• 분석과학
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• 제34권1호
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• pp.9-16
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• 2021

In the group of commonly prescribed β-blocker drugs, one of the enantiomers is generally relatively more active than the others. This study aims to develop a technique for the chiral analysis of select β-blockers based on proton nuclear magnetic resonance (1H-NMR) spectrometry. (S)-2-Tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid ((S)-TBMB) was synthesized and utilized as a chiral derivatizing agent. Pure β-blocker enantiomers were isolated from racemates by semi-preparative liquid chromatography prior to derivatization. The reaction time and concentration of (S)-TBMB were controlled to improve the derivatization procedure. No racemization was found during the analysis. High-performance liquid chromatography (HPLC) analysis was also performed for comparative purposes. High agreement between the NMR and HPLC methods was achieved in the determination of (R)-metoprolol in a standard solution of the (S) isomer.

• 생약학회지
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• 제54권1호
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• pp.38-43
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• 2023

A simple and accurate assay was developed for the quantitative analysis of 1-deoxynojirimycin (1-DNJ) derived from the silkworm (Bombyx mori). Normal-phase high-performance liquid chromatography coupled with an evaporative light scattering detector (HPLC-ELSD) and a hydrophilic interaction liquid chromatography column was used. Various parameters were applied to optimize the analysis method. The limits of detection and quantification of 1-DNJ were 2.97 × 10^-3 and 9.00 × 10^-3 mg/mL, respectively. The calibration curve showed good linearity results. The concentration range and the r² value were 0.0625-1.0 mg/mL and 0.9997, respectively. The accuracy test demonstrated a significantly high recovery rate (89.95-103.22%). The relative standard deviation was ≤ 1.00%. Thus, a method for the accurate identification and quantitative analysis of 1-DNJ in silkworms was developed. Moreover, in this procedure, the process of derivatization of 1-DNJ, which was required in previous experiments, could be eliminated. This technique may be actively utilized for the development of pharmaceuticals and health functional foods using 1-DNJ.

• 대한임상검사과학회지
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• 제47권4호
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• pp.306-312
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• 2015

알러지 반응이 일어나면 histamine이 방출되기 때문에 histamine을 정량 측정함으로써 유발된 알러지의 정도를 확인 할 수 있다. 일반적으로는 항원-항체반응으로 microplate reader를 이용하여 흡광도를 측정하여 정량 한다. 본 연구에서는 histamine 방출량을 측정함에 있어서 일반적인 항원-항체반응과 분석 화학적인 방법으로 HPLC-MS를 이용한 방법을 비교하였다. 세포주는 RBL-2H3를 사용하였고, C48/80으로 자극시켜 알러지를 유발하였다. 유발된 알러지는 ${\beta}$-hexosaminidase의 측정으로 탈 과립을 확인하였으며 실험의 정당성을 위하여 세포독성 능을 확인하였다. Histamine 정량에서 항원-항체반응에 의한 측정의 정량한계는 10.257 ppm이었고, HPLC-MS에 의한 정량한계는 0.020 ppm으로 현저한 차이를 보였다. 알러지 활성 및 항 알러지 실험에 있어서 histamine의 측정은 HPLC-MS를 이용한 분석이 더 정밀하고 정확한 실험인 것을 확인하였다.

• 한국해양학회지:바다
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• 제20권2호
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• pp.71-77
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• 2015

High-Performance Liquid Chromatography (HPLC) 분석방법은 식물플랑크톤의 생물량 및 일차생산력을 추정하기 위한 지시자로서 chlorophyll a 농도를 측정하고 carotenoids의 종류를 파악해 종조성을 확인하기 위해 널리 이용되고 있다. 그러나 대량시료의 분석에 요구되는 시료 전처리 과정 중 여과지 분쇄는 상당한 시간과 숙련이 요구된다. 본 연구에서는 엽록소 및 carotenoids의 정량분석에 대한 여과지 분쇄의 영향을 파악하고자 동해 남서부 해역의 시료를 이용해 여과지 분쇄 전후의 광합성 색소 농도를 비교 평가했다. HPLC 분석에서 여과지 분쇄 생략 시 Chl a의 경우 평균 45% 과소평가되었다. 또한 pico, nano 크기 식물플랑크톤의 지표색소인 Zeaxanthin, 19'-butanoyloxyfucoxanthin, 19'-hexanoyloxyfucoxanthin는 최대 77~85% 과소평가되었다. 크기가 작은 식물플랑크톤의 경우 여과지 분쇄가 생략될 경우 불완전한 추출로 지표색소의 농도가 실제보다 저평가될 가능성이 크다는 것을 확인하였다. 따라서 HPLC 분석에서 여과지 분쇄 생략 시 Chl a 뿐 아니라 carotenoids 또한 과소평가 되므로 모든 경우에서 여과지 분쇄 과정이 반드시 필요하다고 판단된다.

• 한국응용과학기술학회지
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• 제10권1호
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• pp.1-8
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• 1993

The possibilities for HPLC analysis of lipids have been revolutionised by the availability of evaporative light-scattering detectors, with which the response is independent of the nature of the mobile phase and does not depend On the presence of specific chromophores in the lipids. It was thus possible to develop an HPLC procedure, involving ternary gradient elution, for separating all the lipid classes in animal tissues in a single step. Although reversed-phase HPLC has been widely used for the analysis of molecular species of lipids, sliver ion chromatography can be a valuable alternative. For example, a stable silver ion column for HPLC was developed which permitted resolution of molecular species of triacylglycerols, even from such complex samples as fish oils, again With light-scattering detection and gradient elution. The capacity for HPLC resolution of diastereomeric diacyl-sn-glycerol derivatives, prepared from triacylglycerols. has lead to a new simple method for stereospecific analysis of the latter.

• Archives of Pharmacal Research
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• 제9권1호
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• pp.5-9
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• 1986

Partialy purified ginseng proteins were either treated with sodium dodecyl sulfate (SDS) and .betha.-mercaptoethanol to denature the proteins or not, and subjected to Thin Layer Chromatography (TLC) and High Performance Liquid Chromatography (HPLC) to compare the components of each fraction. Standard proteins of known molecular weights (MW) were also either treated with SDS and .betha.-mercaptoethanol or not, and subjected to HPLC to obtain regression lines for MW determination. From the retention times obtained from samples in eiether case by HPLC, the MW were estimated as following in SDS treated condition, Gl fraction showed three peaks each with MW of above 100, 000, 51, 000 and 19, 000. Gll showed one original peak with MW of 21, 000 and Gll, two peaks each with MW of 19, 000 and 14, 000. On the other hand, in non-SDS treated condition, GI fraction showed two peaks each with MW of above 200, 000 NA 52, 000. Gll showed one original peak with MW of 41, 000 and Gill, three peaks each with MW of 28, 000, 19, 000 and 14, 000.

• 생명과학회지
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• 제10권2호
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• pp.115-124
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• 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
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• 제39권5호
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• pp.488-493
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• 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.

• 분석과학
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• 제26권6호
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• pp.357-363
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• 2013

Selenium-containing proteins were separated from selenium-enriched yeast (SEY) using Trizol$^{(R)}$ reagent followed by anion exchange (AE) chromatography. This method is simpler and less time consuming than electrophoresis. Five selenium containing proteins were identified by on-line AE HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry). Each protein was enzymatically hydrolyzed to seleno-amino acids and separated with RP (reverse phase) HPLC for the identification of selenoproteins.

• Food Science and Biotechnology
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• 제18권2호
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• pp.561-564
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• 2009

A high performance liquid chromatography (HPLC) method has been developed for determination of 11 ginsenosides in black ginseng (BG, white ginseng that is subjected to 9 cycles of $95^{\circ}C$ for 3 hr). After eluted by gradient elution of water-acetonitrile without buffer in 70 min, 11 ginsenosides in BG were identified. The proposed method provided good linearity ($R^2$>0.9995), accuracy (92.2-106.6%), and intra- and interday precision (RSD<2.6%). In addition, ginsenosides compositions in white, red, and black ginsengs were investigated using this method, respectively. Interestingly, in BG, the content of ginsenoside $Rg_3$ which does not existed in white ginseng was 7.51 mg/g, approximately 20 times than that in red ginseng.