• Title/Summary/Keyword: Sample preparation method

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QuEChERS 전처리법과 GC-TOF/MS, ECD, NPD를 이용한 잔류농약 다성분분석 (Multi-residue Analysis of Pesticides using GC-TOF/MS, ECD, NPD with QuEChERS Sample Preparation)

  • 박정욱;김애경;김종필;이향희;박덕웅;문수진;하동룡;김은선;서계원
    • 농약과학회지
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    • 제18권4호
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    • pp.278-295
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    • 2014
  • 농수산물검사소에서는 빠르고 정확한 잔류농약검사법이 필요하므로 QuEChERS 시료 전처리법과 GC-TOF/MS(가스크로마토그래피 비행시간질량분석기와 GC-ECD(전자포획검출기), GC-NPD(질소인검출기) 기기분석을 이용하여 잔류농약 동시다성분 분석의 가능성을 살펴보았다. GC-TOF/MS에서는 138종의 농약성분을 0.3, $0.5{\mu}g/g$수준으로 상추에 처리 후 회수율 측정을 하였다. 동시다성분 회수율기준 70~130% 범위에 들어오고 표준편차 20% 이내인 농약은 61종이었다. GC-ECD, NPD에서는 145종의 농약성분 중 71종이 적정한 회수율 범위 내에 들었다. 이러한 결과는 일부 농약성분에 대해 QuEChERS 시료 전처리법과 GC-TOF/MS, GC-ECD, NPD를을 이용한 잔류농약 동시다성분분석 방법 적용 가능성을 보여주었다.

Solid Phase Microextraction법을 이용한 식품포장재 중의 잔류용제 분석 (Analysis of Residual Solvents in Food Packaging Materials Using Solid Phase Microextraction Method)

  • 서택교;박상현;이윤수;김정한;권익부
    • 한국식품위생안전성학회지
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    • 제14권1호
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    • pp.76-83
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    • 1999
  • Solid phase microextraction (SPME) was used for the determination of 6 standard solvents (methanol, isopropanol, methyl ethyl ketone, ethyl acetate, cyclohexane, toluene) in food packaging materials. SPME method is a solvent-free sample preparation technique in which a fused silica fiber coated with polymeric organic liquid is introduced into the headspace above the sample. SPME method using fiber coated polydimethylisiloxane (PDMS) was compared with static headspace (SHS) method used as a reference. It was found that the optimal adsorption condition using PDMS-SPME method was 2$0^{\circ}C$ for 15 minutes for the standard solvents. Detection limits, linearity, reproducibility and recovery of both SHS and PDMS-SPME methods have been determined using 6 standard solvents. Both methods were characterized by high reproducibility and good linearity. Using SHS methods, the mean recovery of the 6 standard solvents was ranged from 75.5% to 105.8% with a mean relative standard deviation (RSD) of 0.3% to 4.8%. With PDMS-SPME method, the mean recovery of the 6 standard solvents was ranged from 86.7% to 108.3% with a mean RSD of 0.4% to 2.5%. The detection limits of both methods were the same for toluene, cyclohexane and methyl ethyl ketone; those of PDMS-SPME method were higher than those of SHS method for methanol, isopropanol and ethyl acetate. PDMS-SPME fiber shoed excellent adsorption for non-polar solvents such as toluene, while it showed relatively low adsorption for polar solvents such as methanol.

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온도 조절이 가능한 트립신 전처리 반응침의 제작 (Fabrication of the temperature controllable microreactor for trypsin treatment)

  • 심태석;이국녕;주황수;김대원;김병기;김용협;김용권
    • 대한전기학회:학술대회논문집
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    • 대한전기학회 2003년도 추계학술대회 논문집 전기물성,응용부문
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    • pp.45-48
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    • 2003
  • In the research of proteomics, mass spectrometry analysis is the essential method for identification of the unknown proteins. Trypsin treatment for the sample preparation of mass spectrometry is the inevitable procedure[1]. However, sample preparation procedure is cumbersome and time consuming. To resolve these problems, Temperature controllable microreactor was designed and fabricated. It consists of metering chamber, micro channel, reaction chamber, platinum (Pt) thin film heater and a temperature sensor so that micro metering and mixture of reagent with temperature control can be done on the same chip. The total size of the fabricated microreactor was $37{\times}30{\times}1\;mm^3$ and the size of channel cross section was $200{\times}100{\mu}m^2$. PID temperature controller was realized using NI DAQ, PCI-MIO-l6E-1 board and LabVIEW program.

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Comparison of Two Methods to Extract DNA from Formalin-Fixed, Paraffin-Embedded Tissues and their Impact on EGFR Mutation Detection in Non-small Cell Lung Carcinoma

  • Hu, Yu-Chang;Zhang, Qian;Huang, Yan-Hua;Liu, Yu-Fei;Chen, Hong-Lei
    • Asian Pacific Journal of Cancer Prevention
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    • 제15권6호
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    • pp.2733-2737
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    • 2014
  • Objective: Molecular pathology tests are often carried for clinicopathological diagnosis and pathologists have established large collections of formalin-fixed, paraffin-embedded tissue (FFPE) banks. However, extraction of DNA from FFPE is a laborious and challenging for researchers in clinical laboratories. The aim of this study was to compare two widely used DNA extraction methods: using a QIAamp DNA FFPE kit from Qiagen and a Cobas Sample Preparation Kit from Roche, and evaluated the effect of the DNA quality on molecular diagnostics. Methods: DNA from FFPE non-small cell lung carcinoma tissues including biopsy and surgical specimens was extracted with both QIAamp DNA FFPE and Cobas Sample Preparation Kits and EGFR mutations of non-small cell lung carcinomas were detected by real-time quantitative PCR using the extracted DNA. Results and Conclusion: Our results showed that DNA extracted by QIAamp and Cobas methods were both suitable to detect downstream EGFR mutation in surgical specimens. Howover, Cobas method could yield more DNA from biopsy specimens, and gain much better EGFR mutation results.

시편의 성형방법이 반복삼축압축시험을 이용한 지반의 액상화 평가에 미치는 영향에 관한 연구 (A Study on the Effects of Sample Preparation on Liquefaction Estimation Using Cyclic Triaxial Test Conditions)

  • 이익효;김동수;김준석;황지훈;서성호
    • 한국지반공학회논문집
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    • 제19권2호
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    • pp.57-64
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    • 2003
  • 지진하중조건에서 포화된 모래의 액상화 가능성은 심도 있는 연구가 진행되어 왔다. 이러한 연구에서 대표적인것은 실험실에서 반복삼축압축시험에 의하여 모래의 반복강도를 결정하는 것이다. 본 연구는 재성형된 포화 균등모래의 액상화 특성에 있어서 시편의 성형방법에 따른 영향을 검증하기 위하여 수행되었다. 건조시료의 공기중낙하다짐, 습윤층다짐, 습윤진동층다짐 등 3가지 방법에 의하여 동일한 밀도로 다짐된 포화된 균등한 모래에 대하여 삼축압축시험이 수행되었다. 같은 밀도에서 다른 방법에 의하여 성형된 포화된 균등한 모래의 액상화 저항특성인 반복응력비는 크게 다른 것으로 확인되었다.

시료 준비 방법에 따른 등숙 시기별 초당 및 찰옥수수 교잡종의 과피 두께 비교 (Comparison of Kernel Sample Preparation Methods at Different Grain Filling Periods for Determining Pericarp Thickness in Super Sweet and Waxy Corn Hybrids)

  • 한성진;오태영;강민정;강종원;왕승현;박태춘;강건;정종욱;소윤섭
    • 한국작물학회지
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    • 제64권2호
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    • pp.102-108
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    • 2019
  • 본 연구는 식용옥수수 풋이삭의 식감의 결정에 영향을 미치는 과피의 두께를 측정하는 방법을 규명하기 위하여 과피 시료의 준비 방법에 따른 과피 두께의 차이와 등숙 시기별 과피 두께의 변화를 조사하기 위하여 수행하였다. 1. 찰옥수수와 초당옥수수 각 3품종의 시료를 수확 직후 생옥수수(생시료) 알곡을 바로 측정하거나 상온의 음지에서 완전(건조시료) 건조시키거나 $-4^{\circ}C$로 냉동시킨 후 과피를 측정하였다. 2. 시료 준비 방법과 등숙 시기에 따른 삼원 교호작용의 유의성이 인정되어 어느 한 요인에 대한 일반적인 결론을 도출하기 보다는 각 시료 준비 방법과 특정 등숙 시기에 따른 과피 두께의 비교를 수행하였다. 3. 초당옥수수는 건조시료에서 등숙이 진행됨에 따라 비교적 안정된 과피 두께 측정값을 얻을 수 있었으며 찰옥수수는 비해 모든 시료 준비 방법에서 초당옥수수보다 안정된 값을 보였다. 특히 풋찰옥수수 수확 적기인 수정 후 24일경에는 시료 준비 방법에 따른 차이는 크게 나타나지 않을 것으로 기대된다.

Analysis of Hypoxia-Inducible Factor Stabilizers by a Modified QuEChERS Extraction for Antidoping Analysis

  • Kim, Si Hyun;Lim, Nu Ri;Min, Hophil;Sung, Changmin;Oh, Han Bin;Kim, Ki Hun
    • Mass Spectrometry Letters
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    • 제11권4호
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    • pp.118-124
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    • 2020
  • An analytical method was developed for hypoxia-inducible factor (HIF) stabilizers based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) sample preparation and liquid chromatography-high resolution mass spectrometry analysis. HIF stabilizers potentially enhance the performance of athletes, and hence, they have been prohibited. However, the analysis of urinary HIF stabilizers is not easy owing to their unique structure and characteristics. Hence, we developed the QuEChERS preparation technique for a complementary method and optimized the pH, volume of extraction solvent, and number of extractions. We found that double extraction with 1% of formic acid in acetonitrile provided the highest recovery of HIF stabilizers. Moreover, the composition of the mobile phase was also optimized for better separation of molidustat and IOX4. The developed method was validated in terms of its precision, detection limit, matrix effect, and recovery for ISO accreditation. To the best of our knowledge, this is the first demonstration of the application of the QuEChERS method, which is suitable as a complementary analytical method, in antidoping.

Application of Rapid Sample Preparation Method and Monitoring for Cholesterol Content in Chicken Egg and Egg powder

  • Park, Jung-Min;Jeong, In-Seek;Kwak, Byung-Man;Ahn, Jang-Hyuk;Leem, Donggil;Jeong, Jayoung;Kim, Jin-Man
    • 한국축산식품학회지
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    • 제33권5호
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    • pp.672-677
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    • 2013
  • The aim of this study was to develop sample preparation method and evaluate the exact cholesterol content in egg and egg powder purchased from Korean markets, and to determine whether significant differences exist among various egg products, since a variety of products are available in Korean markets and there are no recent databases for cholesterol. To evaluate the cholesterol content in chicken egg sold in Korean local market, a simple method using non-heated saponification to determine cholesterol for emulsified foods was applied. The results of recovery for egg and egg powder were in a range of 92.4-105.0%, with a relative standard deviation between 1.1% and 2.8% by using gas chromatography-flame ionization detector. Therefore, the total cholesterol content in whole egg was estimated between 160.8 and 226.3 mg/egg (AV(average) $186.8{\pm}3.5$), which is similar or lower than previously reported levels. The value for cholesterol in egg powder was estimated between 2.94 and 3.49 mg/g (AV $3.23{\pm}0.15$). We suggested method that can be applicable to chicken egg and egg powder matrix as providing rapid and accurate determination of cholesterol in egg and egg powder. This information will be helpful for processed food producers for deciding food labels of cholesterol content.

Rapid Identification of Staphylococcus Species Isolated from Food Samples by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

  • Kim, Eiseul;Kim, Hyun-Joong;Yang, Seung-Min;Kim, Chang-Gyeom;Choo, Dong-Won;Kim, Hae-Yeong
    • Journal of Microbiology and Biotechnology
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    • 제29권4호
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    • pp.548-557
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    • 2019
  • Staphylococcus species have a ubiquitous habitat in a wide range of foods, thus the ability to identify staphylococci at the species level is critical in the food industry. In this study, we performed rapid identification of Staphylococcus species using Matrix-Assisted Laser Desorption/Ionization Time-of-Flight mass spectrometry (MALDI-TOF MS). MALDI-TOF MS was evaluated for the identification of Staphylococcus reference strains (n = 19) and isolates (n = 96) from various foods with consideration for the impact of sample preparation methods and incubation period. Additionally, the spectra of isolated Staphylococcus strains were analyzed using principal component analysis (PCA) and a main spectra profile (MSP)-based dendrogram. MALDI-TOF MS accurately identified Staphylococcus reference strains and isolated strains: the highest performance was by the EX method (83.3~89.5% accuracy) at species level identification (EDT, 70.3~78.9% accuracy; DT, less than 46.3~63.2% accuracy) of 24-h cultured colonies. Identification results at the genus level were 100% accurate at EDT, EX sample preparation and 24-h incubation time. On the other hand, the DT method showed relatively low identification accuracy in all extraction methods and incubation times. The analyzed spectra and MSP-based dendrogram showed that the isolated Staphylococcus strains were characterized at the species level. The performance analysis of MALDI-TOF MS shows the method has the potential ability to discriminate between Staphylococcus species from foods in Korea. This study provides valuable information that MALDI-TOF MS can be applied to monitor microbial populations and pathogenic bacteria in the food industry thereby contributing to food safety.

Quantitative analysis and validation of naproxen tablets by using transmission raman spectroscopy

  • Jaejin Kim;Janghee Han;Young-Chul Lee;Young-Ah Woo
    • 분석과학
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    • 제37권2호
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    • pp.114-122
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    • 2024
  • A transmission Raman spectroscopy-based quantitative model, which can analyze the content of a drug product containing naproxen sodium as its active pharmaceutical ingredient (API), was developed. Compared with the existing analytical method, i.e., high-performance liquid chromatography (HPLC), Raman spectroscopy exhibits high test efficiency owing to its shorter sample pre-treatment and measurement time. Raman spectroscopy is environmentally friendly since samples can be tested rapidly via a nondestructive method without sample preparation using solvent. Through this analysis method, rapid on-site analysis was possible and it could prevent the production of defective tablets with potency problems. The developed method was applied to the assays of the naproxen sodium of coated tablets that were manufactured in commercial scale and the content of naproxen sodium was accurately predicted by Raman spectroscopy and compared with the reference analytical method such as HPLC. The method validation of the new approach was also performed. Further, the specificity, linearity, accuracy, precision, and robustness tests were conducted, and all the results were within the criteria. The standard error of cross-validation and standard error of prediction values were determined as 0.949 % and 0.724 %, respectively.