• Title/Summary/Keyword: analytical validation

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Determination of Neonicotinoid Pesticides in Commercial Agricultural Products by LC-MS/MS (LC-MS/MS를 이용한 농산물중 Neonicotinoid 계 농약분석)

  • Hwang, Lae-hong;Yang, Hye-ran;Lee, Jae-kyoo;Kim, Chang-kyu;Kim, Min-jung
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.312-318
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    • 2020
  • A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for neonicotinoid pesticide analysis in agricultural products. Four compounds (imidacloprid, clothianidin, acetamiprid, thiacloprid) were extracted with acetonitrile from agricultural products and cleaned up by NH2 solid-phase extraction procedure, and eluted with 0.1% formic acid in methanol/dichloromethane (5/95, v/v). The limit of detection and quantification were 0.0001-0.0005 mg/kg and 0.001 mg/kg, respectively. The mean recoveries of neonicotinoid pesticide from agricultural products were in the range of 90.7-100.9% and 94.4-99.8%, as spiked at 0.2 mg/kg and 0.02 mg/kg, respectively. This validation satisfied the national criteria for pesticide analytical methods. In summary, The present method is fast, precise and sensitive enough for the Positive List System (PLS), and we conclude that the method is also suitable for neonicotinoid pesticide determination in a wide range of agricultural products.

An Analytical Method for the Validation of a Salt-enhancing Peptide Using a Liquid Chromatography and a Nuclear Magnetic Resonance (NMR) Spectroscopy (HPLC와 NMR를 이용한 염미성 펩타이드 분석방법 검증)

  • Park, Sun You;Jeong, Yong Jin;Kim, Mi-Yeon;Hwang, Ji Hong;Kwon, Taeg Kyu;Seo, Young Ho
    • Journal of Life Science
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    • v.27 no.11
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    • pp.1324-1330
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    • 2017
  • Salt, or sodium chloride (NaCl), is a critical ingredient in many foods. It has roles in the flavor profiles of food products, textures of foods and preservation of foods against microbes. However, it increases risks of hypertension and is closely related to the development of cardiovascular disease. In recent years, health concerns related to sodium intake caused an increased demand for salt-reduced products in worldwide; it became necessary to develop natural salt-alternative products that are globally competitive. In a recent study, researchers succeeded in obtaining a natural salt enhancer through the hydrolysis of vegetable- and animal-matter mixtures. This study used various methods to identify and quantify peptide-containing arginine as a salt-alternative peptide (SAP) in an optimum combination. Arginine, or dipeptide-containing arginine, was analyzed as a standard substance using an NMR spectroscopy. The NMR carbon signal of the guanidine group of the standard substance was verified in a similar location (the L-arginine (Arg) was 156.8 ppm, the Arg-Alanine was 156.4 ppm and the Arg-Serine was 156.4 ppm). The results suggested that it is possible to analyze peptide-containing arginine quantitatively through the hydrolysis of vegetable- and animal-matter mixtures.

A Study of the Effect of Acculturative Stress on the Marital Conflicts of Immigrant Women Who Are Married to Korean Men -Focusing on the Mediating Effect of Social Support- (결혼이주여성의 문화적응스트레스가 부부갈등에 미치는 영향 -사회적 지지의 조절효과 중심으로-)

  • Lee, Young-Sil;Cho, Myoung-Hee;Hong, Sung-Hee
    • Journal of Family Resource Management and Policy Review
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    • v.16 no.4
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    • pp.171-194
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    • 2012
  • This study focuses on immigrant women who are married to Korean men and who live in a multicultural family situation in Gyeonggi-do. These women experience acculturative stress and marital conflict and this study aims to determine how social support seeks to mediate the effects of those stressors. The women in this study participated in activities and received services from one of Gyeonggi-do Province's civic organizations, religious organizations, or social service organizations, such as the Social Welfare Agency and the Multicultural Family Support Center. In order to verify the study's hypothesis, the researchers used the following statistical analytical methods : t-test, two-way ANOVA and multi-regression analysis. Analysis of the study's results showed that the highest degree of marital conflict was found in the sub-zones and variables that were personal. Those variable were : the difference in mindset and values (personal domain), economic problems (communal living area), a child's upbringing and education issues (third party area), and the participant's sex life (in the marital relationship). The hypothesis was tested using the research model validation and the results are summarized as follows. First, in order to analyze the relationship between the marriage migration females' acculturative stress and the impact of that stress on marriage conflict, the hierarchical regression analysis was used. It identified that a direct correlation existed between acculturative stress and marriage conflict; where a higher degree of acculturative stress was present, a higher degree of marriage conflict was found. Second, the study found a statistical significance in the correlation and relationship (${\beta}$=.208, p<0.05) between the acculturative stress of the marriage migration female and material support. In other words, the material support can be seen as having a moderating effect on the acculturative stress, which is the independent variable, and the marital conflict, which is the dependent variable.

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Analytical Assessment of Blast Damage of 270,000-kL LNG Storage Outer Tank According to Explosive Charges (270,000 kL급 LNG 저장 탱크 외조의 폭발량에 따른 손상도 해석적 평가)

  • Kim, Jang-Ho Jay;Choi, Seung-Jai;Choi, Ji-Hun;Kim, Tae-Kyun;Lee, Tae-Hee
    • Journal of the Korea Concrete Institute
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    • v.28 no.6
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    • pp.685-693
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    • 2016
  • The outer tank of a liquefied natural gas (LNG) storage tank is a longitudinally and meridionally pre-stressed concrete (PSC) wall structure. Because of the current trend of constructing larger LNG storage tanks, the pre-stressing forces required to increase wall strength must be significantly increased. Because of the increase in tank sizes and pre-stressing forces, an extreme loading scenario such as a bomb blast or an airplane crash needs to be investigated. Therefore, in this study, the blast resistance performance of LNG storage tanks was analyzed by conducting a blast simulation to investigate the safety of larger LNG storage tanks. Test data validation for a blast simulation of reinforced concrete panels was performed using a specific FEM code, LS-DYNA, prior to a full-scale blast simulation of the outer tank of a 270,000-kL LNG storage tank. Another objective of this study was to evaluate the safety and serviceability of an LNG storage tank with respect to varying amounts of explosive charge. The results of this study can be used as basic data for the design and safety evaluation of PSC LNG storage tanks.

Development of Evaluation Criteria for Online Problem-Based Science Learning (온라인 문제기반 과학 탐구과제 평가준거 개발)

  • Choi, Kyoungae;Lee, Sunghye;Chae, Yoojung
    • Journal of The Korean Association For Science Education
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    • v.37 no.5
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    • pp.879-889
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    • 2017
  • The purpose of this study is to develop the evaluation criteria for students' research reports on online science inquiry problems that promote thinking abilities. The steps of developing the evaluation criteria are as follows; First, based on previous study results and literature review, the evaluation categories of the science inquiry contents were determined: 1) knowledge, 2) logical and analytical thinking, 3) critical thinking, 4) science process skills, 5) problem-solving, and 6) creative thinking. Second, evaluation criteria are developed according to the following steps: 1) define each category, 2) identify sub-category, 3) develop evaluation criteria for all categories that could serve as guidelines in the development of scoring rubrics, and 4) expert validation processes were performed. Finally, the usability test for these evaluation categories and criteria were done by being applied to the development of real scoring rubrics for 24 problems included in e-learning contents. Then the users' feedbacks were filed and the implications of this study were discussed.

Prediction on the Quality of Forage Crop Seeded in Spring by Near Infrared Reflectance Spectroscopy (NIRS) (근적외선 분광법에 의한 춘계 파종 사초의 성분추정)

  • Lee, Hyo-Won
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.31 no.4
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    • pp.409-414
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    • 2011
  • This study was conducted to find out an alternative way of rapid and accurate analysis of forage quality. Near Infrared Reflectance Spectroscopy (NIRS) was used to evaluate the possibility of forage analysis. 175 samples consisted of Italian ryegrass, whole crop barley and pea seeded spring in 2009 were collected. The samples were analyzed for moisture, crude protein (CP), crude ash (CA), acid detergent fiber (ADF), and neutral detergent fiber (NDF), and also scanned using NIRSystem with wavelength from 400~2,500 nm. Multiple linear regression was used with wet analysis data for developing the calibration model and validated unknown samples. The important index in this experiment were SEC, SEP. The r2 value for moisture, CP, CA, ADF, and NDF in calibration set was 0.65, 0.97, 0.93, 0.99, and 0.97 and also was 0.15, 0.94, 0.96, 0.98 and 0.98 in validation set, respectively. The results of this experiment indicates that NIRS was reliable analytical method to assess forage quality for CP, CA ADF and NDF except moisture content in forage when proper samples incorporated into the equation development.

Bioequivalence of Atorva Tablet® to Lipitor Tablet® (Atorvastatin 20 mg) (리피토정® (아토르바스타틴 20 mg)에 대한 아토르바정®의 생물학적동등성)

  • Lim, Hyun-Kyun;Lee, Tae-Ho;Lee, Jae-Hyun;Youm, Jeong-Rok;Song, Jin-Ho;Han, Sang-Beom
    • Journal of Pharmaceutical Investigation
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    • v.38 no.2
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    • pp.135-142
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    • 2008
  • The present study describes the evaluation of the bioequivalence of two atorvastatin tablets, Lipitor $Tablet^{(R)}$ (Pfizer, reference drug) and Atorva $Tablet^{(R)}$ (Yuhan, test drug), according to the guidelines of Korea Food and Drug Administration (KFDA). Forty-nine healthy male Korean volunteers received each medicine at the atorvastatin dose of 40 mg in a $2{\times}2$ crossover study with a two weeks washout interval. After drug administration, serial blood samples were collected at a specific time interval from 0-48 hours. The plasma atorvastatin concentrations were monitored by an high performance liquid chromatography -tandem mass spectrometer (LC-MS/MS) employing electrospray ionization technique and operating in multiple reaction monitoring (MRM) and positive ion mode. The total chromatographic run time was 4.5 min and calibration curves were linear over the concentration range of 0.1-100 ng/mL for atorvastatin. The method was validated for selectivity, sensitivity, linearity, accuracy and precision. $AUC_t$ (the area under the plasma concentration-time curve from time zero to 48hr) was calculated by the linear log trapezoidal rule method. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were complied trom the plasma concentration-time data. Analysis of variance was carried out using logarithmically transformed $AUC_t$ and $C_{max}$. No significant sequence effect was found for all of the bioavailability parameters indicating that the crossover design was properly performed. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for Atorva $Tablet^{(R)}$ / Lipitor $Tablet^{(R)}$ were ${\log}\;0.9413{\sim}{\log}\;1.0179$ and ${\log}\;0.831{\sim}{\log}\;1.0569$, respectively. These values were within the acceptable bioequivalence intervals of ${\log}\;0.8{\sim}{\log}\;1.25$. Based on these statistical considerations, it was concluded that the test drug, Atorva $Tablet^{(R)}$ was bioequivalent to the reference drug, Lipitor $Tablet^{(R)}$.

Development of Simultaneous Analysis of Ferulic Acid, Caffeic Acid, Catechin and Taxifolin from Health Functional Food Pinus Pinaster Bark Extract by UPLC-MS/MS (건강기능식품 프랑스해안송껍질추출물 중 UPLC-MS/MS를 이용한 Ferulic acid, Caffeic acid, Catechin, Taxifolin 동시분석법 개발 연구)

  • Oh, Jae-Myoung;Kim, Ji An;Hu, Soo Jung;Choi, Yoon Hee;Oh, Keum Soon
    • Journal of Food Hygiene and Safety
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    • v.34 no.5
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    • pp.431-437
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    • 2019
  • This study was conducted to develop a simultaneous analysis method for ferulic acid, caffeic acid, catechin and taxifolin from Health Functional Food (HFF) Pinus Pinaster bark extract. The simultaneous analytical method for ferulic acid, caffeic acid, catechin and taxifolin is carried out using UPLC-MS/MS. The method validation was performed to determine selectivity, linearity, accuracy, limit of detection (LOD), limit of quantification (LOQ) and precision for ferulic acid, caffeic acid, catechin and taxifolin. LC-MS/MS method was established using an Acquity UPLC BEH $C_{18}$ Column and was applied for these 4 compounds. Product-ion traces, at m/z $194.2{\rightarrow}133$, $180.2{\rightarrow}135$, $290.3{\rightarrow}245$, $304.3{\rightarrow}248$, were used for quantitative analysis of ferulic acid, caffeic acid, catechin and taxifolin, respectively. Excellent linearity ($r^2=0.999$) was observed for ferulic acid, caffeic acid, catechin and taxifolin in the concentration range (50-2500 mg/L). The observed recoveries of these 4 compounds were found to be between 84.9 and 104.9%, while precision was between 1.20 and 4.43% relative standard deviation (% RSD).

Folate retention in Namul according to various heating methods (다양한 열 처리방법에 대한 나물류의 엽산 잔존율)

  • Jung, Jae Eun;Jeong, Hea-Jeong;Hyun, Taisun;Park, Su-Jin;Chun, Jiyeon
    • Korean Journal of Food Science and Technology
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    • v.51 no.5
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    • pp.425-431
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    • 2019
  • Selected leafy vegetables, widely used for Korean Namul dishes, were heat-treated in different ways and their folate retention was investigated. The Lactobacillus casei method was applied for folate estimation and validated to ensure reliability of analytical data. The folate content in Namul highly varied, from 29.7 to $293.4{\mu}g/100g$, depending on the heating methods and the types of vegetables. Most of the Namul variants showed increased folate content on heat treatment. Frying yielded higher folate retention than the other cooking methods (blanching, steaming, baking, and panfrying), and pig weed showed the highest folate retention (3.3 times, $293.4{\mu}g/100g$). L. casei assay for folate estimation showed 95.7% recovery and relative standard deviations less than 2% for both reproducibility and repeatability, indicating good accuracy and precision. Quality of the folate assay was assured by monitoring a quality control chart and a proficiency test (z-score= -0.1) during the entire of study.

Comparison of Loop-Mediated Isothermal Amplification and Real-Time PCR for the Rapid Detection of Salmonella Typhimurium, Listeria monocytogenes and Cronobacter sakazakii Artificially Inoculated in Foods (식품에 인위접종된 Salmonella Typhimurium, Listeria monocytogenes, Cronobacter sakazakii의 신속검출을 위한 Real-time PCR과 Loop-mediated isothermal amplification 비교)

  • Kim, Jin-Hee;Oh, Se-Wook
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.135-139
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    • 2019
  • The objective of this research was to compare loop-mediated isothermal amplification (LAMP) with real-time polymerase chain reaction (PCR) for the rapid detection of pathogens in foods. In this study, the limits of detection (LODs) for Salmonella Typhimurium, Listeria monocytogenes, and Cronobacter sakazakii were evaluated in various foods. Among 11 samples tested for S. Typhimurium, LAMP and real-time PCR had the same LODs in beef and duck meat whereas real-time PCR was more sensitive than the LAMP in 8 samples. However, S. Typhimurium in chocolate samples was not detected by real-time PCR. The sensitivity of real-time PCR was high in all samples inoculated with L. monocytogenes and C. sakazakii whereas LAMP was more sensitive than real-time PCR in oil-rich foods. Therefore, LAMP can be shown as an easrer, more convenient method, as well as effective analytical method for testing difficult samples when employed in PCR.