• KSBB Journal
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• 제14권4호
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• pp.408-413
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• 1999

빠른 분석시간과 우수한 분리도를 가진 분석기기로서 크로마토그래피가 분취용으로 이용되기 위해서는 많은 시료양을 취급할 수 있어야 한다. 이 경우 충전물과 관의 크기가 커지게 되면 관의 효율은 분석용에 비해서 떨어지게 된다. 순도와 수율에 미치는 변수가 서로 복잡하게 연관되어 있기때문에 특히 분취용 조업조건의 최적화는 많은 경험과 실험이 요구된다. 또한 많은 상관된 실험변수들이 있고 분리하고자 하는 물질의 종류가 다양하기 때문에 수학적 모델을 적용하여 시료가 관내에서 거동 (behavior)을 예측하는 것이 쉽지 않다. 이러한 문제점을 해결하기 위해서 외국에서는 최소한의 실험을 통하여 고분가 가치 물질을 효율적이고 경제적으로 얻기 위한 크로마토그래피용 프로그램을 활발하게 이용하기 시작하였다. 인하대학교 고순도분리연구실에서 개발된 HCI 프로그램은 단지 LC에 국한된 것이 아니라 GC,SFC (supercritical fluid chromatography) 뿐만아니라 연속식 시스템인 SMB (simulated moving bed)까지 확장될 예정이다.

• 한국축산식품학회지
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• 제41권2호
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• pp.335-342
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• 2021

Vitamin B12 deficiency may lead to serious health issues in both infants and adults. A simple analytical method involving sample pretreatment with enzyme, followed by cyanide addition under acidic conditions; separation on an immunoaffinity column; and high-performance liquid chromatography (HPLC) was developed for the rapid detection and quantitation of vitamin B12 in powdered milk. Detection limit and powdered milk recovery were determined by quantitative analysis. The limits of detection and quantitation were 2.71 and 8.21 ㎍/L, respectively. Relative standard deviations of the intra-day and inter-day precisions varied in the ranges of 0.98%-5.31% and 2.16%-3.90%, respectively. Recovery of the analysis varied in the range of 83.41%-106.57%, suggesting that the values were acceptable. Additionally, vitamin B12 content and recovery in SRM 1849a were 54.10 ㎍/kg and 112.24%, respectively. Our results suggested that the analytical method, including the sample pretreatment step, was valid. This analytical method can be implemented in many laboratory-scale experiments that seek to save time and labor. Therefore, this study shows that immunoaffinity-HPLC/ultraviolet is an acceptable technique for constructing a reliable database on vitamin B12 in powdered milk containing starch as well as protein and/or fat in high amounts.

• 분석과학
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• 제21권4호
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• pp.284-295
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• 2008

플라스틱 시료 중 각종 유해물질 유무 확인을 위한 여러 가지 시험항목을 저비용으로 빠르게 분석할 수 있는 방법으로 Combustion ion chromatography(연소IC)를 사용한 방법을 채택하였다. F, Cl 및 Br의 3개 항목에 대하여 연소IC로 시험법 유효화 검증을 실시한 결과, 검량선은 0.5~4.0 mg/kg 농도범위에서 $r^2$ = 0.999~1.000의 상관관계 계수를 갖는 좋은 직선성을 나타내었으며, 검출한계는 0.005~0.024 mg/kg, 정량한계는 0.014~0.073 mg/kg 이였다. 인증표준물질(CRM)을 사용한 연소IC의 회수율은 95.5~104.9%이었다. 본 결과를 토대로 국내외 시험기관간 비교 숙련도 시험을 실시하였으며, 그 결과 연소IC 방법이 전기전자제품 중에 halogen-free 및 기타 유해물질 규제 대응을 위한 효율적인 분석방법임을 확인하였다.

• FOCUS: LIFE SCIENCE
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• 제1호
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• pp.8.1-8.3
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• 2024

Ultra-high performance liquid chromatography (UHPLC) systems are integral to modern analytical laboratories, necessitating careful maintenance and operation protocols to ensure optimal performance. This document provides comprehensive guidelines for the proper shutdown and reactivation of UHPLC systems to prevent damage and maintain operational efficiency. • Shutdown: Remove the column and replace it with a union to avoid blockages. Flush the system with a compatible solvent mix, clean mobile phase reservoirs to prevent microbial growth, flush the pump with storage solvent, and clean the autosampler, including the needle and injection port. • Reactivation: Inspect the system for wear or damage, gradually reintroduce mobile phases starting with a weak solvent, reinstall the column securely, and perform system checks on baseline stability, pressure consistency, and detector performance. By adhering to these guidelines, laboratories can ensure the longevity and reliability of their UHPLC systems, maintaining high analytical performance and minimizing downtime. These procedures help prevent common issues such as blockages, contamination, and component wear, thereby supporting efficient and accurate analytical operations.

• 식품과학과 산업
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• 제55권1호
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• pp.45-57
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• 2022

This study was proceeded the analytical methods using various analytical instruments for polycyclic aromatic hydrocarbons (PAHs) in food products. Various analytical methods were developed to determine levels of PAHs including benzo[a]pyrene, benzo[a]anthracene, benzo[b]fluoranthene, and chrysene formed in various food products using gas chromatography-mass spectrometry (GC-MS), enzyme-linked immunosorbent assay (ELISA) and raman spectroscopy. Recently, the rapid on-site response for the detection of hazardous substances in food aims to develop an onsite rapid detection of a simplified technical analysis method to reduce the time and cost required for analysis of PAHs. Current PAHs detection methods have been reviewed along with new raman spectroscopy analytical method.

• 한국환경과학회지
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• 제6권2호
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• pp.183-187
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• 1997

유기인제 농약을 70% acetone으로 추출한 다음 dlchloromethane 층으로 옮겨 추출물을 florisil로 충진된 open-column에서 chromatography를 행하였다. 마지막 추출물을 nitrogen-phosphorus detector(GC/NPD)을 가진 GC로 분석하였다. Narrow-bore capillary GC(Ultra-2)에 대해 18 가지의 유기인제 농약의 회수율이 88.7%에서 100.0%에 달하였다. 본 분석 방법의 최소 검출 준위는 0.019 - 0.035 mg/kg 이었으며 sample throughput(추출, open-column chro-matography 및 GC 분석)도 상당히 개선되었다.(sample당 8시간)

• 분석과학
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• 제7권3호
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• pp.403-411
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• 1994

본 실험은 알팔파의 Allelopathy와 Autotoxicity에 관련되는 생리활성 물질의 분리, 정제, 동정하기 위하여 실시되었다. 알팔파 생잎 1kg을 80% MeOH로 추출하여 silica gel TLC와 DCCC의 분리와 정제과정을 거쳐 HPLC로 동정하였다. HLPC 분석결과 4개의 phenolic 물질(salicylic acid, rutin, quercetin, scopoletin) 등이 동정되었다. 이들 물질을 이용한 발아실험에서도 모두 알팔파의 발아와 생육에 억제적으로 작용하였으며, 이 중 quercetin의 처리가 가장 억제적이었다. 따라서 최소한 이들 물질이 알팔파의 Allelopathy와 Autotoxicity에 관련하는 것으로 생각되었다.

• Bulletin of the Korean Chemical Society
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• 제33권6호
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• pp.1967-1971
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• 2012

A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg.

• 분석과학
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• 제36권6호
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• pp.281-290
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• 2023

Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate N-nitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 1-50 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.

• 한국산업보건학회지
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• 제10권1호
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• pp.126-146
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• 2000

To develop and evaluate formaldehyde measurement method using 2,4-dinitro-phenylhydrazine (2,4-DNPH) coated sampler and gas chromatography, laboratory test and field test were conducted. Results of this study are as follows. Limit of detection(LOD) of measurement methods, HPLC-UVD, GC-NPD and GC-FID, is $0.008{\mu}g/m{\ell}$ $0.060{\mu}g/m{\ell}$, $0.472{\mu}g/m{\ell}$ respectively. Coefficiency of measurement methods, HPLC-UVD, GC-NPD and GC-FID, is 0.008, 0.009, 0.020 respectively. Desorption efficiency of sep-pak xposure aldehyde sampler and sorbent sample tube is 1.05(range : 0.99 - 1.12), 1.02(range : 0.99 - 1.06) respectively. Samples of sorbent sample tube and sep-pak xposure aldehyde sampler turned out to be stored at refrigerator, according to storage test results. Measurement methods of HPLC-UVD, GC-NPD, GC-FID, according to results of precision for the combined sampling and analytical procedure, became acceptable to OSHA evaluation standard. Field test using exposure chamber met the NIOSH overall uncertainty recommendation(less than 25%). Overall uncertainty of Sepak-HPLC(UVD), Tube-GC(NPD), Tube-GC(FID) is 11.0% - 17.0%. Consequently gas chromatography(GC-NPD, GC-FID) and high performance liquid chromatography(EPA TO-11) using 2,4-DNPH coated sampler for formaldehyde measurement turned out to be suitable to measure personal formaldehyde exposure at workplaces.