• Title/Summary/Keyword: linearity analysis

Search Result 1,155, Processing Time 0.035 seconds

Sorption of PAHs by Soil Humins and Effect of Soil Inorganic Matrixs (PAHs의 토양휴민과의 흡착특성 및 토양 무기물의 영향 해석)

  • Lim, Dong-Min;Lee, Seung-Sik;Shin, Hyun-Sang
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.28 no.12
    • /
    • pp.1337-1346
    • /
    • 2006
  • Soil humin is the insoluble fraction of humic materials and play an important roles in the irreversible sorption of hydrophobic organic contaminants onto soil particles. However, there have been limited knowledge about the sorption and chemical properties of humin due to the difficulties in its separation from the inorganic matrix(mainly clays and oxides). In this study, de-ashed soil humins($Hu_1-Hu_6$) were isolated from a soil residues(Crude Hu) after removing alkali-soluble organic fractions followed by consecutive dissolution of the mineral matrix with 2%-HF for 2 hr. The humin samples were characterized by elemental analysis and $^{13}C$ NMR spectroscopic method and their sorption-desorption behavior for 1-naphthol were investigated from aqueous solution. The results were compared one another and that with peat humin. $^{13}C$ NMR spectra features indicate that the soil humin molecules are mainly made up of aliphatic carbons(>80% in total carbon) including carbohydrate, methylene chain. Freundlich sorption parameter, n was increased from 0.538 to 0.697 and organic carbon-normalized sorption coefficient(log $K_{OC}$) values also increased from 2.43 to 2.74 as inorganic matrix of the soil humin removed by HF de-ashing. The results suggest that inorganic phase in humin plays an important, indirect role in 1-naphthol sorption and the effects on the sorption non-linearity and intensity are analyzed by comparison between the results of soil humin and peat humin. Sorption-desorption hysteresis were also observed in all the humin samples and hysteresis index(HI) at low solute concentration($C_e$=0.1 mg/L) are in order of Peat humin(2.67)>De-ashed humin(0.74)>Crude Hu(0.59).

Determination of secondary aliphatic amines in surface and tap waters as benzenesulfonamide derivatives using GC-MS (Benzenesulfonamide 유도체로 GC-MS를 사용한 지표수 및 수돗물 중 2차 지방족 아민의 분석)

  • Park, Sunyoung;Jung, Sungjin;Kim, Yunjeong;Kim, Hekap
    • Analytical Science and Technology
    • /
    • v.31 no.2
    • /
    • pp.96-105
    • /
    • 2018
  • This study aimed to improve the method for detecting eight secondary aliphatic amines (SAAs), so as to measure their concentrations in fresh water and tap water samples. NaOH (8 mL, 10 M) and benzenesulfonyl chloride (2 mL) were added to a water sample (200 mL), and the mixture was stirred at $80^{\circ}C$ for 30 min. An additional NaOH solution (10 mL) was added and the stirring was continued for another 30 min. The pH of the cooled mixture was adjusted to 5.5-6.0 by adding HCl (35 %), and the SAAs were extracted using dichloromethane (50 mL). This extraction was repeated once. The extract was then washed with $NaHCO_3$ (15 mL, 0.05 M) and dried over $Na_2SO_4$ (4 g). The extract was finally concentrated to 0.1 mL, of which $1{\mu}L$ was analyzed for SAAs by GC-MS. The linearity of the spike calibration curves was high ($r^2=0.9969-0.9996$). The detection limits of the method ranged from 0.01 to $0.20{\mu}g/L$, and its repeatability and reproducibility (expressed as relative standard deviation) were both less than 10 % (6.6-9.4 %). Its accuracy (measured in percentage error) ranged between 2.4 % and 6.1 %. The established method was applied to the analysis of five surface water and 82 tap water samples. Dimethylamine was the only SAA detected in all the water samples, and its average concentration was $0.79{\mu}g/L$ (range: $0.20-2.54{\mu}g/L$). Therefore, this study improved the analytical method for SAAs in surface water and tap water, and the regional and seasonal concentration distributions were obtained.

Quantification of Odorants from Animal Husbandry using Solid-phase Microextraction (고상(固相) 미세 추출법에 의한 축산 관리시설에서 발생하는 악취성 가스 화합물의 정량적 평가)

  • Kim, Jae-Hyuck;Choi, Hong-Lim;Kown, So-Young;Lim, Hong-Lae;McConnell, Laura L.;Arispe, Susana;Park, Chul-Hwi;Kim, Hyun-Ook
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.28 no.2
    • /
    • pp.158-164
    • /
    • 2006
  • Offensive odor from CAFO(concentrated animal feeding operation) and its control have become a significant issue in Korea. Control of odors from the CAFO requires to identify major odorant and their generation mechanisms. In this study, an easy method to collect gas sample and to quantify its odorants is proposed. The method involves on-site odorant extraction with solid-phase microextraction and quantitation with GC/MSD or GC/FID. Analytes of the current study include: trimethylamine(TMA), carbon disulfide($CS_2$), dimethyl sulfide(DMS), dimethyl disulfide(DMDS), acetic acid(AA), propionic acid(PA) and n-butyric acid(BA). The resulting linearity($R^2$) of calibration curve for each analyte was good over the range from several ppbv to ppmv; 0.984 for TMA(0.056-1.437), 0.996 for $CS_2$(0.039-0.999), 0.994 for DMS(0.029-0.756), 0.995 for DMDS(0.024-0.623), 0.992 for AA(0.068-1.314), 0.955 for PA(0.047-0.940), and 0.976 for BA(0.036-0.712). Method detection limits were 5.67, 6.39, 5.78, 25.2, 0.098, 0.363 and 0.099 ppbv for AA, PA, BA, TMA, DMS, $CS_2$, and DMDS, respectively. With the developed method, odorants from poultry, swine, and cattle barns were analysed. All the compounds but DMDS were detected from the sample collected in the poultry barn, and their levels exceeded the representative published human olfactory threshold.

Simultaneous Determination of 8 Preservatives (6 Parabens, 2-Phenoxyethanol, and Chlorphenesin) in Cosmetics by $UPLC^{TM}$ ($UPLC^{TM}$를 이용한 화장품 중 보존제 8종(파라벤 6종, 페녹시에탄올, 클로페네신)의 동시분석)

  • Park, Jeong-Eun;Lee, So-Mi;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.33 no.4
    • /
    • pp.263-267
    • /
    • 2007
  • Parabens are used in nearly all types of cosmetics and toiletries because they are formulated well and have broad spectrum of activity, interness, low costs and excellent chemical stability in relation to pH. 2-phenoxyethanol and chlorphenesin are common preservatives which are usually used in combination with parabens in cosmetics. Toxicity of parabens is generally low but application of parabens to damaged or broken skin has resulted in sensitization. Moreover, the possibility of their estrogenic potential, anesthetic effects and reproductive toxicity has been reported. Consequently there are some regulations in use of parabens. And the maximum permitted concentrations of chlorphenesin and 2-phenoxyethanol in cosmetic products are authorized by the same reasons. So it is important to control and estimate the amount of parabens in products. In this article, we proposed a valid method for the simultaneous determination of 8 preservatives including parabens in a short time using ultra performance liquid $chromatography^{TM}\;(UPLC^{TM})$. Separation of eight components was achieved in less than 10 min and resolutions were reasonable (USP resolution ${\geqq}\;2$). And limit of detection and quantification were evaluated. The method was suitably validated for specificity, linearity, precision (repeatability, intermediate precision) and accuracy for assay (recovery) based on International conference on harmonisation (ICH) guideline. The method was applicable to analysis of preservatives in cosmetic products.

Simultaneous HPLC Determination of Marker Compounds for the Standardization of Hedyotis diffusa (백운풀의 지표성분 설정 및 품질표준화를 위한 정량 분석법)

  • Bang, Han-Yeol;Yang, Eun-Ju;Kim, Jeong-Ah;Song, Kyung-Sik
    • Journal of Life Science
    • /
    • v.23 no.8
    • /
    • pp.1025-1031
    • /
    • 2013
  • From a 95% ethanolic extract of H. diffusa, four marker compounds (HD1~HD4) were isolated, which were relatively unique and exist in comparably high contents. The structures of marker compounds were identified as digitolutein (1), 2-hydroxy-3-methylanthraquinone (2), (E/Z)-6-O-p-coumaroyl scandoside methyl ester (4:1 mixture) (3), and (E/Z)-6-O-p-methoxycinnamoyl scandoside methyl ester (4:1 mixture) (4), respectively, on the basis of $^{13}C$ and $^1H$-NMR analyses. The calibration curves of marker compounds showed high linearity, as their correlation coefficient ($R^2$) were in the range of 0.9991~0.9999. In addition, the limit of detection (LOD) and the limit of quantification (LOQ) were $0.03{\sim}0.07{\mu}g/ml$ and $0.099{\sim}0.231{\mu}g/ml$, respectively. The intra-day/inter-day precision and accuracy were 0.23~2.00%/0.25~1.16% and 94.60~108.44%/94.73-110.23%, respectively. The optimal HPLC conditions for the simultaneous quantification of HD1~HD4 were as follows: stationary phase; Merck Chromolith RP-18e ($100{\times}4.6mm$, $5{\mu}m$), column temp.; room temperature, UV detection at 280 nm, flow rate; 2.0 ml/min, injection volume; $10{\mu}l$, mobile phase; start with the mixture of 80% solvent A ($H_2O$ containing 0.5% acetic acid) and 20% solvent B (methanol containing 0.5% acetic acid) and gradually decrease solvent A to 40% in 9 min., then retain this condition to 18 min. Under the HPLC condition, the four marker compounds 1~4 were successfully separated without any interference of other constituents. The results obtained in this study are expected to be helpful for the development of nutraceutics and natural medicines and for the quality control of this plant.

Analysis of Image Processing Characteristics in Computed Radiography System by Virtual Digital Test Pattern Method (Virtual Digital Test Pattern Method를 이용한 CR 시스템의 영상처리 특성 분석)

  • Choi, In-Seok;Kim, Jung-Min;Oh, Hye-Kyong;Kim, You-Hyun;Lee, Ki-Sung;Jeong, Hoi-Woun;Choi, Seok-Yoon
    • Journal of radiological science and technology
    • /
    • v.33 no.2
    • /
    • pp.97-107
    • /
    • 2010
  • The objectives of this study is to figure out the unknown image processing methods of commercial CR system. We have implemented the processing curve of each Look up table(LUT) in REGIUS 150 CR system by using virtual digital test pattern method. The characteristic of Dry Imager was measured also. First of all, we have generated the virtual digital test pattern file with binary file editor. This file was used as an input data of CR system (REGIUS 150 CR system, KONICA MINOLTA). The DICOM files which were automatically generated output files by the CR system, were used to figure out the processing curves of each LUT modes (THX, ST, STM, LUM, BONE, LIN). The gradation curves of Dry Imager were also measured to figure out the characteristics of hard copy image. According to the results of each parameters, we identified the characteristics of image processing parameter in CR system. The processing curves which were measured by this proposed method showed the characteristics of CR system. And we found the linearity of Dry Imager in the middle area of processing curves. With these results, we found that the relationships between the curves and each parameters. The G value is related to the slope and the S value is related to the shift in x-axis of processing curves. In conclusion, the image processing method of the each commercial CR systems are different, and they are concealed. This proposed method which uses virtual digital test pattern can measure the characteristics of parameters for the image processing patterns in the CR system. We expect that the proposed method is useful to analogize the image processing means not only for this CR system, but also for the other commercial CR systems.

A Study on Migration of Ethylenediamine and Hexamethylenediamine from Polyamide Utensils (Polyamide 조리기구로부터 Ethylenediamine 및 Hexamethylenediamine의 이행에 관한 연구)

  • Eom, Mi-Ok;Kwak, In-Shin;Yoon, Hae-Jung;Jeon, Dae-Hoon;Choi, Hyun-Chul;Kim, Hyung-Il;Sung, Jun-Hyun;Park, Na-Young;Kim, So-Hee;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
    • /
    • v.25 no.1
    • /
    • pp.36-42
    • /
    • 2010
  • The method for the determination of ethylenediamine (EDA) and hexamethylenediamine (HMDA) in food simulants was developed, and migration amounts of these compounds was monitored for 124 polyamide (PA) utensils. The diurethane derivatives of EDA and HMDA, which produced by reaction with ethyl chloroformate, were analyzed by using gas chromatograph (GC)/flame ionization detector (FID) and GC/mass spectrometer (MS). The developed method was validated with $0.3\;{\mu}g/mL$ of limit of detection (LOD) for EDA and $0.1\;{\mu}g/mL$ of LOD for HMDA, > 0.999 of linearity($r^2$) and > 88% of recovery. The EDA was detected 1.31 and $02.06\;{\mu}g/mL$ for 2 samples in water. The HMDA was detected $0.29\;-\;0.93\;{\mu}g/mL$ for 3 samples in 20% ethanol and $0.26\;-\;0.44\;{\mu}g/mL$ for 10 samples in n-heptane. These migration levels were below the specific migration limits (SML) of $12\;{\mu}g/mL$ and $2.4\;{\mu}g/mL$ for EDA and HMDA established in EU.

Simultaneous Determination of UV Absorbers Migrated from Polyethylene and Polypropylene Food Packaging Materials into Food Simulants by HPLC-UVD (HPLC-UVD를 이용한 폴리에틸렌, 폴리프로필렌 기구 및 용기·포장 유래 자외선흡수제 동시분석법)

  • Choi, Heeju;Choi, Jae Chun;Bae, In-Ae;Lee, Chanyong;Park, Se-Jong;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
    • /
    • v.32 no.5
    • /
    • pp.434-442
    • /
    • 2017
  • The UV light in sunlight breaks down the chemical bonds in a polyolefin polymer through a process called photodegradation, ultimately causing cracking, chalking, colour changes, and loss of physical properties such as impact strength, tensile strength, elongation, and others. UV absorbers are used to prevent or terminate the oxidation of plastics by UV light. They are receptive to UV radiation and dissipate the energy harmlessly as heat. Benzotriazoles and benzophenones are used mainly in polyolefins such as polyethylene and polypropylene. In this study, we have developed a method for the analysis of 12 UV absorbers, which are Uvinul 3000, Cyasorb UV 24, Uvinul 3040, Tinuvin 312 and P, Seesorb 202, Chimassorb 81, Tinuvin 329, 234, 326, 328 and 327, migrated from the food packaging materials into four food simulants for aqueous, acidic, alcoholic and fatty foods. The UV absorbers in food simulants were determined by reversed-phase high performance liquid chromatograph-ultraviolet detector with 310 nm after solid-phase extraction with a hydrophilic-lipophilic balance (HLB) cartridge or dilution with isopropanol. The analytical method showed a good linearity of coefficient ($R^2{\geq}0.99$), limits of detection (0.049~0.370 mg/L), and limits of quantification (0.149~1.120 mg/L). The recoveries of UV absorbers spiked to four food simulants ranged from 70.05% to 110.13%. The developed method would be used as a reliable tool to determine concentrations of the migrated UV absorbers.

Establishment of an Analytical Method for Novobiocin in Livestock Products Using HPLC-UVD (HPLC-UVD를 이용한 축산식품 중 Novobiocin의 시험법 확립)

  • Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
    • /
    • v.44 no.3
    • /
    • pp.263-268
    • /
    • 2012
  • Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.

Determination of the Levels of Bisphenol A Diglycidyl Ether (BADGE), Bisphenol F Diglycidyl Ether (BFDGE) and Their Reaction Products in Canned Foods Circulated at Korean Markets (캔 제품의 bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE) 유도체 및 분해산물 분석법)

  • Kim, Hee-Yun;Lee, Jin-Sook;Cho, Min-Ja;Yang, Ji-Yeon;Baek, Ji-Yun;Cheong, So-Young;Choi, Sun-Hee;Kim, Young-Seon;Choi, Jae-Chun
    • Korean Journal of Food Science and Technology
    • /
    • v.42 no.1
    • /
    • pp.8-13
    • /
    • 2010
  • Bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE) were obtained by a polymerization reaction of epichlorohydrin (ECH) with bisphenol A (BPA) or bisphenol F (BPF). These compounds are commonly used as monomers or additives such as a polymerization stabilizer and a hydrochloric acid scavenger of epoxy resin, polyvinyl chloride (PVC)-containing organosols and polyester lacquers, that are applied to the internal surface of most canned foods to impart chemical resistance. The unreacted BADGE, BFDGE and their reaction products migrating from epoxy resin, PVC-containing organosol and/or polyester lacquer-based food packaging materials into the foods have recently become an issue of great concern because of increased customer demand for safety. This study was conducted to develop a rapid and sensitive simultaneous analysis method based on HPLC/FLD and HPLC/APCI-mass and to evaluate the concentration of BADGE, BFDGE and their metabolites, BADGE $H_2O$, BADGE $2H_2O$, BADGE HCl, BADGE 2HCl, BADGE HCl $H_2O$, BFDGE $H_2O$, BFDGE $2H_2O$, BFDGE HCl, BFDGE 2HCl and BFDGE HCl $H_2O$ for 133 canned food samples. The method provided a linearity of 0.9997-0.9999, a limit of detection of $0.01-0.13\;{\mu}g/mL$, a limit of quantitation of $0.03-0.44\;{\mu}g/mL$ and a recovery (%) of 85.64-118.18. The number of samples containing BADGE, BFDGE or their metabolites were: 28/133 (21.1%), with levels of 0.400-0.888 mg/kg being observed for aqueous foods (19/133) and 0.093-0.506 mg/kg being observed for oily foods (9/133).