• 한국수산과학회지
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• 제43권4호
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• pp.293-297
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• 2010

To prevent amnesic shellfish poisoning (ASP) resulting from the consumption of shellfish contaminated with domoic acid, the quantitative analysis of domoic acid is very important. We validated a high performance liquid chromatography (HPLC) method for accurate and precise quantification of domoic acid. A clear peak and the isolation of domoic acid resulted on injecting a 50% methanol extract of CRM-ASP-Mus-c mussel reference material using HPLC. The limit of detection of domoic acid under the established HPLC conditions was $0.10\;{\mu}g/g$, and the limit of quantification of the toxin under the same conditions was $0.25\;{\mu}g/g$. The intra-accuracy and precision for domoic acid in CRM-ASP-Mus-c were 90.7-95.7% and 0.28-22.25%, respectively. The inter-accuracy and precision for domoic acid were 89.1-97.1% and 1.7-4.1%, respectively. The mean recovery of domoic acid in methanol extracts from ten species of marine invertebrates was 88.6-1105.1%.

• 생약학회지
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• 제43권4호
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• pp.286-290
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• 2012

Many diterpenoids from Siegesbeckia species (Compositae) and their anti-inflammatory actions have been examined. In this research, high-performance liquid chromatography-ultraviolet spectrophotometer (HPLC-UV) method was used to compare the quantitative level of kirenol (ent-pimarane-type diterpenoid) in the aerial parts of Korean S. glabrescens and S. pubescens and the Chinese Siegesbeckiae Herba. Fingerprints of the two HPLC chromatograms of Korean S. glabrescens and S. pubescens were similar, but considerably different from Chinese Siegesbeckiae Herba. The content of kirenol in S. pubescens ($16.51{\pm}0.10$ mg/ml dry weight as mean${\pm}$RSD) was higher than S. glabrescens ($13.48{\pm}0.12$ mg/g dry weight). These values were considerably higher than the Chinese Siegesbeckiae Herba ($1.55{\pm}0.74$ mg/g dry weight). Thin layer chromatography (TLC) analysis demonstrated the containing of kirenol in the three plant materials, but the presence of siegeskaurolic acid (entkaurane-type diterpenoid) only in the Chinese Siegesbeckiae Herba.

• 한국환경농학회지
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• 제23권4호
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• pp.251-257
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• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.

• Journal of Microbiology and Biotechnology
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• 제16권4호
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• pp.643-646
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• 2006

Because of potential health hazards of aflatoxins for humans, the present study was conducted to monitor aflatoxin $B_1\;(AFB_1)$ in livestock feeds. A total of 249 samples of feeds collected in Korea were analyzed by DC-ELISA for qualitative analysis of $AFB_1$. Then, 27 samples that were verified to contain $AFB_1$ by DC-ELISA were quantitated by HPLC/FLD. HPLC/FLD analysis revealed that only one sample collected from a farm contained 11 ppb of $AFB_1$, whereas the other samples collected from feed companies did not contain $AFB_1$. The presence of $AFB_1$ was further confirmed by LC/MS analysis. TLC analysis indicated that the result of the DC-ELISA was most likely due to possible contamination of other mycotoxins rather than $AFB_1$. In conclusion, HPLC/FLD analysis following DC-ELISA is necessary for rapid and accurate detection of $AFB_1$.

• 한국산학기술학회논문지
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• 제15권1호
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• pp.396-401
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• 2014

본 논문에서는 록소프로펜 제제의 분석 시간을 단축하고 제품 출하 속도를 향상시키기 위하여 근적외부(NIR) 스펙트럼 측정법을 이용하여 기존에 사용하던 HPLC 방법과 상호 비교해 보고자 하였다. 제제학적으로 사용되는 다른 첨가제들과 함께 록소프로펜 혼합시료를 제조하고, NIR 분광광도계와 HPLC로 록소프로펜을 정량하고 평가하였다. 두 시험법의 밸리데이션 항목으로 특이성, 정확성 및 정밀성을 실시하였다. NIR 측정법이 검증되었고, 제약산업 분야의 제조공정 중 품질관리를 위한 적합한 결과를 얻었다. 결론적으로 록소프로펜을 분석하는데 있어서 NIR 측정법을 사용하면 기존의 HPLC 정량법을 NIR의 결과로 대치할 수 있을 것이다.

• 분석과학
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• 제23권1호
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• pp.97-101
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• 2010

(R)-N-3,5-dinitrobenzoyl (DNB) phenylglycinol로 부터 만들어진 키랄 선택제가 라세미 Nacylnaphthylalkylamines의 분리에 HPLC 키랄 정지상으로 이용된 바 있다. 본 연구에서는 (R)-phenylglycinol 유도체 키랄 선택제를 이용하여 키랄 크로마토그래피와 NMR 분광법에 의한 광학순도를 측정하였다. NMR과 HPLC 실험결과를 참값과 비교하여 각 광학순도 측정값의 정확도와 정밀도를 계산하였다. NMR 방법의 오차는 +2.2%, 평균 RSD는 4.54% 이었고, HPLC 방법의 오차는 -3.5%, 평균 상대표준편차는 3.23% 이었다.

• 대한화학회지
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• 제45권6호
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• pp.524-531
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• 2001

Microcystin-LR, -YR 및 -RR과 같은 독성 microcystin의 분석에 있어서 정확성을 높이기 우해 고상 추출을 통한 micro-HPLC/IS/MS를 사용하였다. 이러한 microcystin-LR, -YR, -RR를 확인하는데 HPLC/UV로는 238nm에서의 흡광도를 측정하였고, 질량스펙트럼에서는 1 35m/z 및 $[M+H]^+$m/z의 특성 피이크만을 검출하여 왔다. 본 연구에서는 이중 전하에 해당하는 새로운 선들이 LR에서는 507m/z, PR에서는m/z, YR에서는 532m/z에서 추가로 검출되었다. 이 방법을 사용하여 대청호에서 독성 microcystin의 존재성을 조사하였다.

• 생명과학회지
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• 제34권1호
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• pp.59-67
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• 2024

산딸기, 치자, 유백피의 혼합물인 복합 천연물 LS-RUG-com이 위염, 위궤양, 식도성 역류염 및 Helicobacter를 억제함을 확인한 바, LS-RUG-com을 건강기능식품 개별인정형 소재로 개발하고자 하였다. 본 연구에서는 소재 개발을 위한 LS-RUG-com 분석방법을 확립하고자 하였으며, 산딸기, 치자 및 유백피의 지표물질을 HPLC/UV system을 이용하여 분석방법을 최적화하였다. 본 연구에서는 분석법 validation을 입증하기 위하여 특이성(specificity), 정확성(accuracy), 정밀성(precision), 검출한계 및 정량한계(detection & quantitation limit) 및 직선성(linearity)을 평가하였으며, 그 결과 본 연구의 HPLC/UV 동시 분석법이 산딸기, 치자 분석에 적합하며, 신뢰성이 있음을 증명하였다. 또한 유백피의 HPLC/UV 단독 분석법이 적합하며 신뢰성이 있음을 증명하였다.

• 공업화학
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• 제9권3호
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• pp.404-406
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• 1998

가스 크로마토그래피(GC)와 가스 크로마토그래피(HPLC)를 이용하여 imidazoline계 양이온 계면활성제 분석을 수행하였다. 염기 가수분해와 산 가수분해 후 GC로 imidazoline ring의 original fatty acid의 alkyl chain 분포를 조사하였다. 역상 C18 분리관을 사용하고 0.1M $NaClO_4$가 함유된 methanol과 acetonitrile의 50:50(v/v)액을 용리액으로 할 때 imidazoline의 homologous한 total alkyl chain 분포가 HPLC에서 훌륭하게 분리되었으며, GC 결과와 좋은 일치를 보여주었다. 본 연구의 분석법으로, imidazoline계 양이온 계면활성제의 소수성 alkyl chain 분석 및 평균 분자량 결정이 가능하였으며, 전처리 필요없이 HPLC법을 이용한 imidazoline 의 검출한계는 10ng이었다.

• 대한본초학회지
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• 제22권2호
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• pp.97-102
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• 2007

Objectives : This study presents a high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-MS/MS) methods for the quantitative and qualitative analysis of various active components in Samul-tang, which is composed of four crude herbs. Methods : HPLC-ESI-MS/MS for the determinations of paeoniflorin and 5-HMF (5-hydroxymethyl 2-furaldehyde) in the Samul-tang, the separation method was performed on an COSMOS1L 5C18-AR-Il (2.0 X 150 mm I.D.) column by gradient elution with 0.1% acetic acid and 5% CH3CN in water (A)-0.1% acetic acid and 5% H20 in CH3CN (B) as the mobile phase at a flow-rate of 300 ${\mu}L/min$ with detection at quadrupole mass spectrometer. The all marker substances were always detected as the base peaks in the positive ion mode. Results : The paeoniflorin of Paeoniae Radix in Samul-tang showed a strong base peak [M+H2O]+ in the positive detection mode to give the following as; paeoniflorin (498.109 [M+H2O]+, 479.8 [M]+, 301 [M-glucose]+, 179.3 [glucose]+). Based on the HPLC retnetion time and MS of standard compounds confirmed the identity of active compounds in Rehmanniae Radix Preparata as follows; 5-HMF (127.0[M+H]+, 109.3 [M-OH]+) in the positive ion mode. Conclusion : According to the above results, HPLC-ESI-MS method permits assignment of tentative structures such as paeoniflorin and 5-HMF in the Samul-tang.