• Title/Summary/Keyword: 상대표준편차

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Analysis and Monitoring of Aflatoxin M1 in Milks (우유 중 아플라톡신 M1 오염도 조사연구)

  • Park, Sung-Kug;Kang, Young-Woon;Kwon, Ki-Sung;Lee, Gwang-Ho;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.44 no.2
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    • pp.247-250
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    • 2012
  • Raw milk samples (n=28) obtained from milk tanks in 3 dairy plants of different regions and commercial milks (n=100) were collected from six cities. These samples were analyzed for the level of aflatoxin $M_1$ contamination using immunoaffinity columns and high performance liquid chromatography coupled with fluorescent detectors. Confirmation of aflatoxin $M_1$ ($AFM_1$) identified in positive samples was based on the formation of the hemiacetal derivative ($AFM_{2a}$) after derivatization with trifluroacetic acid. The average concentrations of aflatoxin $M_1$ in the raw milks were 25.1 ng/kg, and those values in commercial milks were 29.8 ng/kg. The highest level of aflatoxin $M_1$ in milk was 72.7 ng/kg. These results showed that the contamination of aflatoxin $M_1$ in milks consumed in the Korea was quite low compared to the standard in Korea Food Code (aflatoxin $M_1$ 500 ng/kg).

Multicomponent pesticides analysis by automated liquid phase microextraction (자동화된 LPME(Liquid Phase Microextraction)장치를 이용한 다성분 농약분석)

  • Myung, Seung-Woon;Jung, Hong-Rae
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.224-231
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    • 2005
  • In this study, the optimum conditions for the LPME (liquid phase microextraction) were investigated to overcome several shortcomings of traditional liquid-liquid extraction method. The LPME, which is automatic and dynamic, was used to analyze the five pesticides (dementon-S-methyl, diazinon, parathion, fenitrothion, EPN) extracted from vegetable, and HP 6890 GC/NPD was used as an analytic instrument. It was possible to optimize the extraction condition using the automatic LPME. The optimum extraction rate was obtained at pH 3.0 and $100{\mu}g/mL$ of salt concentration and standard curve showed linearity with over $R^2=0.9921$ in the range of $0.2{\sim}10{\mu}g/g$. The relative standard deviations were 7.7%, 9.8%, 7.8%, 9.7% and 8.2% in the $5.0{\mu}g/g$ concentration of dementon-S-methyl, diazinon, parathion, fenitrothion and EPN, respectively. The acquired accuracies were satisfactory showing 12.7%, 7.8%, 10.4%, -6.7% and -0.7% for dementon-S-methyl, diazinon, parathion, fenitrothion and EPN respectively.

Flow Injection Spectrophotometric Determination of Cobalt with 2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)aniline (2-(5-브로모-2-피리딜아조)-5-(N-프로필-N-슬포프로필아미노)아닐린을 사용하여 흐름주입법에 의한 코발트의 분광광도법적 정량)

  • Kang, Sam Woo;Kim, In Yong;Han, Hong Seok;Lee, Seung Seok
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.57-63
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    • 1993
  • Spectrophotometric determination of cobalt by flow injection method is described. 2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino) aniline rapidly forms a water-soluble complex with cobalt in $NH_3-NH_4Cl$ buffer solution at pH 10.5. The absorption maxima of this complex is at 545 nm with molar absorptivity of $58000L\;mol^{-1}\;cm^{-1}$. The calibration curve of cobalt is linear over the range of 0.1 to 0.6ppm and the detection limit is 25ppb. The relative standard deviation is ${\pm}0.72%$ for 0.5ppm and the sampling rate is $60samples\;hr^{-1}$. The interfering effect of some cations and anions was investigated. Ni(II), Cu(II), Fe(III) and $CN^-$ interfered severely. The interfering effect of these matallic ions could be decreased by adding $1.0{\times}10^{-3}M$ EDTA solution to the carrier stream.

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Simultaneous analysis and occurrences of six pharmaceuticals in surface water by LC/ESI-MS/MS (LC/ESI-MS/MS를 이용한 하천수 중 잔류 6종 의약물질의 동시분석 및 모니터링)

  • Kim, Byung-Ju;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.572-578
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    • 2010
  • The extraction/clean-up and concentrating of pharmaceuticals from surface water were performed by HLB (Hydrophilic-Lipophilic Balanced) cartridge. The method allows for the simultaneous determination of six pharmaceuticals by HPLC/ESI(+)-MS/MS. Recoveries of the pharmaceutical were between 71.1 to 92.6% (except fenbendazole) and the overall variability of the method was below 11.2% (RSD). The calibration curves for the pharmaceuticals from blank surface water showed good linearities (above $r^2$ = 0.99) in the concentration range of 0.007~1.2 ng/mL. The limit of detection (LOD) and the limit of quantification (LOQ) were 7.2~128.7 pg/mL and 23.8~429.1 pg/mL, respectively. The present analytical method can be useful for monitoring residual pharmaceuticals in surface water and other aquatic samples. High concentrations of iopromide and fenbendazole were detected in a few samples of surface water.

Optimization of analytical conditions for the determination of nitrosamines in chlorinated tap water by high performance liquid chromatography (액체크로마토그래피를 이용한 수돗물 중 nitrosamine 화합물 분석의 최적화)

  • Han, Ki-Chan;Kim, He-Kap
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.551-559
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    • 2010
  • This study was conducted to establish an analytical method for the determination of seven nitrosamines in chlorinated tap water by precolumn derivatization followed by high performance liquid chromatography coupled with fluorescence detection. The derivatization procedure was optimized for denitrosation and dansylation, and then two extraction methods, liquid-liquid extraction (LLE) with dichloromethane and solid phase extraction (SPE), were compared. The SPE method employing the optimized derivation procedure showed higher extraction recovery (54.4-88.7%) and reproducibility (1.9-19.4%) than the LLE method (51.4-87.7% and 4.2-33.3%, respectively). The method detection limits were between 0.5 and 4.4 ng/L. When chlorinated water samples were collected from two treatment plants and ten household taps, and analyzed for nitrosamines, Nnitrosodimethylamine (NDMA) was the major compound found between 26.1 and 112 ng/L.

Square-Wave Anodic Stripping Voltammetric Study of Germanium(Ⅳ)-Morin Complex (Germanium(Ⅳ)-Morin 착물에 대한 네모파 양극벗김 전압전류법적 연구)

  • Sohn, Se Chul;Park, Yong Joon;Joe, Kih Soo
    • Journal of the Korean Chemical Society
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    • v.41 no.11
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    • pp.590-593
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    • 1997
  • Square-wave anodic stripping voltammetry was applied to the germanium(IV)- Morin complex in 0.5 M sulfuric acid as a supporting electrolyte. The peak potential appeared at - 0.606 V vs. Ag/AgCl. Effects of sulfuric acid concentration, Morin concentration, accumulation potential, and accumulation time on the stripping peak current for the complex of germanium(IV)-Morin were studied. Interferences by other metal cations that affect on stripping peak current were also investigated. The detection limit was found to be $3.76{\times}10^{-7}M(27 {\mu}g/L)$ for germanium(IV) using 60 seconds of accumulation time. The relative standard deviation (n=8) for 0.4 mg/L($5.5{\times}10^{-6}$ M) germanium(IV) was 3.2%.

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Studies on the Development of Liquid Chromatographic Methods for Pesticide Residues (II) : The Development of the Analytical Method for Thiocarbamates Herbicides (잔류농약의 액체 크로마토그래피 분석법 개발에 관한 연구 (II) Thiocarbamates 제초제의 잔류농약 분석법 개발)

  • Lee Dai Woon;Choi Yong Wook
    • Journal of the Korean Chemical Society
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    • v.36 no.1
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    • pp.66-74
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    • 1992
  • A method for the multiresidual simultaneous analysis of 11 thiocarbamates was studied using HPLC. Thiocarbamate in Chinese cabbage was analyzed in the order of extraction, partition, and cleanup in their optimum condition. Acetone was chosen as an extracting solvent. As a partitioning solvent, the mixture of 50% methylene chloride and petroleum ether containing extremely small water content showed good recoveries of thiocarbamate from the water layer. Partition efficiency was affected by pH of the water layer; it remained almost constant under the acidic and neutral condition while decreasing under the basic condition. The comparison done in cleanup step showed that the column chromatographic method is superior to the treatment of coagulating reagent. As an absorbent, the mixture of charcoal, magnesia, and celite with the ratio of 1 : 2 : 4 gave better recoveries and also effectively removed chlorophyll. Over the total procedure, the average recoveries for thiocarbamates in Chinese cabbage were 91% at about 2 ppm fortification level within the relative standard deviation of 8%, and the minimum detection limit (MDL) was 2.2${\sim}$9.3 ng.

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A Study on the Evaluation Methods of Residual Flux Cleaning Ability by Alternative Semi-Aqueous Cleaners Using Metal Test Tools After Soldering with Solder Paste (솔더페이스트로 솔더링 후 잔류 플럭스 오염물에 대한 준수계 세정제의 금속치구를 이용한 세정성능 평가방법 연구)

  • Lee, Dong-Kee
    • Clean Technology
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    • v.14 no.2
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    • pp.103-109
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    • 2008
  • In this study, in order to develop evaluation method of the cleaning efficiency of residual flux which remains on the surface after soldering with solder paste, a specially designed metal tool is used to reduce spread uncertainty of flux while soldering. Using this tool, the measurement of cleaning efficiency of flux after soldering for some typical alternative semi-aqueous cleaners and 1,1,1-TCE by weighing method was conducted. As the test result of cleaning efficiency for each cleaner at several different cleaning times, the precision of the data is confirmed to within about 4% relative standard deviation (RSD) range. So, it is considered that this would be a good evaluation method for evaluating the cleaning efficiency of the residual flux which remains after solder paste soldering in the alternative cleaning. The results of this test method shows that the cleaning efficiency of ST 100SX and Neozal 750H in the cleaning of residual flux was better than other semi-aqueous cleaners, but its cleaning efficiency was clearly inferior to 1,1,1-TCE.

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Spectrofluorimetric Determination of Pb ion in Aqueous Media Using an Optical Sensor (광센서를 이용한 수용액 중 납이온의 형광분광법적 정량)

  • Lee, Sang Hak;Seo, Hyo Suk
    • Journal of the Korean Chemical Society
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    • v.46 no.5
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    • pp.407-411
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    • 2002
  • A method to determine lead ion in aqueous media using an optical sensor loaded on a fluorescent optode membrane incoporating a metal ion-selective ionophore, a proton-selective chromoionophore and lipophilic anionic sites has been studied. The effects of pH and thickness of membrane on the fluorescence intensity were investigated. The effects of foreign ions such as $Na^+$, $K^+$, $Mn^{2+}$ and $Zn^{2+}$ on the determination of lead ion were also studied. The linear range in the calibration curve for the determination of lead ion was found to be 5.0${\times}10^-7$ to 5.0${\times}$$10^-3$M and the correlation coefficient in this range was -0.99107 under the optimal experimental conditions. The relative standard deviation of the blank signals was 3.0% and the detection limit of lead ion was 5.0${\times}$$10^-9$M.

Extraction-Spectrophotometric Determination of Cimetidine in Pharmaceutical Samples as an Ion Pair with Bromothymol Blue (티몰블루와 함께 이온쌍으로서 약제 샘플에서 시메티딘의 추출-분광광도 측정)

  • Zargar, B.;Pourreza, N.;Shahrouz, M.
    • Journal of the Korean Chemical Society
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    • v.55 no.1
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    • pp.46-49
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    • 2011
  • A highly sensitive and selective extraction-spectrophotometric method has been developed for determination of trace amounts of cimetidine. This method is based on the extraction of cimetidine as an ion pair with bromothymol blue (BTB) into chloroform and measuring its absorbance at 417 nm. The effect of different variables such as pH, concentration of BTB, volume of chloroform and shaking time was investigated. The effect of interfering ions on the extraction was also studied. The calibration curve was linear in the range of 0.25-8 ${\mu}gmL^{-1}$ with correlation coefficient of 0.9997. The detection limit based on 3Sb was 0.14 ${\mu}gmL^{-1}$ and relative standard deviation for 10 replicated measurements of 1.0 and 4.0 ${\mu}gmL^{-1}$ of cimetidine was 3.2 and 1.49%, respectively. The proposed method was applied to the determination of cimetidine in pharmaceutical samples with good recoveries.