• Title/Summary/Keyword: Quantification Method

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The Evaluation of Usefulness of Wide Beam Reconstruction Method on Segmental Perfusion and Regional Wall Motion in Myocardial Perfusion SPECT (심근관류 SPECT의 분절별 관류 및 국소벽 운동에서 Wide Beam Reconstruction기법의 유용성 평가)

  • Seong, Yong-Joon;Kim, Tae-Yeob;Moon, Il-Sang;Cho, Seong-Wook;Woo, Jae-Ryong
    • The Korean Journal of Nuclear Medicine Technology
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    • v.15 no.1
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    • pp.51-57
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    • 2011
  • Purpose: The aim of this study is to identify clinical usefulness of Wide Beam Reconstruction (WBR) which is called Xpress.cardiac$^{TM}$ to confirm the agreement between segmental perfusion and regional wall motion in myocardium compared to conventional OSEM method. Materials and Methods: Subjects were separated two groups. First group was composed of 20 normal control group. Second group was composed of 10 patients (abnormal group) who had coronary artery disease. Subjects underwent myocardial perfusion SPECT ($^{201}Tl$ rest and $^{99m}Tc$-MIBI stress). Image acquisition and reconstruction were that rest stage was each step per 30, 15 seconds and stress stage was each step per 25, 13 seconds, OSEM and WBR methods were applied. Segmental perfusion and regional wall motion were applied 20-segment model of QPS, QGS algorithm in AutoQuant. Status of perfusion was composed of 5 point scoring system (0=normal, 1=mild, 2=moderate, 3=severe hypokinesia, 4=dyskinesia). Status of regional wall motion was also composed of 5 point scoring (0=normal, 1=mild, 2=moderate, 3=severe hypokinesia, 4=dyskinesia). We evaluated the agreement between conventional OSEM and WBR through automatic quantification value. Results: The agreement of rest segmental perfusion between conventional OSEM and WBR in normal patients was 99% (396/400, k=0.662, p<0.0001) and one of rest regional wall motion was 83.8% (335/400, k=0.283), the agreement of stress segmental perfusion was 95.8%(383/400, k=0.656), one of stress regional wall motion was 87.3% (349/400, k=0.390). The match rate of rest segmental perfusion in abnormal patients was 83% (166/200, k=0.605, p<0.0001) and one of rest regional wall motion was 55.5% (111/200, k=0.385), the agreement of stress segmental perfusion was 79.5% (159/200, k=0.682), one of stress regional wall motion was 63.5% (127/200, k=0.486). Conclusion: Compared to conventional OSEM, WBR method had a good agreement of segmental perfusion in myocardium in normal and abnormal groups. However regional wall motion showed meaningful low agreement. Although WBR offers high resolution and contrast ratio, it is not useful method for gated myocardial perfusion SPECT.

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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.

Monitoring of Uniconazole by GC-NPD (GC-NPD 동시분석법을 이용한 유니코나졸 잔류실태조사)

  • Kim, Eun-Jeung;Choi, Bu-Chuhl;Choi, Su-Jeong;Hong, Chae-Kyu;Kim, Eun-Hee;Choi, Chae-Man;Seo, Young-Ho;Hwang, Young-Sook;Jang, Mi-Ra;Hwang, In-Sook;Kim, Moo-Sang;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.378-381
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    • 2012
  • The monitoring of the uniconazole residual pesticide for agricultural products was conducted by multiclass pesticide multiresidue methods. Samples were collected from June to November, 2011. Uniconazole pesticide was detected in 49 samples from a total of 3,939 samples. The amount of uniconazole pesticide ranged from 0.09 to 17.89 mg/kg in 49 samples. This method was described for the simultaneous determination of uniconazole by gas chromatography with a nitrogen phosphorus detector (GC-NPD) and mass spectrometry (MS). The limit of detection and quantification were 0.006 and 0.018 mg/kg GC-NPD, respectively. For an evaluation of the GC-NPD method, uniconazole spiked into gyeojachae at a level of 0.5, 5 mg/kg was determined. The recoveries of uniconazole by the GC-NPD method ranged from 83.4 to 101.4%. The results indicate that the method of simultaneous analysis is applicable to uniconazole analysis.

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
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    • v.44 no.3
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    • pp.263-268
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    • 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.

Development of a Simultaneous Analytical Method for Determination of Trinexapac-ethyl and Trinexapac in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 식물생장조절제 Trinexapac-ethyl과 대사산물 Trinexapac의 동시분석법 개발)

  • Jang, Jin;Kim, Heejung;Ko, Ah-Young;Lee, Eun-Hyang;Ju, Yunji;Chang, Moon-Ik;Rhee, Gyu-Seek;Suh, Saejung
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.318-327
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    • 2015
  • BACKGROUND: Trinexapac-ethyl is a plant growth regulator (PGR) that inhibits the biosynthesis of plant growth hormone (gibberellin). It is used for the prevention of lodging, increasing yields of cereals, and reducing mowing of turf. The experiment was conducted to establish a determination method for trinexapac-ethyl and its metabolites trinexapac in agricultural products using LC-MS/MS.METHODS AND RESULTS: Trinexapac-ethyl and trinexapac were extracted from agricultural products with methanol/ distilled water and the extract was partitioned with dichloromethane and then detected by LC-MS/MS. Limit of detection(LOD) was 0.003 mg/kg and limit of quantification(LOQ) was 0.01 mg/kg, respectively. Matrix matched calibration curves were linear over the calibration ranges (0.01-1.0 mg/L) for all the analytes into blank extract withr2> 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, 50LOQ,n=5). Recoveries of trinexapacethyl and trinexapac were within the range of 73.6-106.9%, 72.7-99.2%, respectively. The relative standard deviations (RSDs) were less than 9.0%. All values were consistent with the criteria ranges requested in the CODEX guideline(CAC/GL 40, 2003).CONCLUSION: The proposed analytical method was accurate, effective and sensitive for trinexapac-ethyl and trinexapac determination and it can be used to as an official method in Korea.

Method Validation for Determination of Lignan Content in Fermented Sesame by Bioconversion (생물전환된 참깨 발효물의 Lignan 화합물의 분석법 검증)

  • Jung, Tae-Dong;Kim, Jae-Min;Choi, Sun-Il;Choi, Seung-Hyun;Cho, Bong-Yeon;Lee, Jin-Ha;Lee, Sang Jong;Park, Seon Ju;Heo, In Young;Lee, Ok-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.5
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    • pp.646-652
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    • 2017
  • The aim of this study was to investigate method validation for determination of sesamol, sesamin, and sesamolin in non-fermented sesame and fermented sesame by bioconversion. For validation, the specificity, linearity, precision, accuracy, limits of detection (LOD), and quantification (LOQ) of sesamol, sesamin, and sesamolin were measured by HPLC. Linearity tests showed that the coefficients of calibration correlation ($R^2$) for sesamol, sesamin, and sesamolin were 0.9999. Recovery rates of lignan contents in non-fermented and fermented sesame were high in the ranges of 100.27~115.10% and 98.43~114.90%, respectively. The inter-day and intra-day precisions of sesamin and sesamolin analyses for non-fermented and fermented sesame were 0.27~1.94% and 0.25~0.69%, respectively. The LOD and LOQ were $0.23{\sim}0.34{\mu}g/g$ and $0.70{\sim}1.03{\mu}g/g$, respectively. These results indicate that the validated method is appropriate for the determination of sesamol, sesamin, and sesamolin.

Quantitative Elemental Analysis in Soils by using Laser Induced Breakdown Spectroscopy(LIBS) (레이저유도붕괴분광법을 활용한 토양의 정량분석)

  • Zhang, Yong-Seon;Lee, Gye-Jun;Lee, Jeong-Tae;Hwang, Seon-Woong;Jin, Yong-Ik;Park, Chan-Won;Moon, Yong-Hee
    • Korean Journal of Soil Science and Fertilizer
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    • v.42 no.5
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    • pp.399-407
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    • 2009
  • Laser induced breakdown spectroscopy(LIBS) is an simple analysis method for directly quantifying many kinds of soil micro-elements on site using a small size of laser without pre-treatment at any property of materials(solid, liquid and gas). The purpose of this study were to find an optimum condition of the LIBS measurement including wavelengths for quantifying soil elements, to relate spectral properties to the concentration of soil elements using LIBS as a simultaneous un-breakdown quantitative analysis technology, which can be applied for the safety assessment of agricultural products and precision agriculture, and to compare the results with a standardized chemical analysis method. Soil samples classified as fine-silty, mixed, thermic Typic Hapludalf(Memphis series) from grassland and uplands in Tennessee, USA were collected, crushed, and prepared for further analysis or LIBS measurement. The samples were measured using LIBS ranged from 200 to 600 nm(0.03 nm interval) with a Nd:YAG laser at 532 nm, with a beam energy of 25 mJ per pulse, a pulse width of 5 ns, and a repetition rate of 10 Hz. The optimum wavelength(${\lambda}nm$) of LIBS for estimating soil and plant elements were 308.2 nm for Al, 428.3 nm for Ca, 247.8 nm for T-C, 438.3 nm for Fe, 766.5 nm for K, 85.2 nm for Mg, 330.2 nm for Na, 213.6 nm for P, 180.7 nm for S, 288.2 nm for Si, and 351.9 nm for Ti, respectively. Coefficients of determination($r^2$) of calibration curve using standard reference soil samples for each element from LIBS measurement were ranged from 0.863 to 0.977. In comparison with ICP-AES(Inductively coupled plasma atomic emission spectroscopy) measurement, measurement error in terms of relative standard error were calculated. Silicon dioxide(SiO2) concentration estimated from two methods showed good agreement with -3.5% of relative standard error. The relative standard errors for the other elements were high. It implies that the prediction accuracy is low which might be caused by matrix effect such as particle size and constituent of soils. It is necessary to enhance the measurement and prediction accuracy of LIBS by improving pretreatment process, standard reference soil samples, and measurement method for a reliable quantification method.

Study for Residue Analysis of Herbicide, Clopyralid in Foods (식품 중 제초제 클로피랄리드(Clopyralid)의 잔류 분석법)

  • Kim, Ji-young;Choi, Yoon Ju;Kim, Jong Su;Kim, Do Hoon;Do, Jung Ah;Jung, Yong Hyun;Lee, Kang Bong;Kim, Hyo Chin
    • Korean Journal of Environmental Agriculture
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    • v.37 no.4
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    • pp.283-290
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    • 2018
  • BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.

Simultaneous Multicomponent Analysis of Preservatives in Cosmetics by Gas Chromatography (GC를 이용한 화장품 살균·보존제의 다성분 동시분석법)

  • Cho, Sang Hun;Jung, Hong Rae;Kim, Young Sug;Kim, Yang Hee;Park, Eun Mi;Shin, Sang Woon;Eum, Kyoung Suk;Hong, Se Ra;Kang, Hyo Jeong;Yoon, Mi Hye
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.45 no.1
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    • pp.69-75
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    • 2019
  • Preservatives of cosmetics is managed by positive list in Korea. Positive list requires a proper quantitative analysis method, but the analysis method is still insufficient. In this study, gas chromatography with flame ionization detector was used to simultaneously analyze 14 preservatives in cosmetics. As a result of method validation, the specificity was confirmed by the calibration curves of 14 preservatives showing good linearity correlation coefficient of above 0.9997 except dehydroacetic acid (0.9891). The limits of detection (LOD) and quantification (LOQ) of 14 preservatives were 0.0001 mg/mL ~ 0.0039 mg/mL and 0.0003 mg/mL ~ 0.0118 mg/mL, respectively, but they were 0.0204 mg/mL, 0.0617 mg/mL for dehydroacetic acid, respectively. The precision (Repeatability) of the values was less than 1.0%, but 7.1% for dehydroacetic acid. The Accuracy (% recovery) of 14 preservatives in cosmetics showed 96.9% ~ 109.2%. Finally, this method was applied to 50 cosmetics available in market. Results showed that the commonly used preservatives were chlorophene, phenoxyethanol, benzyl alcohol and parabens. However, the amount of the detected preservatives was within maximum allowed limits established by KFDA.

Development and Validation of Analytical Method and Antioxidant Effect for Berberine and Palmatine in P.amurense (황백의 지표성분 berberine과 palmatine의 분석법 개발과 검증 및 항산화 효능 평가)

  • Jang, Gill-Woong;Choi, Sun-Il;Han, Xionggao;Men, Xiao;Kwon, Hee-Yeon;Choi, Ye-Eun;Park, Byung-Woo;Kim, Jeong-Jin;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.35 no.6
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    • pp.544-551
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    • 2020
  • The aim of this study was to develop and validate a simultaneous analytical method for berberine and palmatine, which are representative substances of Phellodendron amurense, and to evaluate the antioxidant activity. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for berberine and palmatine using high-performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for berberine and palmatine exhibited 0.9999. The LODs for berberine and palmatine were 0.32 to 0.35 µg/mL and the LOQs were 0.97 to 1.06 µg/mL, respectively. The inter-day and intra-day precision values for berberine and palmatine were from 0.12 to 1.93 and 0.19 to 2.89%, respectively. The inter-day and intra-day accuracies were 98.43-101.45% and 92.39-100.60%, respectively. In addition, the simultaneous analytical method was validated for the detection of berberine and palmatine. Moreover, we conducted FRAP and NaNO2 scavenging activity assays to measure the antioxidant activities of berberine and palmatine, and both showed antioxidant activity. These results suggest that P.amurense could be a potential natural resource for antioxidant activity and that the efficacy can be confirmed by investigating the content of the berberine and palmatine.