• Title/Summary/Keyword: Quantification Analysis

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Development of an Analytical Method for Fluxapyroxad Determination in Agricultural Commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Fluxapyroxad 잔류분석법 개발)

  • Kwon, Ji-Eun;Kim, HeeJung;Do, Jung-Ah;Park, Hyejin;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.29 no.3
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    • pp.234-240
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    • 2014
  • Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

Applied-Mineralogical Characterization and Assessment of Some Domestic Bentonites (I): Mineral Composition and Characteristics, Cation Exchange Properties, and Their Relationships (국내산 벤토나이트에 대한 응용광물학적 특성 평가 (I): 광물 조성 및 특징과 양이온 교환특성과의 연계성)

  • 노진환
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.4
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    • pp.329-344
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    • 2002
  • Mineralogical and chemical characterization of some domestic bentonites, such as quantitative XRD analysis, chemical leaching experiments, pH and CEC determinations, were done without any separation procedures to understand their relationships among mineral composition, characteristics, and cation exchange properties. XRD quantification results based on Rietveld method reveal that the bentonites contain totally more than 25 wt% of impurities, such as zeolites, opal-CT, and feldspars, in addition to montmorillonite ranging 30~75 wt%. Cation exchange properties of the zeolitic bentonites are deeply affected by the content of zeolites identified as clinoptilolite-heulandite series. Clinoptilolite is common in the silicic bentonites with lighter color. and occurs closely in association with opal-CT. Ca is mostly the dominant exchangeable cation, but some zeolitic bentonites have K as a major exchangeable cation, The values of cation exchange capacity (CEC) determined by Methylene Blue method are comparatively low and have roughly a linear relationship with the montmorillonite content of the bentonite, though the correlated data tend to be rather dispersed. Compared to this, the CEC determined by Ammonium Acetate method, i.e.‘Total CEC’, has much higher values (50~115 meq/100 g). The differences between those CEC values are much greater in zeolitic bentonites, which obviously indicates the CEC increase affected by zeolite. Other impurities such as opal-CT and feldspars seem to affect insignificantly on the CEC of bentonites. When dispersed in distilled water, the pH of bentonites roughly tends to increase up to 9.3 with increasing the alkali abundance, especially Na, in exchangeable cation composition. However, some bentonites exhibit lower pH (5~6) so as to regard as ‘acid clay’. This may be due to the presence of $H^{+}$ in part as an exchangeable cation in the layer site of montmorillonite. All the works of this study ultimately suggest that an assesment of domestic bentonites in grade and quality should be accomplished through the quantitative XRD analysis and the ‘Total CEC’measurement.

Cellular Analysis and Measurement of Mucin in Sputum of Chronic Airway Disease (만성기도질환의 객담세포분석과 mucin의 측정)

  • Kim, Ki-Up;Kim, Yang-Ki;Shin, Chan-Young;Kim, Do-Jin;Uh, Soo-Taek;Kim, Yong-Hoon;Ko, Kwang-Ho;Park, Choon-Sik
    • Tuberculosis and Respiratory Diseases
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    • v.49 no.1
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    • pp.82-92
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    • 2000
  • Background : In chronic airway disease, mucus secretion is increased, but extraction of mucin, which is the main component of mucus secretion, is a very complicated and limited in clinical use. Recently, monoclonal antibody for mucin was developed for possible clinical use. In this study, cellular analysis and quantification of respiratory mucin in sputum of patients with chronic airway diseases were performed. Method : Sputum was collected from patients with asthma(n=33), bronchiectasis(n=8) or chronic bronchitis (n=13) by spontaneous expectoration or by hypertonic saline induction. Collected sputums was treated by 0.1% dithiotreitol to dissociate the disulfide bond of the mucus and filtered through a nylon gauze. Total cell count, viability and differential count were measured. For detection of mucin, collected samples were treated with sodium dodecyl sulfate polyacrylamide gel electrophoresis and then with monoclonal antibody(HMO2), as the primary antibody, and PAS stain. The amount of mucin was measured with ELISA by HMO2. Correlation with clinical information, cellular analysis, and amount of measured mucin were analyzed. Results : Total cell counts of sputum were significantly increased in patients with bronchiectasis but viability remained the same. Eosinophils were significantly increased in patients with asthma, neutrophils in bronchiectasis chronic bronchitis, respectively (p<0.05). The results of Western blotting and PAS staining confirmed the presence of glycoproteins and matched? with mucin. The amounts of mucin measured by ELISA were not significantly different among the disease groups. Significant correlation was identified between the amount of mucin and viability(r=-0.482, p<0.05). Conclusion : Inflammatory cells in the sputum of those with chronic airway disease were different for each disease type. Measurement of mucin by ELISA via monoclonal antibodies may be a simple method for the evaluation of chronic airway disease.

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Mineralogical Characteristics of the Lower Choseon Supergroup in the Weondong Area (원동지역 하부 조선누층군의 광물학적 특성)

  • Kim, Ha;Sim, Ho;Won, Moosoo;Kim, Myeong-Ji;Lee, Ju-Ho;Song, Yun-Goo
    • Economic and Environmental Geology
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    • v.49 no.5
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    • pp.349-360
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    • 2016
  • This study determined mineralogical characteristics and discussed the meaning of mineralogical changes of the lower Choseon Supergrouop in the Weondong area based on the field geological investigation and the drilling core description using X-ray diffraction (XRD) mineral quantification and Scanning Electron Microscopy (SEM) observation. 100 samples with depth were collected from the core (250 m long) at a site in the study area. Especially, to investigate the changes from the upper Daegi Formation to the lower Hwajeol Formation, the samples were collected closely with the interval of about 0.3 m at this section. All samples were made into power using mortar for XRD. Mineral quantitative analysis was executed using Relative Intensity Ratio (RIR) method with corundum as an internal standard phase. Calcite, $2M_1$ illite and quartz are main constituents in most of samples. Dolomite and siderite are significantly observed in the Sesong Formation. As the results of quantitative analysis for the major minerals, the upper Daegi Formation is dominated by calcite with over 80%. The Sesong Formation includes high percentage of dolomite and siderite with the intercalation of thin layers containing high calcite and $2M_1$ illite contents. Hwajeol Formation is characterized by the alternation between thin layers of $2M_1$ illite and quartz-dominated layer (IQDL) and calcite-dominated layer (CDL). IQDL is more frequent in the lower part, whereas CDL is more common in the upper part. The boundary between Daegi Formation and the Sesong Formation is distinct, whereas the boundary between the Sesong Formation and the Hwajeol Formation tends to be changed gradually in mineralogy. The result of SEM observation shows that quartz and $2M_1$ illite are detrital, and a significant amount of calcite also shows detrital form with some recrystallized one, indicating that the repeated influx of terrestrial materials had changed the mineralogy of the shallow sea depositional environment in the early Paleozoic era.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

Establishment of Choline Analysis in Infant Formulas and Follow-up Formulas by Ion Chromatograph (이온크로마토그래프를 이용한 조제유류 및 영아용·성장기용 조제식 중 콜린 함량 분석법 연구)

  • Hwang, Kyung Mi;Ham, Hyeon Suk;Lee, Hwa Jung;Kang, Yoon Jung;Yoon, Hae Seong;Hong, Jin Hwan;Lee, Hyoun Young;Kim, Cheon Hoe;Oh, Keum Soon
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.411-417
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    • 2017
  • This study was conducted to establish the analysis method for the contents of choline in infant formulas and follow-up formulas by ion chromatograph (IC). To optimize the method, we compared several conditions for extraction, purification and instrumental measurement using spiked samples and certified reference material (CRM; NIST SRM 1849a) as test materials. IC method for choline was established using Ion Pac CG column and 18 mM $H_2SO_4$ mobile phase. The parameters of validation were specificity, linearity, LOD, LOQ, recovery, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity, $R_2$ was over 0.999 in range of 0.5~10 mg/L. The detection limit and quantification limit were 0.14, 0.43 mg/L. The accuracy and precision of this method using CRM were 95%, 2.1% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested products were acceptable contents of choline compared with component specification for nutrition labeling. The standard operating procedures were prepared for choline to provide experimental information and to strengthen the management of nutrient in infant formula and follow-up formula.

Monitoring of Aflatoxins in Medicinal Herbs (유통 생약재의 아플라톡신 모니터링)

  • Kim, Yong-Hoon;Kang, Han-Saem;Oh, Sun-Woo;Lee, Hwa-Jung;Kim, Mi-Gyeong;Chung, So-Young;Choi, Seon-Hee;Bang, Su-Jin;Han, Kyung-Jin;Lee, Ji-Won;Kim, Young-Seon;Kim, Hee-Yun
    • Korean Journal of Food Science and Technology
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    • v.42 no.1
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    • pp.27-32
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    • 2010
  • This study was conducted to monitor aflatoxins in various medicinal herbs, providing available data for the safety of those products. To monitor aflatoxins in medicinal herbs, a total of 400 samples of 40 different herbs were collected in commercial retailers in Seoul, Daejeon, Gwangju, Daegu, and Busan from March to August, 2008. The samples that passed the sensory evaluation were tested for aflatoxins. Aflatoxins in samples were analyzed by HPLC-florescence coupled with photochemical enhancement. Samples were extracted with 70% methanol and then diluted to the appropriate concentration. A refining process was performed using an immunoaffinity column. The analytical method used in this study was validated. The $R^2$ value for aflatoxin $B_1$ was 0.99946, and the detection range was from 0.25 to 10.0 ng/mL. The accuracy of the analysis was ranged from 83.2% to 101.8%. The relative standard deviation (RSD) in the aflatoxin $B_1$ analysis was 3.4%, demonstrating the precision of this method. In addition, the detection limit and quantitative analysis limit of aflatoxin $B_1$ was $0.53\;{\mu}g/kg$ and $1.76\;{\mu}g/kg$, respectively. These results indicated that the analytical method used in this study was appropriate. The results of HPLC showed that 1% (4 samples) of the samples may contain aflatoxins. The concentration of quantified aflatoxin was $2.3\;{\mu}g/kg$ for both Quisqualis fructus and Remotiflori radix samples. The other samples were below the limit of quantification. Moreover, the concentration of aflatoxin $B_1$ which is made by specific fungi were below the level of regulation. Only 20% of aflatoxin $B_1$ were transferred to hot water. Therefore, the levels of aflatoxins in medicinal herbs were considered to be safe especially considering the aflatoxin transfer ratio.

Performance of Occupational Health Services by Type of Service : Cost Benefit Analysis (사업장 보건관리 사업의 형태별 수행성과 분석 -비용편익 분석을 중심으로-)

  • Cho, Tong Ran;Kim, Hwa Joong
    • Korean Journal of Occupational Health Nursing
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    • v.4
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    • pp.5-29
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    • 1995
  • Occupational health services in Korea have been operated as dual types : one is operated by occupational health care manager and the other is health care agency without their own personnel. The performance of occupational health service should be different due to the variety of characteristics of health care manager and workplace, qualification of health care manager. This study is to analyze performance of occupational health care services with a particular consideration of job performance shape and efficiency, based on comparing those two types of health care management to show on the basic data for the settlement of more qualitative health care management system at workplace. For this study, total 391 places in Seoul and Inchon city area ; 154 places (39.4%) managed by designated health care manager and 237 places (60.6%) by the agency with their commission are selected as research samples. Tools for data collection are questionnares that have been investigated during the period of 20 September 1993-20 December 1993. Those data are compared with percentiles, mean, standard deviation and B/C ratio using SPSS PC program. Conclusions observed from the tests and each comparison could be summerized as follows : 1. Occupational health care have been accomplished at workplaces with designated people than with agencies people, and coverage rate of the occupational health care services has differences, due to management types. The reason of these results is due to visit only one or two times monthly by the agencies, while their own health care manager obsess, at the workplaces all the times. 2. Most of the expense for environmental control of all health care services expenditures shows that there is almost no fundamental improvement because more expenses are needed for procuring personal protective equipment and measuring work environment instead of environmental improvement. 3. It is investigated how much the cost of occupational health care services needs per worker, and calculated how much the cost needs per service hour per worker. The results from this show that the cost of occupational health services at workplaces with their own managers used less than the cost of health care agencies, eventually the former gives better services with less cost than the latter. 4. Benefit/Cost ratio is also produced by total benefit/total cost. The result from the above way reads 4.57 as a whole, while their own manager having workplaces reads 4.82 and the agencies do l.56. Even if their own manager performing workplaces spent more cost, this system produces more benefit than the agencies management. 5. The B/C ratio for medical organization such as local clinic, health care center and pharmacy shows more than or equal to at the workplaces controlled by the agencies. It is inferred that benefit would be much less than the cost used, with so being inefficient. 6. It is assumed that the efficiency ratio of health education is equal to reduction rate of workers medical organization visit. Estimated reduction rate 5%, 10%, 15%, show that the efficiency ratio of health education have an effect on producing benefits. It is estimated that more benefit can be produced if more qualitative education will be provided for enhancing health care efficiency. 7. Results of this study cannot be generalized because there are large scale of deviation in case of workplaces with less than 300 full time workers, but B/C ratio reads 2.69 as a whole and 3.25 at workplaces with their own health care manager are higher than 1.63 at the workplaces manged by the agencies. Finally, all the benefit concerning health care services could not be quantified, measured and shown on the value of money. This is a reason that a considerable part of benefits are so underestimated. This is also thought that measurement tools should be developed for measuring benefits of health care services with a comprehensive quantification. in the future. It is also expected that efficiency of occupational health care services should be investigated using cost-effectiveness analysis.

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Development of Program for Renal Function Study with Quantification Analysis of Nuclear Medicine Image (핵의학 영상의 정량적 분석을 통한 신장기능 평가 프로그램 개발)

  • Song, Ju-Young;Lee, Hyoung-Koo;Suh, Tae-Suk;Choe, Bo-Young;Shinn, Kyung-Sub;Chung, Yong-An;Kim, Sung-Hoon;Chung, Soo-Kyo
    • The Korean Journal of Nuclear Medicine
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    • v.35 no.2
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    • pp.89-99
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    • 2001
  • Purpose: In this study, we developed a new software tool for the analysis of renal scintigraphy which can be modified more easily by a user who needs to study new clinical applications, and the appropriateness of the results from our program was studied. Materials and Methods: The analysis tool was programmed with IDL5.2 and designed for use on a personal computer running Windows. For testing the developed tool and studying the appropriateness of the calculated glomerular filtration rate (GFR), $^{99m}Tc$-DTPA was administered to 10 adults in normal condition. In order to study the appropriateness of the calculated mean transit time (MTT), $^{99m}Tc-DTPA\;and\;^{99m}Tc-MAG3$ were administered to 11 adults in normal condition and 22 kidneys were analyzed. All the images were acquired with ORBITOR. the Siemens gamma camera. Results: With the developed tool, we could show dynamic renal images and time activity curve (TAC) in each ROI and calculate clinical parameters of renal function. The results calculated by the developed tool were not different statistically from the results obtained by the Siemens application program (Tmax: p=0.68, Relative Renal Function: p:1.0, GFR: p=0.25) and the developed program proved reasonable. The MTT calculation tool proved to be reasonable by the evaluation of the influence of hydration status on MTT. Conclusion: We have obtained reasonable clinical parameters for the evaluation of renal function with the software tool developed in this study. The developed tool could prove more practical than conventional, commercial programs.

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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.