calibration standard curves in GF-AAs and ICP-MS, the concentrations of lead in quality control material and samples were measured, and the degree of agreement was compared. Results: The detection limit of the ICP-MS was lower than that of GF-AAs. The coefficient of variation of reference materials was shown to be stable in the ICP-MS and GF-AAs. When the correspondence between the two equipments was verified by bias of the analysis values, a concordance was shown, and approximately 98% of the ideal reference lines were present within ${\pm}40%$ of the deflection. Conclusion: GF-AAs showed high sensitivity to single heavy metal analysis, but it took much time and showed higher detection limit than ICP-MS. Therefore, it would be considered necessary to switch to ICP-MS analysis method, considering that the level of lead exposure is gradually decreasing.

Stimultaneous Determination of Ephedrine Alkaloids in Ephedra sinica and Wolbigachul-tang by High Performance Liquid Chromatography (고성능 액체 크로마토그래피를 이용한 마황 및 월비가출탕 전탕액에서 에페드린류의 동시분석)

  • Song, Miyoung;Kim, Jung-Ok;Leem, HyunHee;Kim, Hojun
    • Journal of Korean Medicine for Obesity Research
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    • v.20 no.2
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    • pp.97-108
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    • 2020
  • Objectives: Ephedra sinica and Wolbigachul-tang which contains Ephedra sinica are used to treat obesity in Korean medicine. The aim of this study was to analyze the quantities of ephedrine alkaloids by high-performance liquid chromatography. Methods: The analysis was performed using a YMC-Triat C18 column with operating at 25℃, and UV detection at 210 nm. The mobile phase used a gradient flow with 0.1% H3PO4 in water and acetonitrile. Specificity, linearity, precision, accuracy, limit of detection, and limit of quantification were measured for validation anaylsis. This method was applied to analyze the quantities of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang. Results: The concentration per Ephedra sinica (gram) of ephedrine and pseudoephedrine in Ephedra sinica decoction are 4.74±0.22 mg and 2.19±0.10 mg, respectively and in Wolbigachul-tang decoction are 6.39±0.34 mg and 2.97±0.21 mg, respectively. The retention time of ephedrine was 23.6 min and that of pseudoephedrine was 25.8 min, and norephedrine and methylephedrine were not detected. Conclusions: In conclusion, analyzed the concentration of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang by the developed validation method.

High-Performance Liquid Chromatographic Determination of Tricyclazole Residues in Rice Grain, Rice Straw, and Soil

  • Lee, Young-Deuk;Lee, Jung-Hun
    • Applied Biological Chemistry
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    • v.41 no.8
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    • pp.595-599
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    • 1998
  • An analytical method was developed to determine tricyclazole residues in rice grain, straw, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Tricyclazole was extracted with methanol from moist rice grain, straw, and soil samples. n-Hexane washing was employed to remove nonpolar co-extractives during liquid-liquid partition. Tricyclazole was then extracted with dichloromethane from alkaline aqueous phase, while acidic interferences remained in the phase. Dichloromethane extract was further purified by silica gel column chromatography prior to HPLC determination. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate the tricyclazole residue in sample extracts monitored at ${\lambda}_{max}$ 225nm. Recoveries from fortified samples averaged $95.5{\pm}3.0%\;(n=6),\;87.5{\pm}20.%\;(n=6),\;and\;84.3{\pm}2.8%$ (n=12) for rice grain, straw, and soil, respectively. Detection limit of the method was 0.02 mg/kg for rice grain and soil samples while 0.05 mg/kg for rice straw samples. The proposed method was reproducible and sensitive enough to evaluate the safety of tricyclazole residues in rice grain, straw, and soil.

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Determination of Polychlorinated Biphenyls in the Soil by Perchlorination (염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석)

  • Moon, Moon,Chul-Ho;Choi, Choi,Sang-Ki;Kim, Kim,Jung-Ho
    • Journal of Environmental Science International
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    • v.4 no.3
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    • pp.97-97
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

Determination of Polychlorinated Biphenyls in the Soil by Perchlorination (염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석)

  • Moon, Moon, Chul-Ho;Choi, Choi, Sang-Ki;Kim, Kim, Jung-Ho
    • Journal of Environmental Science International
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    • v.4 no.3
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    • pp.249-258
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

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A New Chemiluminescence Method for Determination of Cytosine Arabinoside in Pharmaceutical Preparations

  • Cai, Z.;Zhang, X.;Lu, D.F.;Gan, J.N.
    • Bulletin of the Korean Chemical Society
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    • v.33 no.1
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    • pp.171-176
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    • 2012
  • A novel chemiluminescence (CL) system was established for the determination of cytosine arabinoside (Ara-C) in pharmaceutical preparations. It was showed that a clear CL signal was observed when Eosin Y mixed with Fenton reagent. The CL intensity was decreased significantly when Ara-C was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with the Ara-C concentration. Based on this, we developed a new method for the determination of Ara-C using a flow injection analysis (FIA) technique with CL detection. Under the optimal conditions, the linear range of Ara-C concentration was $6.0{\times}10^{-9}\sim1.0{\times}10^{-7}mol/L$ (R = 0.9982) with a detection limit of $7.6{\times}10^{-10}mol/L$ (S/N=3), the RSD was 5.6% for $6.0{\times}10^{-8}mol/L$ Ara-C (n = 11). The method was successfully applied to the determination of Ara-C in injection samples. The possible chemiluminescence reaction mechanism was discussed.

Improved High-Performance Liquid Chromatographic Method for the Determination of N-vanillyl-n-nonivamide(nonivamide) in Korean Hot Peppers (HPLC 법에 의한 국산 고추에 함유되어 있는 Nonivamide의 신규 분석법 개발)

  • Choi, Suk-Hyun
    • Journal of the East Asian Society of Dietary Life
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    • v.16 no.5
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    • pp.585-591
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    • 2006
  • We report a novel HPLC method for analyzing the capsaicinoids and nonivamide. The following conditions were used: a total column and column temperature of $3^{\circ}C$, a detection wavelength of 280 nm, an eluent containing acetonitrile : 0.5% formic acid(31:69, v/v). The experimental data was compared with standard nonivamide and capsaicin. The results showed that nonivamide was eluted in 96.7 minutes with a recovery ratio of 96.5% after adding known nonivamide. In addition, the detection limit for nonivamide was 18.6 ng. The capsaicinoids from Korean pepper were extracted (after blooming 60th) from 3 breeds cultivated in Korea, Buchon, Chungyang and Hanbando. and crisis it analyzed sympathizes the nonivamide in the result nonivamide from the Buchon and the Chungyang which are not detected from the Hanbando $0.16{\sim}0.24{\mu}g/g$ it detects with very small amount it contains it confirmed the each capsaicinoid with the HPLC and the LC-MS. These results are expected contribute to the quality control of various product processes, which includes product delivery inspection as well as examining the capsaicinoids present in the product for possible medicine manufacture and various foodstuff, and the nonivamide content, which may be a feed for various manufacturing processes involving chemical synthesis.

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Simple and Rapid Identification of Low Level Hepatitis B Virus DNA by the Nested Polymerase Chain Reaction

  • Jang, Jeong-Su;Lee, Kong-Joo
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.469-474
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    • 1996
  • A rapid and sensitive method has been developed to detect hepatitis B virus DNA (HBV) by nested polymerase chain reaction (PCR) technique with primers specific for the surface and core regions in capillary thermal cycler within 80 min. The lower limit for detection by present PCR method is $10^{-5}$ pg of recombinant HBV DNA which is equivalent to that determined by one round of PCR amplification and Southern blot hybridization analysis. When boiled HBV positive serum was serially diluted 10-fold, HBV DNA was successfully determined in $1{\mu}l-10^{-3}$ of serum. HBV DNA was detected by present method in 69 clinical samples including HBsAg positives and negatives by enzyme-linked immunosorbent assay (ELISA). When serum samples were amplified by nested PCR using surface and core region primers, HBV DNAs were detected in 37 of 69 samples (53.6%) and 18 of 69 samples (26.1%), respectively. These results can inform the infectious state of HBsAg positive pateints. A simple and rapid nested PCR protocol by using boiled serum as DNA template has been described for the clinical utility to determine HBV DNA in human serum.

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