• Food Science and Biotechnology
• /
• 제15권2호
• /
• pp.220-226
• /
• 2006

Component having antioxidant activity on lard during heating was separated from hexane extract of spinach, and its characteristic chemical structure was speculated through nuclear magnetic resonance spectroscopy, liquid chromatography-mass spectrometry, and Fourier transform infrared spectrophotometry. Lard was heated with hexane-, ethyl ether-, ethyl acetate-, or ethanol extract of spinach at $180^{\circ}C$ for 20 hr. Hexane extract of spinach, having highest antioxidant activity on lard during heating, was fractionated by silicic acid column chromatography (SACC), and SACC fractions having higher antioxidant activity on lard during heating were further separated by thin layer chromatography (TLC). Isolated compound from SACC fractions of hexane extract of spinach by TLC had sugar moieties and benzene ring along with hydroxy, carbonyl, and alkyl groups in the structure.

• 고려인삼학회:학술대회논문집
• /
• 고려인삼학회 1980년도 학술대회지
• /
• pp.53-57
• /
• 1980

Red ginseng powder was administered at a dose of 2.7 g per day for 3 months to 21 diabetic patients who were under the treatment with insulin. It was found that the ginseng powder was effective to 12 patients and ineffective to 9 patients. Based on these clinical results, experiments were carried out to elucidate factors which concerned with improvement of pathological conditions of diabetes mellitus. In the previous symposium, we reported that red ginseng powder contained an anti-lipolytic peptide, or an insulin-like peptide. In the course of purification of the insulin-like peptide in the ginseng, we found another fraction which possessed anti-lipolytic activity. The anti-lipolytic factor of the fraction was purified by gel filtration on Bio Gel P-2 column and Dowex $50W{\times}4$ column chromatography. The character of the finally purified material was examined by thin-layer chromatography, high-speed liquid chromatography and mass spectrometry. With these examinations, the active principle was indentified to be adenosine. Pharmacological significance of these insulin-like substances, the peptide and adenosine, was discussed.

• 생명과학회지
• /
• 제10권2호
• /
• pp.115-124
• /
• 2000

The present study was undertaken to separate the available components effectively, such as tetrodotoxin(TTX), docosahexaenoic acid(DHA, C22:6,ω-3) and eicosapentaenoic acid (EPA, C20:5,ω -3) from pufferfish liver waste, which are known to have high values as bioactive materials. By using ultrafiltration, it was possible to separate high contents of 68mg TTX from pufferfish liver waste. In contrast, by activated charcoal column, it was to obtain about 54mg TTX. The recovering ratios were 65.3% and 45.0% in the two different methods of ultrafiltration and activated charcoal column, respectively. From the results of HPLC and gas chromatography-mass spectrometry(GC-MS), the obtained toxins were identified to be TTX and its derivatives. In addition, it was also possible to obtain 72.3g DHA and 11.4g EPA from 1kg of pufferfish liver by high performance liquid chromatography (HPLC). These amounts of DHA and EPA were also 17.70% and 1.04% in the total lipid of pufferfish liver oil from analysis of gas chromatography(GC), respectively.

• 한국식품과학회지
• /
• 제39권5호
• /
• pp.488-493
• /
• 2007

국내유통중인 곡류, 견과류 및 그 가공품 총 25품목, 393건의 시료에 대해 immunoaffinity column 정제방법을 이용하여 총아플라톡신 오염실태를 조사하였으며, 그 결과 곡류 및 곡류가공품 6건, 견과류 및 견과류 가공품 37건에서 아플라톡신 오염이 확인되었으며 오염수준은 아플라톡신 $B_1$으로서 $0.04-2.65{\mu}g/kg$, 총아플라톡신으로서 $0.04-5.51{\mu}g/kg$ 범위로 나타났다. Immunoaffinity column 정제를 거쳐 HPLC-FLD로 분석한 결과 아플라톡신이 검출된 시료에 대해서 LC-MS/MS로 확인하였으며, 그 결과 모두 아플라톡신으로 확인되었다. 본 연구결과에서 나타난 곡류 및 견과류에 대한 아플라톡신 검출빈도 및 오염수준은 국내, 외 연구 결과와 유사하거나 비교적 낮게 나타났으며 국내 아플라톡신 기준 및 미국, CODEX에서 설정된 기준규격 이하로 검출되었다.

• 한국식품과학회지
• /
• 제43권2호
• /
• pp.224-229
• /
• 2011

시중 유통 중인 과자류, 빵, 떡류, 면류 및 선식 등 432건을 immunoaffinity column으로 정제하여 HPLC-FLD로 제랄레논에 대한 오염실태를 조사하였다. 제랄레논의 검량선은 결정계수($R^2$)가 0.999 이상으로 양호한 직선성을 보였고 검출한계 및 정량한계는 각각 2.0, $6.0{\mu}g/kg$, 회수율 80.2-98.4%이었으며 RSD가 0.82-6.40%로 양호한 재현성을 나타내었다. 제랄레논 모니터링 결과, 과자류 중 스낵과자류 66건 중 3건에서 $6.02-11.82{\mu}g/kg$ 검출되었고 비스킷 71건 중 2건에서는 $14.78-17.83{\mu}g/kg$ 검출되었다. 면류, 빵류 및 떡류에서는 제랄레논이 검출되지 않았으며 침출차 14건에서 최고 $53.76{\mu}g/kg$ 검출, 선식 24건 중 16건에서 가장 높은 검출율(66.7%)을 나타내었다. 전분 2건, 시리얼두유 1건에서 제랄레논이 각각 5.55-8.56, $10.26{\mu}g/kg$ 검출되었다. 제랄레논 모니터링 결과는 기준이 설정되어 있는 유럽연합(곡류분말: $75{\mu}g/kg$, 빵, 비스킷, 스낵, 아침식사대용 시리얼류: $50{\mu}g/kg$, 영아 및 유아용 시리얼류: $20{\mu}g/kg$) 기준이하의 수준이었으며 국내외 연구보고와 비교한 결과 낮거나 비슷한 수준으로 검토되었다. 연구결과 곡류가공품에 대한 제랄레논 오염수준은 높지 않았으나 지구 온난화로 기후변화에 민감한 곰팡이독소와 같은 자연독소의 발생 증가가 우려되므로 선제적으로 대응하는 안전관리가 요구된다.

• 한국식품과학회지
• /
• 제40권3호
• /
• pp.354-359
• /
• 2008

국내유통 중인 대두, 붉은콩, 검은콩 녹두 등 6품목의 두류 총 127건을 immunoaffinity column 정제방법 및 HPLC-FLD을 이용하여 제랄레논에 대한 오염실태를 조사하였다. 상관계수($R^2$) 0.999 이상으로 양호한 직선성을 보였고 검출한계 및 정량한계는 각각 2.0 ${\mu}g/kg$, 6.0 ${\mu}g/kg$, 회수율 82.2-98.4%로 나타났다. RSD가 0.82-6.40%로 양호한 재현성을 나타내었다. 모니터링 결과, 대두(백태) 27건 중 1건(3.7%)에서 37.62 ${\mu}g/kg$ 검출되었고 붉은콩(팥) 27건 중 12건 검출되어 44.4%의 검출율을 보였고 그 오염수준은 8.01-38.98 ${\mu}g/kg$이었다. 나머지 시료 검정콩 16건, 녹두 24건, 서리태(속청) 19건, 서목태(약콩) 14건에서는 모두 검출되지 않았다. 따라서 총 시료 127건 중 13건 검출되어 10.2%의 검출율을 보였고 그 오염수준은 8.01-38.98 ${\mu}g/kg$이었다, 검출시료 13건을 LCMS/MS로 확인한 결과 모두 제랄레논임이 확인되었다. 본 연구결과에서 나타난 두류의 검출빈도 및 오염수준은 유럽연합에서 설정된 기준규격 이하의 수준이었으나 곰팡이독소의 생성의 특이성을 고려한다면 지속적이고 광범위하게 오염실태 조사가 되어야 한다고 판단된다.

• 한국독성학회:학술대회논문집
• /
• 한국독성학회 2006년도 추계학술대회
• /
• pp.65-74
• /
• 2006

Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

• 한국식품위생안전성학회지
• /
• 제35권4호
• /
• pp.326-333
• /
• 2020

본 연구는 불법적으로 식품에 사용될 수 있는 부정물질 11종에 대한 안전관리 강화를 위해 정량 및 정성 분석이 가능한 HPLC-DAD와 LC-MS/MS를 검증하기 위해 수행되었다. 확립된 시험법은 AOAC 가이드라인에 따라 직선성, 정밀성, 정량한계 및 회수율 등을 통해 유효성을 확인하였다. 본 실험에서 정량한계를 포함하여 검량선을 작성하였고, 모두 0.99 이상의 직선성을 확인하였다. 또한 정확성은 LC (90.0-106%), LC-MS/MS (83.0-114%) 이고, 정밀도는10% 이하로 재현성이 우수하였다. 확립된 시험법은 식품 중 부정물질 안전관리 및 모니터링에 활용될 것으로 사료된다.

• 한국응용과학기술학회지
• /
• 제38권6호
• /
• pp.1568-1576
• /
• 2021

본 연구에서는 인체에 보다 안전한 천연 화장품보존제 발굴을 목표로 하여 인간유래 항균펩타이드 LL-37의 짧은 유사체인 FK-13을 화장품보존제로 사용하고자 연구를 진행하였다. 이를 위해 13개의 아미노산으로 구성된 FK-13 펩타이드를 고상 펩타이드 합성법로 합성하였고 reversed phase-high performance liquid chromatography (RP-HPLC)로 정제 후 liquid chromatography-mass spectrometry (LC-MS)를 이용하여 순도와 분자량을 확인하였다. 합성된 FK-13을 이용하여 미생물에 대한 방부력을 검정하였고 화장품에 적용 가능성을 살펴보았다. FK-13은 3개의 그람-양성균 (Staphylococcus aureus, Bacillus subtilis, Staphylococcus epidermidis)과 3개의 그람-음성균 (Escherichia coli, Salmonella typhimurium, Pseudomonas aeruginosa), 그리고 진균인 Candida glabrata 에서도 높은 항균 활성을 보였으며 넓은 항균활성 스펙트럼을 나타내었다. 이를 바탕으로 화장품보존제로서의 적합성을 확인하였다. 또한 FK-13은 고온에서 분자의 열안정성을 보였으며 기존의 천연 한방화장품 방부제 및 화학보존제들과의 항균활성 비교 실험에서도 보다 월등한 항균활성 효능을 나타내었다. 따라서 FK-13 펩타이드는 인체 친화적이고 효과적인 항균활성을 나타내므로, 기존 화학보존제를 대체할 새로운 천연 화장품보존제로 적용이 가능할 것으로 판단된다.

• Bulletin of the Korean Chemical Society
• /
• 제34권6호
• /
• pp.1684-1688
• /
• 2013

A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.