• Journal of Applied Biological Chemistry
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• 제59권2호
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• pp.107-112
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• 2016

Pectolinarin was isolated from the ethyl acetate fraction of Cirsium setidens using open column chromatography and was analyzed using spectrometry. Pectolinarin content in Cirsium spp. was determined using HPLC/UV. Pectolinarin content in the aerial part of Cirsium spp. was higher than that in the root and pappus. Pectolinarin content was highest in the aerial part of C. chlorolepis (110.65mg/g extract). Consequently, the aerial part of C. chlorolepis has potential for use in new natural medicinal products, health supplements, and beverages.

• Bulletin of the Korean Chemical Society
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• 제27권2호
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• pp.291-294
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• 2006

A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC $C_{18}$ column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

• 한국잡초학회지
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• 제8권3호
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• pp.258-264
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• 1988

밭 주요(主要) 우점잡초(優占雜草) 중 allelopathy 작용성(作用性)을 보였던 쑥, 냉이, 쇠비름 및 토끼풀에 대하여 이들 잡초(雜草) 중에 존재(存在)하는 phenol화합물(化合物)을 Paper chromatography(PC) 및 High performance liquid chromatography(HPLC)에 의하여 분리(分離) 확인(確認)하였고, 검출(檢出)된 phenol화합물(化合物)이 검정식물(檢定植物)의 발아(發芽) 및 생장(生長)에 미치는 영향(影響)을 검토(檢討)하였다. PC에 의하여 검정(檢定)된 phenol화합물(化合物)은 4초종(草種) 모두에서 methanol추출물(抽出物) 보다는 물추출물(抽出物)에서 많은 종류(種類)가 확인(確認)되었다. 4초종(草種)의 두가지 추출물(抽出物) 모두에서 PC로 분리(分離)된 phenol화합물(化合物)은 ferulic acid이었으며, benzoic acid는 물추출물(抽出物)에서만 확인(確認)되었다. HPLC에 의해서는 hydroquinone, p-hydroxybenzoic, ferulic 및 cinnamic acid가 전초종(全草種)에서 분리(分離)되었다. PC 및 HPLC로 분리(分離) 확인(確認)된 phenol화합물(化合物) 중 p-hydroxyhenzoic, ferulic 및 cinnamic acid는 검정식물(檢定植物)의 발아(發芽) 및 발아후(發芽後) 생육(生育)에 높은 억제효과(抑制效果)를 보였다. 이들 phenol화합물(化合物)은 일반적(一般的)으로 발아(發芽)보다는 유묘(幼苗)의 근생장(根生長)에 더 큰 저해(沮害)를 나타내었다.

• Macromolecular Research
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• 제15권2호
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• pp.134-141
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• 2007

The direct chromatographic separation of enantiomers by chiral stationary phases (CSPs) has been extensively developed over the past two decades, and has now become the most popular method for the analytical and preparative separations of enantiomers. Polysaccharide derivatives coated onto silica gel, as CSPs, playa significantly important role in the enantioseparations of a wide range of chiral compounds using high-performance liquid chromatography (HPLC). Unfortunately, the strict solvent limitation of the mobile phases is the main defect in the method developments of these types of coated CSPs. Therefore, the immobilization of polysaccharide derivatives onto silica gel, via chemical bonding, to obtain a new generation of CSPs compatible with the universal solvents used in HPLC is increasingly important. In this article, our recent studies on the immobilization of polysaccharide derivatives onto the silica gel, as CSPs, through radical copolymerization with various vinyl monomers are reported. Polysaccharide derivatives, with low vinyl content, can be efficiently fixed onto silica gel with high chiral recognition.

• 분석과학
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• 제34권4호
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• pp.160-171
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• 2021

Synthetic azo dyes are used extensively in herbal medicines to render the medicines more visually attractive to consumers. This study developed and validated a rapid high-performance liquid chromatography (HPLC) method to determine whether synthetic colorants such as Tartrazine, Auramine O, Metanil yellow, Sunset yellow, and Orange II are used extensively in Typha orientalis. To increase the recovery of the synthetic dyes, this method employed containing 50 mM ammonium acetate in 70 % methanol at first extraction and 100 mM HCl in 70 % methanol at second extraction. Five synthetic pigments in Typha orientalis were separated by gradient elution with a mobile phase consisting of acetonitrile and 50 mM ammonium acetate in distilled water at ultra-violet (UV) detection 428 nm or 500 nm. Additionally, this study established the liquid chromatography tandem mass spectrometry (LC-MS/MS) method to confirm positive samples suspected by HPLC results. The HPLC-UV method had good linearity, indicating r²> 0.999. The recoveries of the samples spiked with three different concentration ranged from 73.8~91.5 %, and relative standard deviation values indicated 0.2~5.2 %. The established LC-MS/MS could successfully identify the synthetic pigments in herbal medicine samples. The study demonstrates that Typha orientalis adulterated by yellowish synthetic dyes can be successfully distinguished when using the HPLC-UV method.

• 한국식품저장유통학회지
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• 제30권1호
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• pp.28-41
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• 2023

Non-aflatoxigenic Aspergillus oryzae and aflatoxigenic A. flavus cannot be clearly identified by partial sequencing of the internal transcribed spacer (ITS) and 18S ribosomal ribonucleic acid (18S rRNA) regions. This study aimed to compare the accuracy among three aflatoxin detection methods using ultra-performance liquid chromatography (UPLC), high-performance liquid chromatography (HPLC), and an enzyme-linked immunosorbent assay (ELISA) kit and to select the non-aflatoxigenic Aspergillus sp. isolated from soybean paste. All analytical methods were suitable according to the international standards of Codex Alimentarius FAO-WHO (CODEX) or the Ministry of Food and Drug Safety (MFDS). UPLC exhibited the best of limit of detection (LOD) and limit of quantification (LOQ). Based on UPLC, HPLC, and the ELISA kit assay, the P5 and P7 strains isolated from soybean paste had 1,663.49, 1,468.12, and >20 ㎍/kg and 1,470.08, 1,056.73, and >20 ㎍/kg, respectively, detected and re-identified as A. flavus. In contrast, the P3 and P4 strains (A. oryzae), which were detected below the MFDS standards in all assays, were confirmed as non-aflatoxigenic fungi. Among the methods evaluated for quantitative analysis of aflatoxin, UPLC and HPLC are superior in terms of accuracy, and the ELISA kit rapidly detects low concentrations of aflatoxin. Furthermore, this study demonstrates that any Aspergillus sp. isolated for use as a fermentation starter should be analyzed for potential aflatoxin production using UPLC and HPLC for accurate quantitative analysis or ELISA for the rapid detection of low-level concentrations of aflatoxin.

• 보존과학회지
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• 제31권3호
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• pp.299-308
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• 2015

본 연구는 1996년 천안시 유량동에서 출토된 분홍색 단령의 염료 동정을 통해 조선시대에 사용된 적색 염료를 실증하기 위한 것이다. 이를 위해 유물에 사용된 염료를 추출하고 이것을 당시 염색에 사용되었을 것으로 추정되는 적색계 염료(홍화, 소목, 꼭두서니)에서 추출한 염료와 함께 고성능액체크로마토그래피분석을 실시하였다. 그 결과 유물에서 추출한 염료와 홍화염색포의 추출 염료는 같은 시간대인 17.5분에서 피크가 나타났다. 이때 자외/가시선 분광 분석 결과는 두 시료 모두 519nm에서 최대흡수파장이 나타나 기존 홍화의 홍색소 분석 결과와 같은 것으로 조사되었다. 또한 negative ion mode에서 질량분석을 실시한 결과 유물과 홍화 염색포에서 추출한 염료 시료는 carthamin의 분자량인 910을 나타내는 m/z 909에서 같은 시간대의 피크가 확인되었다. 이와 같은 결과로 이 분홍 단령 직물을 염색하는데 사용된 염재는 홍화인 것으로 동정되었다.

• 생약학회지
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• 제41권4호
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• pp.313-318
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• 2010

Guibi-tang, a traditional herbal medicine, is used for anti-oxidant, anti-osteoporosis, hemostasis and gastroprotection. To develop an analysis method of simultaneous determination of six compounds, swertisin, decursinol, glycyrrhizin, 6-gingerol, costunolide and decursin in Guibi-tang, a high performance liquid chromatography was used with diode array detector. Six bioactive components were separated on a SHISEIDO $C_{18}$ column ($5\;{\mu}m$, 4.6 mm I.D.${\times}$250 mm) with column temperature $30^{\circ}C$. The gradient elution was composed of water with 0.1% trifluoroacetic acid (TFA) and acetonitrile. UV wavelength was set at 230 nm, 254 nm and 330 nm, respectively. Calibration curve showed good linear regression ($R^2$ > 0.9999). The limits of detection (LOD) and the limits of quantification (LOQ) ranged in 0.03 - 0.23 ${\mu}g/ml$ and 0.08 - $0.70\;{\mu}g/ml$, respectively. The RSD values of intra- and inter-day test were in the range of 0.03 ~ 0.96% and 0.01 ~ 1.46%, respectively. The evaluated results of accuracy test were varied from 92.28% ~ 105.14% with RSD < 1.60%. In conclusion, this developed simultaneous determination method was accuracy and sensitive to the quality evaluation of Guibi-tang.

• Environmental Analysis Health and Toxicology
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• 제29권
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• pp.18.1-18.9
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• 2014

Objectives The purpose of this study was to determine a separation method for each arsenic metabolite in urine by using a high performance liquid chromatography (HPLC)-inductively coupled plasma-mass spectrometer (ICP-MS). Methods Separation of the arsenic metabolites was conducted in urine by using a polymeric anion-exchange (Hamilton PRP X-100, $4.6mm{\times}150mm$, $5{\mu}m$) column on Agilent Technologies 1260 Infinity LC system coupled to Agilent Technologies 7700 series ICP/MS equipment using argon as the plasma gas. Results All five important arsenic metabolites in urine were separated within 16 minutes in the order of arsenobetaine, arsenite, dimethylarsinate, monomethylarsonate and arsenate with detection limits ranging from 0.15 to $0.27{\mu}g/L$ ($40{\mu}L$ injection). We used G-EQUAS No. 52, the German external quality assessment scheme and standard reference material 2669, National Institute of Standard and Technology, to validate our analyses. Conclusions The method for separation of arsenic metabolites in urine was established by using HPLC-ICP-MS. This method contributes to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies for arsenic exposure in South Korea.

• 한국가금학회지
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• 제31권3호
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• pp.137-143
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• 2004

The fractional synthesis rates(FSR) were measured with 2l-wk and 3l-wk-old broiler breeder pullets and hens to investigate the effect of sexual maturity on FSR. The FSR were obtained from chicken tissues and blood samples using High-Performance Liquid Chromatography/Mass Spectrometry(HPLC/MS). A L-l-13C, 15N -leucine saline solution was infused by bolus injection as a tracer into broiler breeder pullets in the experiment. A rapid HPLC/MS method was developed to measure the isotopic enrichments of leucine in plasma, tissue samples, and eggs. The enrichments of stable isotope leucine incorporated into protein and the enrichments of the stable isotope free leucine were measured in liver, breast muscle and blood samples. Two sets of experiments were conducted. In experiment one, 2l-wk-old, sexually immature broiler breeder pullets were divided into groups of three and blood samples were collected at 20 or 30 min intervals until 1.5 h from initial injection. The pullets were sacrificed in groups of three at varying time intervals for 7 h after injection. The liver, breast muscle and blood samples were removed for analysis. The FSR were estimated to be 8.7l%/day for liver, 4.06％/day for breast muscle, and 5.08％/day for blood samples in 30 minutes after injection from the enrichment ratios. In experiment two, sexually matured 3l-wk-old broiler breeder hens were assorted into groups of three and blood samples were obtained at 20 or 30 min intervals for 2 h. The FSR for blood samples were determined. The broiler breeder hens were sacrificed in groups of three at various time intervals until 7 h after injection and liver, breast muscle and blood samples were removed for analysis. The FSR were calculated to be 5.96％/day for liver. Eggs were collected from five chickens daily for 10 days after large bolus injection. The average of total enrichments of stable isotope in egg albumin was increased by 0.064% at 4 days after injection and was back to normal in 7 days.