• 한국작물학회지
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• 제56권3호
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• pp.244-249
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• 2011

본 연구는 콩 함유 사포닌의 함량을 쉽고 빠르게 정량할 수 있는 방법을 개발하기 위하여 시도하였다. 사포닌 표준 물질인 soyasaponin I은 대두에서 직접 분리하여 동정하였고, 분석은 HPLC/MS/MS를 이용하였으며 그 결과는 다음과 같다. 1. DAD 또는 ELSD를 이용하여 분석할 때보다 전처리 과정을 획기적으로 줄일 수 있어 신품종 육성의 선발과 같은 대량의 분석에 적합하였다. 2. Soyasaponin I의 함량은 나물콩과 같은 소립종에서 대립종에 비해 함량이 유의하게 높은 것으로 나타났다.

• Fisheries and Aquatic Sciences
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• 제16권3호
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• pp.159-164
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• 2013

The mouse bioassay and high performance liquid chromatography (HPLC) post-column oxidation method are different methods of quantifying paralytic shellfish poisoning toxins. In this study, we compared their ability to accurately quantify the toxicity levels in two types of field sample (oysters and mussels) with different toxin profiles for routine regulatory monitoring. A total of 72 samples were analyzed by both methods, 44 of which gave negative results, with readings under the limit of detection of the mouse bioassay ($40{\mu}g/100g$ saxitoxin [STX] eq). In 14 oysters, the major toxin components were gonyautoxin (GTX) 1, -2, -3, -4, -5, decarbamoylgonyautoxin-2 (dcGTX2), and decarbamoylsaxitoxin (dcSTX), while 14 mussels tested positive for dcSTX, GTX2, -3, -4, -5, dcGTX2, neosaxitoxin (NEO), STX, and dcSTX. When the results obtained by both methods were compared in two matrices, a better correlation ($r^2=0.9478$) was obtained for mussels than for oysters ($r^2=0.8244$). Additional studies are therefore needed in oysters to investigate the differences in the results obtained by both methods. Importantly, some samples with toxin levels around the legal limit gave inconsistent results using HPLC-based techniques, which could have a strong economic impact due to enforced harvest area closure. It should therefore be determined if all paralytic shellfish poisoning toxins can be quantified accurately by HPLC, and if the uncertainties of the method lead to doubts regarding regulatory limits.

• 약학회지
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• 제56권5호
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• pp.280-287
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• 2012

A high-performance liquid chromatography (HPLC) combined with ultraviolet (UV) method for the simultaneous determination of ${\alpha}$-cyperone and nootkatone was developed for the quality control of Cyperus rotundus Linne. The separation was performed on a KR100-$5C_{18}$ ($4.6{\times}250mm$) column, and an elution gradient composed of methanol and water with a flow-rate of 1.0 ml/min. Detection wavelength was set at 254 nm. The optimum extraction for the detection of the ${\alpha}$-cyperone and nookatone was achieved by ultrasonic with methanol for an hour. Two marker compounds ${\alpha}$-cyperone and nootkatone in Cyperi Rhizoma showed good linearity ($R^2$ >0.999) in the concentration range of $12.5{\mu}g/ml$ to $200{\mu}g/ml$. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.04~1.23% and 0.08~0.68%, respectively, and the overall recoveries of 97.45~105.58% for the two compounds analyzed. Additionally, a difference was observed in the cluster analysis and principal component analysis between Cyperi Rhizoma in Korea and China. The result demonstrated that the principal component analysis is useful to distinguish between Cyperi Rhizoma in Korea and China.

• Journal of Ginseng Research
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• 제29권3호
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• pp.126-130
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• 2005

Ginseng saponins have been known as main active principles and are quantified as the index components of ginseng and its products for quality control. However ginseng saponins are easily hydrolyzed in acidic solutions of crude drug preparations. Due to the hydrolysis of saponins in acidic condition, it is generally difficult to determine ginseng saponins In crude drug preparations. Ginseng saponins, prosapogenins and sapogenins of crude drug extracts were quantified by HPLC. Ginseng saponins were quantified by HPLC on $Lichrosorb-NH_2$ column with acetonitrile/water/1-butanol(80:20:10, v/v). Ginseng $prosapogenin-Rg_2$ and $-Rg_2$ were extracted with ethyl acetate from $50\%$ acetic acid hydrolyzates of saponin fractions and quantified by HPLC on $Lichrosorb-NH_2$ column with acetonitrile/water(90:10, v/v). Ginseng sapogenins, panafadiol and panaxatriol, were extracted with diethyl ether from $7\%-sulfuric$ acid hydrolyzates of saponin fractions and quantified by HPLC on ${\mu}-Bondapak\;C_{18}$ column with acetonitrile/methano1/chloroform(83:10:7, v/v). These methods of analyses of sapogenins and prosapogenins were more useful for quality control than those of ginseng saponins in some of crude drug preparations.

• Archives of Pharmacal Research
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• 제29권4호
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• pp.339-342
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• 2006

A simple high performance liquid chromatographic (HPLC) method was developed for the determination of tolperisone in human plasma. Tolperisone and internal standard (chlorphenesin) were isolated from 1 mL of plasma using 8 mL of dichlormethane. The organic phase was collected and evaporated under nitrogen gas. The residue was then reconstituted with 300 mL aliquot of mobile phase and a 100 mL aliquot was injected onto the $C_{18}$ reverse-phased column. The mobile phase, $45\%$ methanol containing $1\%$ glacial acetic acid and $0.05\%$ 1-hexanesulfonic acid was run at a flow rate of 1 mL/min. The column effluent was monitored using UV detector at 260 nm. The retention times for tolperisone and the internal standard were approximately 7.1 and 8.4 min, respectively. The standard curve was linear with minimal intra-day and inter-day variability. The quantification limit of tolperisone in human plasma was 10 ng/ mL. The proposed method has been applied to the determination of pharmacokinetic profile of tolperisone in Koreans. The T max of tolperisone in Koreans $(0.94{\pm}0.42\;h)$ was not significantly differ from that reported in Europeans (0.5-1 h), but the mean half-life in Koreans $(1.14{\pm}0.27\;h)$ was shorter than that in Europeans $(2.56{\pm}0.2\;h)$. The proposed HPLC method is simple, accurate, reproducible and suitable for pharmacokinetic study of tolperisone.

• 생약학회지
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• 제52권3호
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• pp.186-191
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• 2021

We developed a method to identify and quantify 6-hydroxyluteolin 7-O-glucoside in the powder of Salvia plebeia (PS) using high-performance liquid chromatography coupled with diode array detector (HPLC/DAD) and equipped with reverse-phase INNO C18 column. The analytical method was optimized and validated using novel parameters. The obtained values for the limits of detection and quantification were 3.60 and 10.90 ㎍/mL, respectively. Calibration curve showed good linearity in the concentration range tested (0.00625-0.1 mg/mL, r² = 1.0000), high accuracy (96.2-101.4%), and precision values (RSD ≤ 0.27%). Our analysis support the use of our method for accurately identifying and quantifying 6-hydroxyluteolin 7-O-glucoside from PS in routine analyses and large-scale extraction processes for content determination.

• 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.

• 한국지하수토양환경학회지:지하수토양환경
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• 제14권1호
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• pp.51-60
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• 2009

HPLC에 의한 토양내 화약물질의 분석 방법을 최적화하기 위해 현재 실사격 훈련이 진행 중인 군사격장 2곳에서 토양시료를 채취하여 분석 실험을 수행하였다. 토양과 오염물질의 불균일도를 감안하여 segregation constant 와 homogeneity constant를 기준으로 산정한 결과, 화약물질의 분석을 위한 토양시료채취 최소량은 125g 이었다. 그리고 시료 전처리 과정인 추출단계에서 필요한 적정시료량과 추출액의 비율을 CV값에 근거하여 산정한 결과 토양 10g/ACN 20 mL가 가장 효과적이었다. 미국 EPA에서 지정한 화약물질 14종을 모두 분리하기 위한 HPLC의 용리 조건은 RP C18캘럼을 이용하여 칼럼온더 30${\circ}C$일 때, 이동상 구성 및 유량은 isopropanol : acetonitrile : water의 비율 18 : 12 : 70, 유량 0.80mL/min인 경우가 최적이었다. 분석파장 결정을 위해 분석 파장 230nm와 254nm에서의 화약물질 14종에 대한 검출한계 (detection limit)값과 각 화약물질의 UV/VIS스펙트럼을 비교한 결과 254nm보다 230nm일때가 더 적절하였다. 하지만 NB, 2,4-DNT, 2NT, 4NT및 3NT는 분석파장이 UV254nm일때 더 적절하였다.

• 한국어병학회지
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• 제20권2호
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• pp.139-145
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• 2007

인체에 널리 사용되고 있는 Aspirin (ASA)을 양식 뱀장어 (Anguilla japonica) 약욕 또는 경구 투여한 다음 혈장 중의 ASA와 salicylic acid (SA)의 양을 HPLC로 측정하였다. 뱀장어 혈장은 0.2 M HCl과 0.2 M orthophosphoric acid로 산성화시킨 다음 acetonitrile과 혼합하여 ASA와 SA를 추출하였다. 2약제의 정량은 Novapak C18과 UV detector (237 nm)가 장착된 HPLC로 측정하였다. 이 때 이동상은 740 ㎖의 증류수, 900 ㎕의 orthophosphoric acid와 180㎖의 acetonitrile을 사용하였다. ASA, SA 및 내부 표준물질로 사용한 2-methylbenzoic acid (MBA)의 retention time은 각각 4.8분, 8.4분 및 11.4분이였으며, 측정한계 농도는 ASA가 0.05 ㎍/㎖, SA는 0.01 ㎍/㎖였다. 혈장으로 부터의 평균회수율은 ASA가 70.8-99.6%, SA는 95.2-100.3%였다. 뱀장어에 ASA를 약욕 (20 ppm) 또는 경구투여 (50 ㎎/kg BW) 한 다음 채취한 혈장을 시료로 이 방법으로 ASA와 SA의 양을 측정한 결과 단지 SA만 검출되어졌고, ASA는 검출되지 않았다. 이는 ASA가 혈장내에서 신속히 SA로 분해되기 때문으로 판명되었다. 또 ASA에 약욕시킨 경우에는 약욕 후 3시간후에 혈장내의 SA양이 최고치에 도달하였으며, 경구투여 한 경우에는 7일후에 최고치에 도달하였다. 한편 ASA를 투여한 다음 ASA 무첨가 수조에 수용한 결과 2투여 경로 모두 48시간 이후에는 SA가 0.02-0.03 ㎍/㎖이 검출되어 잔류의 문제도 거의 없었다. HPLC를 이용한 혈장내의 ASA와 SA의 검출법은 신속하며 정확한 방법으로 뱀장어 이외의 어류에도 활용 가능할 것으로 생각된다.

• 대한화장품학회지
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• 제35권1호
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• pp.11-17
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• 2009

스테로이드 함유 표시가 없는 화장품에서 항염증 효과가 있는 글루코코티코스테로이드인 베타메타손프로피오네이트 성분이 검출되었다. 이 화장품은 외용스프레이 및 샴푸로서 주성분으로 아연피리치온을 함유하는 것으로 표기되어 있었다. 화장품에서 스테로이드 구조와 활성을 갖는 물질의 존재를 확인하기 위하여 실리카겔 박층판을 이용한 박층크로마토그래프를 사용하였으며 이 성분을 분리하기 위해 high-performance liquid chromatography (HPLC)를 이용하여 확인 및 정량을 수행하였다. 분취용 HPLC를 이용하여 스테로이드를 함유한 것으로 판단되는 분획을 모은 다음 nuclear magnetic resonance (NMR) 및 mass spectrometry (MS)를 이용하여 스테로이드 성분을 확인하였다. 스테로이드 표준물질로 베타메타손 17-프로피오네이트 및 베타메타손 21-프로피오네이트를 합성하여 사용하였고 이 표준물질과 HPLC 크로마토그램을 비교하여 스테로이드 성분의 함량을 분석하였다. 이 방법으로 아연피리치온 제제와 같은 일부 시판 화장품에서 스테로이드 성분을 확인하였고 reversed-phase high-performance liquid chromatography (RP HPLC) 상의 유지시간 비교를 통하여 스테로이드 성분을 정량한 결과 시험한 총 8종의 화장품 시료 중 2개 제품에서 0.005 ${\sim}$ 0.02%의 베타메타손프로피오네이트가 검출되었다.