• Title/Summary/Keyword: Quantification analysis

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Development of analytical method for determination of spinetoram residues in livestock using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 Spinetoram 공정시험법 개발 및 검증)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun Hyang;Ju, Yun Ji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.29 no.2
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    • pp.94-103
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    • 2016
  • An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r2 > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.

Development of an Analytical Method for the Determination of Pyriofenone residue in Agricultural Products using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 살균제 pyriofenone 분석법 확립)

  • Park, Hyejin;Kim, HeeJung;Do, Jung-Ah;Kwon, Ji-Eun;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.18 no.2
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    • pp.79-87
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    • 2014
  • Pyriofenone is an aryl phenyl ketone fungicide that is newly registered in Korea in 2013 to control powdery mildew on food. The objective of this study was to develop reliable and sensitive analytical method for determination of pyriofenone residue in agricultural products for ensuring the food safety. The pyriofenone residues in all samples(Korean melon, pepper, potato, mandarin, soybean, and hulled rice) were extracted with acetonitrile, partitioned with dichloromethane, and then purified with a silica cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of pyriofenone was 0.05~5 mg/kg with the correlation coefficient ($r^2$) > 0.999. Average recoveries of pyriofenone ranged from 72.8% to 99.5% at the spiked level of 0.05 and 0.5 mg/kg, while the relative standard deviation was 2.3%~6.4%. In addition, the limit of detection and limit of quantification were 0.01 and 0.05 mg/kg, respectively. The results revealed that the developed and validated analytical method was suitable for pyriofenone determination in agricultural products.

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
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    • v.28 no.2
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    • pp.158-164
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    • 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
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    • v.33 no.4
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    • pp.263-267
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    • 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.

Varietal Analysis and Quantification of Resveratrol in Mulberry Fruits (뽕나무 계통별 오디의 레스베라트롤 함량 분석)

  • Kim Hyun-Bok;Kim Jung-Bong;Kim Sun-Lim
    • Journal of Sericultural and Entomological Science
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    • v.47 no.2
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    • pp.51-55
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    • 2005
  • Resveratrol is naturally occurring phytoalexin compounds produced by grape berries, peanuts, and their products in response to stress such as fungal infection, heavy metal ions or UV irradiation. The objective of this study was to develope a reliable high performance liquid chromatographic (HPLC) method for the quantitative determination of trans-resveratrol in mulberry fruit. Samples were extracted in 80% MeOH and filtered with $0.45{\mu}m$ syringe filter. The transresveratrol was separated Waters $C_{18}$ column, using a mobile phase containing 0.025% trifluroacetic acid in 5% acetonitril and 0.035% trifluroacetic acid in 50% acetonitril, detected by photodiode array detector (PDA) at 254 nm and the flow rate was 1ml/min. Under this analytical condition, the mean content of mulberry fruits (fifty varieties) was $777.3{\pm}585.9ppm$. Among the tested samples, 'Mansaengbaekpinosang (II)' was the highest level in 3450.6 ppm. However four accessions including 'Gukbu', 'Sabangso (I)', 'Simseol' and yield mulberry fruit were not able to detected. Eight suitable varieties selected for the production of fruit were 'Jeolgokchosaeng (Chungbuk)' 777.8 ppm, 'Dangsang 7' 771.1 ppm, 'Jangsosang' 133.9 ppm, 'Susungppong' 31.1 ppm, 'Suwonnosang' 639.7 ppm, 'Palcheongsipyung' 1475.9 ppm, 'Kangsun' 864.0 ppm, and 'Jukcheonchosaeng' 1458.5 ppm. 'Daesungppong' which was the first authorized variety for the production of mulberry fruit was 1236.7 ppm. In conclusion, these results suggest that mulberry including fruit and leaf may a good new resource for resveratrol production.

EFFECT OF ENAMEL MATRIX DERIVATIVE (EMD, $EMDOGAIN^{(R)}$) ON THE DIFFERENTIATION OF CULTURED HUMAN PERIODONTAL LIGAMENT CELLS AND MESENCHYMAL STEM CELLS (배양된 사람 치주인대세포와 골수유래간엽줄기세포의 분화에 미치는 법랑기질유도체 (Enamel Matrix Derivative, EMD)의 영향)

  • Park, Sang-Gyu;Jue, Seong-Suk;Kwon, Yong-Dae;Choi, Byung-Joon;Kim, Young-Ran;Lee, Baek-Soo
    • Maxillofacial Plastic and Reconstructive Surgery
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    • v.31 no.4
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    • pp.281-286
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    • 2009
  • Introduction: Enamel matrix derivative (EMD) is a protein which is secreted by Hertwig root sheath and plays a major role in the formation of cementum and attachment of peridontium. Several studies have shown that EMD promoted the proliferation and differentiation of preosteoblasts, osteoblasts and periodontal ligament cells in vitro: however, reports showing the inhibition of osteogenic differentiation by EMD also existed. This study was designed to simultaneously evaluate the effect of EMD on the two cell lines (human mesenchymal stem cells: hMSC, human periodontal ligament derived fibroblasts: hPDLCs) by means of quantitative analysis of some bone related matrices (Alkaline phosphatase : ALP, osteopontin ; OPN, osteocalcin ; OC). Materials and Methods: hMSCs and hPDLCs were expanded and cells in the 4${\sim}$6 passages were adopted to use. hMSc and hPDLCs were cultured during 1,2,7, and 14 days with 0, 50 and 100 ${\mu}g/ml$ of EMD, respectively. ALP activity was assessed by SensoLyte ALP kit and expressed as values of the relative optical density. Among the matrix proteins of the bony tissue, OC and OPN were assessed and quantification of these proteins was evaluated by means of human OC immunoassay kit and human OPN assay kit, respectively. Results: ALP activity maintained without EMD at $1,2^{nd}$ day. The activity increased at $7^{th}$ day but decreased at $14^{th}$ day. EMD increased the activity at $14^{th}$ day in the hPDLCs culture. In the hMSCs, rapid decrease was noted in $7^{th}$ and $14^{th}$ days without regard to EMD concentrations. Regarding the OPN synthesis in hPDLCs, marked decrease of OPN was noted after EMD application. Gradual decrease tendency of OPN was shown over time. In hMSCs, marked decrease of OPN was also noted after EMD application. Overall concentration of OPN was relatively consistent over time than that in hPDLCs. Regarding the OC synthesis, in both of hPDLCs and hMSCs, inhibition of OC formation was noted after EMD application in the early stages but EMD exerted minimal effect at the later stages. Conclusion: In this experimental condition, EMD seemed to play an inhibitory role during the differentiation of hMSCs and hPDLCs in the context of OC and OPN formation. In the periodontium, there are many kinds of cells contributing to the regeneration of oral tissue. EMD enhanced ALP activity in hPDLCs rather than in hMSCs and this may imply that EMD has a positive effect on the differentiation of cementoblasts compared with the effect on hMSCs. The result of our research was consistent with recent studies in which the authors showed the inhibitory effect of EMD in terms of the differentiation of mineral colony forming cells in vitro. This in vitro study may not stand for all the charateristics of EMD; thus, further studies involving many other bone matrices and cellular attachment will be necessary.

Quantification of Isoflavone Malonylglucosides in Soybean Seed during Germination (콩 발아 중 isoflavone malonylglucosides의 함량 변이)

  • Lee, Ju-Won;Yi, Yoo-Jung;Lee, Ju-Hee;Jo, Min-Sik;Choi, Do-Jin;Ma, Mu-Hyun;Kim, Hong-Sik;Kim, Dae-Ok;Yun, Hong-Tae;Kim, Yong-Ho
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.63 no.3
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    • pp.239-247
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    • 2018
  • Soybean produces three major types of isoflavones, daidzein, genistein, and glycitein aglycones and their glucosides and malonylglucosides. It has been known that malonylated glucosides are rapidly converted to their corresponding aglycones due to the unstable thermolabile glucoside malonates; therefore, the analytical study of malonylated glucosides has been insufficient. In this study, we analyzed the malonylglucoside content in soybean seeds. Isoflavone analysis of three soybean cultivars revealed that 81.5~90.0% of the total isoflavones were malonylglucosides, whereas aglycones were rarely detected. Moreover, the total isoflavone content increased during a 5-day germination period where growth regulators and coumaric acid treatments tended to yield higher isoflavone content than the normal germination treatment, however the differences were not significant; notably, the isoflavone accumulation trend continued with additional germination days. The content of malonylglucoside was higher than that of other isoflavones, which was 83.7~86.6% of the total isoflavone content in seeds with a 3-day germination period. Furthermore, isoflavones were significantly accumulated in the hypocotyl of seedlings with a 5-day germination period. The content of isoflavone in the hypocotyl of the Pungsannamul-kong was 10,240 ug/g when treated with coumaric acid, which was considerably higher than that of other cultivars and treatments. Additionally, soybean seeds heated at $60^{\circ}C$ for 1 hour produced higher isoflavone content than non-heated soybean seeds. Our results show that it is possible to increase the isoflavone content in soybean seeds through various treatments.

Reproducibility of Gated Myocardial Perfusion SPECT for the Assessment of Myocardial Function: Comparison with Thallium-201 and Technetium-99m-MIBI (심근 기능 측정에 사용된 게이트 심근 관류 SPECT 방법의 재현성 평가: $^{201}Tl$$^{99m}Tc$-MIBI 게이트 SPECT의 비교)

  • Hyun, In-Young;Seo, Jeong-Kee;Hong, Eui-Soo;Kim, Dae-Hyuk;Kim, Sung-Eun;Kwan, Jun;Park, Keum-Soo;Choe, Won-Sick;Lee, Woo-Hyung
    • The Korean Journal of Nuclear Medicine
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    • v.34 no.5
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    • pp.381-392
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    • 2000
  • Purpose: We compared the reproducibility of $^{201}Tl\;and\;^{99m}Tc$-sestamibi (MIBI) gated SPECT measurement of myocardial function using the Germano algorithm Materials and Methods: Gated SPECT acquisition was repeated in the same position in 30 patients who received $^{201}Tl$ and in 26 who received $^{99m}Tc$-MIBI. The quantification of end-diastolic volume (EDV), end-systolic volume (ESV), and ejection fraction (EF) on $^{201}Tl\;and\;^{99m}Tc$-MIBI gated SPECT was processed independently using Cedars quantitative gated SPECT software. The reproducibility of the assessment of myocardial function on $^{201}Tl$ gated SPECT was compared with that of $^{99m}Tc$-MIBI gated SPECT Results: Correlation between the two measurements for volumes and EF was excellent by the repeated gated SPECT studies of $^{201}Tl$ (r=0.928 to 0.986; p<0.05) and $^{99m}Tc$-MIBI (r=0.979 to 0.997; p<0.05). However, Bland Altman analysis revealed the 95% limits of agreement (2 SD) for volumes and EF were tighter by repeated $^{99m}Tc$-MIBI gated SPECT (EDV: 14.1 ml, ESV: 9.4 ml and EF: 5.5%) than by repeated $^{201}Tl$ gated SPECT (EDV: 24.1 ml, ESV: 18.6 ml and EF: 10.3%). The root mean square (RMS) values of the coefficient of variation (CV) for volumes und EFs were smaller by repeated $^{99m}Tc$-MIBI gated SPECT (EDV: 2.1 ml, ESV 2.7 ml and EF: 2.3%) than by repeated $^{201}Tl$ gated SPECT (EDV: 3.2 ml, ESV: 3.5 ml and EF: 5.2%). Conclusion: $^{99m}Tc$-MIBI provides more reproducible volumes and EF than $^{201}Tl$ on repeated acquisition gated SPECT. $^{99m}Tc$-MIBI gated SPECT is the preferable method for the clinical monitoring of myocardial function.

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Analytical Methods of Hydroxyl Radical Produced by TiO2 Photo-catalytic Oxidation (TiO2 광촉매 산화 반응에서 생성된 수산기 라디칼 분석 방법)

  • Kim, Seong Hee;Lee, Sang-Woo;Kim, Jeong Jin;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.28 no.3
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    • pp.245-253
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    • 2015
  • The performance of $TiO_2$ photo-catalytic oxidation process is significantly dependent on the amount of hydroxyl radicals produced during the process, and it is an essential prerequisite to quantify its production. However, precise and accurate methods for quantification of hydroxyl radicals have not been developed so far. For this reason, this study was initiated to compare existing methods for analysis of hydroxyl radicals produced by $TiO_2$ photo-catalytic oxidation and to propose a new method to overcome the limitation of established methods. To simulate $TiO_2$ photo-catalytic oxidation process, Degussa P25 which has been widely used as a standard $TiO_2$ photo-catalyst was used with the dose of 0.05 g/L. The light source of process was UVC mercury low-pressure lamp (11 W, $2,975mW/cm^2$). The results indicate that both potassium iodide (KI)/UV-vis spectrometer and terephthalic acid (TPA)/fluorescence spectrometer methods could be applied to qualitatively measure hydroxyl radicals via detection of triiodide ion ($I_3{^-}$) and 2-hydroxyterephthalic acid which are produced by reactions of iodine ion ($I^-$) and TPA with hydroxyl radicals, respectively. However, it was possible to quantitatively measure hydroxyl radicals using TPA method coupled with high-performance liquid chromatograph (HPLC). The analytical results using TPA/HPLC method show that hydroxyl radical of 0.013 M was produced after 8 hours operation of photo-catalytic oxidation under specific experimental conditions of this study. The proposed method is expected to contribute to precise the evaluation of the performance of photo-catalytic oxidation process.

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
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    • v.32 no.5
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    • pp.434-442
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    • 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.