• Title/Summary/Keyword: Analytical Chromatography

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Use of HCI Program for Optimization of Operating Conditions in Analytical and Preparative Chromatography (분석 및 분리용 크로마토그래피에서 조업조건의 최적화를 위한 HCI 프로그램의 이용)

  • Lee, Ju-Won;Lee, Min-U;No, Gyeong-Ho
    • KSBB Journal
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    • v.14 no.4
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    • pp.408-413
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    • 1999
  • To separate mixtures analytically and preparatively by LC (Liquid Chormatography), the operating conditions of analytical chromatography should be determined. The HCI program was utilized to find the optimum operating condition accurately and rapidly, and to reduce the number of experiments. In an analytical chromatography, based on the resolution and analysis time, the experimental conditons of deoxyribonucleosides and phopholipids were fixed in terms of taxol was calculated, and the collection time was predicted for the mixture of 5'-IMP and 5'-GMP from the elution profile when and purity wer known.

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Development of Pretreatment Method for Analysis of Vitamin B12 in Cereal Infant Formula using Immunoaffinity Chromatography and High-Performance Liquid Chromatography

  • Park, Jung Min;Koh, Jong Ho;Kim, Jin Man
    • Food Science of Animal Resources
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    • v.41 no.2
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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.

Determination of halogen elements in plastics by using combustion ion chromatography (연소IC를 이용한 플라스틱 중 할로겐 물질 정량)

  • Jung, Jae Hak;Kim, Hyo Kyoung;Lee, Yang Hyoung;Lee, Lim Soo;Shin, Jong Keun;Lee, Sang Hak
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.284-295
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    • 2008
  • For plastics samples, a method using combustion ion chromatography was selected as a method for rapid low-cost analysis to test whether hazardous substances are contained or not. Using combustion ion chromatography, a verification test for F, Cl and Br compounds generated a linear calibration curve with a correlation coefficient of $r^2$ = 0.999~1.000 in the calibration range from 0.5 to 4.0 mg/kg. The detection limits were found to be 0.005~0.024 mg/kg and quantitative limits were found to be 0.014~0.073 mg/kg. The recoveries of combustion ion chromatography using certified reference material (CRM) were found to be 95.5~104.9%. Based on these results, a proficiency test was conducted together with several laboratories in and out of the country, to make comparative analysis of the results from each laboratory. As a result, the data supported the use of combustion ion chromatography as an effective analysis method to deal with regulations for halogen-free electronic products and for other hazardous substances in the electronic products.

A study on analytical methods for polycyclic aromatic hydrocarbons in foods (식품 중 다환방향족탄화수소 분석법 연구)

  • Kim, Yong-Yeon;Shin, Han-Seung
    • Food Science and Industry
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    • v.55 no.1
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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.

Study on the Development of Analytical Method (Multi-Pesticide Residue Method) for Organophosphate Pesticides (유기인제 농약 분석 방법 (Multi-Pesticide Residue Method) 개발에 관한 연구)

  • 이봉헌;김우성
    • Journal of Environmental Science International
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    • v.6 no.2
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    • pp.183-187
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    • 1997
  • Organophosphate pesticides were extracted with 70% acetone and then transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil. The florial extract was analyzed by gas chromatography with nitrogen-phosphorus detector(GC/NPD). Recoveries of the 18 organophosphate pesticides were ranged from 88.7% to 100. 0% for the narrow-bore capillary GC(Ultra-21. The minimum detectable level of this analytical method was 0.019 - 0.035 mg/kg. Sample throughput(extraction, open-column chro- matography, and GC analysts) was decreased considerably (8h per sample).

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SEPARATION, IDENTIFICATION OF BIOACTIVE COMPOUNDS FROM ALFALFA PLANT (알팔파의 생리활성물질 분리 및 동정)

  • Chung, Ill-Min;Kim, Ki-June
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.403-411
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    • 1994
  • To isolate, purity and identify of bioactive compounds involved in alfalfa allelopathy and/or autotoxicity, experiment was conducted. Isolation and separation procedures used from an 80% methanol extract of fresh alfalfa leaves(1kg), silica gel thin layer chromatography(TLC), followed by Droplet Counter Current Chromatography(DCCC). Preliminary identification was examined by high preformance lipid chromatography(HPLC). Four phenolic compound, salicylic acid, scopoletin, rutin, and quercetin, were identified and identified all compounds were phytotoxic to alfalfa seed germination and seedling growth. Among these compounds, quercetin treatment($10^{-3}M$) was most inhibitory to alfalfa seed germination and seedling growth. These compounds may be, at least in part, involved autotoxicity and allelopathy.

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An Investigation on the Extraction and Quantitation of a Hexavalent Chromium in Acrylonitrile Butadiene Styrene Copolymer (ABS) and Printed Circuit Board (PCB) by Ion Chromatography Coupled with Inductively Coupled Plasma Atomic Emission Spectrometry

  • Nam, Sang-Ho;Kim, Yu-Na
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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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.

Determination of N-nitrosodimethylamine in zidovudine using high performance liquid chromatography-tandem mass spectrometry

  • Yujin Lim;Aelim Kim;Yong-Moon Lee;Hwangeui Cho
    • Analytical Science and Technology
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    • v.36 no.6
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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.

Analytical method for analyzing formaldehyde using 2, 4-DNPH and gas chromatography/FID, NPD (2,4-DNPH와 가스크로마토그래프를 이용한 포름알데히드 분석방법)

  • Jeong, Jee Yeon;Park, Seung Hyun;Yi, Gwang Yong;Oh, Se Min
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.10 no.1
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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.

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