• 생약학회지
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• 제41권4호
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• pp.323-327
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• 2010

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of dictamine, obacunone and fraxinellone was established for the quality control of traditional herb Dictamnus dasycarpus cortex. Separation and quantification were successfully achieved with a Shiseido C18 column ($5\;{\mu}m$, 4.6 mm I.D. ${\times}$ 250 mm) by gradient elution of a mixture of methanol and water at a flow rate of 1.0 ml/min. The diode-array UV/Vis detector (DAD) was used for the detection and the wavelength for quantification was set at 236 nm. The presence of dictamine, obacunone and fraxinellone in this extract was ascertained by retention time, spiking with each authentic standard and UV spectrum. All three compounds showed good linearity ($r^2$ > 0.999) in relatively wide concentration ranges. The R.S.D. recovery of each compound was 101.0~103.7% with R.S.D. values less than 1.0%. This method was successfully applied to the determination of contents of dictamine, obacunone and fraxitnellone in three commercial products of D. dasycarpus cortex. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial products.

• Bulletin of the Korean Chemical Society
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• 제34권11호
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• pp.3444-3450
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• 2013

Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

• 한국환경보건학회지
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• 제22권1호
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• pp.36-44
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• 1996

A comparison was made of two detection methods(UV absorbence detection and fluorescence detection with pre-column derivatization, with trifluoroacetic acid) coupled with HPLC for the simultaneous determination of aflatoxin $B_1, B_2, G_1$ and $G_2$. A good separation of the four aflatoxins was achieved on a reversed-phase $C_{18}$ column (30 cm x 3.9 mm) with methanol-acetonitrile-water(20+20+60) for absorbence detection or acetonitrile-water(25+75) for fluorescence detection at the flow rate of 1.0 ml/min. The calibration graphs were linear over the ranges 100 ppb-1 ppm for $B_1/G_1$ and 30~300 ppb for $B_2/G_1$ with absorbence detection, and 1~500 ppb for $B_1/G_1$ and 0.3~150 ppb for $B_2/G_2$ with fluorescence detection. The correlation coefficients were greater than 0.94 and 0.99 for absorbance detection and for fluorescence detection, respectively. The detection limit was 100 ng for $B_1/G_1$ and 30 ng for $B_2/G_2$ with absorbence detection, and 1 ng for $B_1/G_1$ and 0.3 ng for $B_2/G_2$ with fluorescence detection. Recovery rates of aflatoxin $B_1, B_2, G_1$ and $G_2$ added to yeast-extract sucrose broth medium were 66.6%, 59.4%, 67.5% and 59.2%, respectively, for absorbence detection and 82.9%, 71.5%, 80.0% and 69.3%, respectively, for fluorescence detection. The four aflatoxins in culture medium were quantitatively detected by the two methods. The aflatoxins in the rice sample were not detected the absorbence detection method, but were below 10 ppb using the fluorescence detection method. Analysis of aflatoxins by both the absorbence and fluorescence methods coupled with HPLC showed acceptable linearity and good recovery. The absorbence detection was less timeconsuming and safer for treatment. The fluorescence detection was more elective and sensitive though elevated $B_1$ and $G_1$ contents were determined from the TFA-induced conversion of $B_1$ to $B_{2a}$ and $G_1$ to $G_{2a}$.

• 농약과학회지
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• 제2권3호
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• pp.79-84
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• 1998

콩나물중 carbendazim 잔류분을 정량하고 확인할 수 있는 새로운 분석법을 확립하고자 tandem HPLC(UV & FL) 및 APcI를 source로 사용한 LC/MS를 이용하였다. 이를 위해 FL(fluorescence) 검출기를 UV(ultraviolet) 검출기와 나란히 연결하여 UV 검출기의 경우 280 nm 파장을 그리고 FL 검출기의 경우는 excitation파장과 emission파장을 각각 280 mn와 310 nm로 설정하였다. 분석결과 carbendazim의 검출한계는 $0.04{\mu}g/kg$이었다. 콩나물에 carbendazim을 0.5, 1.0 및 2.0 ppm 수준으로 첨가하여 회수율을 측정한 결과 그 평균값은 89.1%이었다. APcI source를 사용한 LC/MS 질량스펙트럼 방법은 콩나물중 carbendazim 잔류분을 최종 확인할 수 있었다. APcI LC/MS 방법은 전자충격에 의한 질량스펙트럼에 비해 훨씬 간단한 fragment를 형성할 뿐 만 아니라 carbendazim의 경우 m/z 133, m/z 159, m/z 191($M^{+}$)의 전형적인 fragment 이온을 형성하므로, 이 방법을 병행한다면 콩나물중 carbendazim 잔류분을 효과적으로 확인할 수 있을 것으로 사료되었다.

• 약학회지
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• 제28권6호
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• pp.321-325
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• 1984

A HPLC determination method of xanthinol nicotinate(I) was developed for study of its stability and characteristics in solutions. I was determined using an ${\mu}-Bondapak\;C_{18}$ column with a mobile phase of methanol: $H_2O$ (1 : 1) and UV absorbance detection at 254nm. The results revealed that the method was enough to use as stability indicating determination with the mean of 99.9% and standard deviation of ${\pm}1.42%$ when analyzed 10 times for standard solution.

• Natural Product Sciences
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• 제27권4호
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• pp.280-283
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• 2021

Cercidiphyllum japonicum is being used for the treatment of obesity and liver fibrosis in Korean local clinics. In the present study, we tried to develop an analytical methodology for the determination of the chemical markers of Cercidiphyllum japonicum. Four chemicals, maltol (1), chlorogenic acid (2), quercetin (3), and avicularin (4), were selected for method validation, and the analytical conditions were optimized and validated using high-performance liquid chromatography coupled with an ultraviolet detector (HPLC-UV). Additionally, the seasonal variations of four markers were monitored every month for six months. The contents of four chemicals markers were most detected in a sample collected in June.

• 한국식품영양과학회지
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• 제45권11호
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• pp.1610-1616
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• 2016

섬쑥부쟁이로부터 고요산혈증 개선에 도움을 주는 기능성 식품 개발을 위하여 최적의 에탄올 추출물 탐색과 high performance liquid chromatography-ultraviolet(HPLC-UV) 분석방법에 의한 validation을 실시하였다. 지표성분으로 3,5-dicaffeoylquinic acid(3,5-DCQA)를 선정하여 표준화를 실시하였으며 검출법 확립을 위한 3,5-DCQA 정량분석은 Luna RP-18 칼럼($4.6{\times}250mm$, $5{\mu}m$)을 이용하여 1% 초산용액과 메탄올을 전개용매로 사용하였다. 용출은 1.0 mL/min의 유속으로 기울기 용출(gradient elution) 방법을 이용하였으며, 320 nm 파장에서 검출한 피크 면적을 이용하여 검량곡선을 작성하여 분석하였다. 본 연구에서 확립한 분석법으로 특이성, 직선성, 정밀성, 정확성, 회수율을 검색하였다. 3,5-DCQA의 검량선으로부터 상관계수($R^2$) 0.9999의 우수한 직선성과 intra-day와 inter-day 분석에서 90% 이상의 회수율과 5% 미만의 RSD를 나타내 정밀성과 정확성을 입증하였다. 검출한계는 $2.68{\mu}g/mL$였고 정량한계는 $8.11{\mu}g/mL$로 나타났다. 섬쑥부쟁이 에탄올 추출물(AGE)은 70과 $80^{\circ}C$에서 30, 50, 70, 80% 에탄올로 3, 4, 5, 6시간 동안 각각 추출하였으며, 지표물질의 검량곡선을 활용하여 각각의 AGE로부터 3,5-DCQA의 함량을 분석하였다. 본 시험법으로 분석한 3,5-DCQA의 함량은 $70^{\circ}C$에서 추출한 70% AGE가 $52.59{\pm}3.45mg/Aster$ glehni 100g의 함량을 나타내 가장 우수하게 나타났다. 그러나 섬쑥부쟁이 추출물에 함유된 5-caffeoylquinic acid(5-CQA)의 함량 비교분석은 에탄올 함량이나 추출 시간에 따른 함량 변화가 미미하게 나타났다. 또한, 다양한 AGE에 대하여 XOD 저해 효능을 검색하였을 때, 3,5-DCQA의 함량이 가장 높은 $70^{\circ}C$에서 추출한 70% AGE에서 우수한 효능을 나타내 기능성 원료 표준화를 위한 적합한 분석법임이 검증되었다. 따라서 본 연구를 통하여 확립된 3,5-DCQA의 분석법은 섬쑥부쟁이 에탄올 추출물로부터 개별인정형 건강기능식품 기능성 원료 개발을 위한 유용한 자료로 활용될 것으로 생각한다.

• 한국식품위생안전성학회지
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• 제3권4호
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• pp.203-209
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• 1988

식품중 보존료의 분석방법을 신속 간단하면서도 정화기 정량할 수 있는 방법 개발을 시도한 바 다음과 같은 결론을 얻었다. 1. HPLC system에 의한 희석법으로는 간장중 paraben류와 , 유산균음료중 SOA를 99%이상의 회수율로 20분 이내에 정량할 수 있었다. 2. GLC system에 의한 직접 추출법으로 간장중 BA와 Paraben류의 동시정량이 가능하였으며 유산균음료와 SOA를 99%이상의 회수율로 신속히 정량 할 수 있다.

• Archives of Pharmacal Research
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• 제16권2호
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• pp.99-103
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• 1993

We describe here the conditions of thin layer chromatography (TLC) and high pressures liquid chromatography (HPLC) to improve the analytical method of phosphotyrosine (p-Tyr) in biological sample. TLC was performed on silica plate with the mixture of propanol and water (2.1 : 1 v/v) as a mobile phase and $R_1$ values were 0.42, 0.39 and 0.33 for phosphotyrosine, phosphothreonine and phosphoserine, respectively. HPLC was performed on $NH_2$ column with a mobile phase of potassium biphosphate solution by UV deterction at 192 nm. The optimum condition of HPLC was obtained at 0.01 M, pH 4.5 with a clear separation within 12 min. These procedures have been applied to the analysis of phosphotyrosine obtained from tyrosine-phosphorylated enolase. Both TLC and HPLC methods were suitable to analyze tyrosine-phosphorylated protein without being affected by contaminants from hydrolysates.

• 한국식품위생안전성학회지
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• 제2권3호
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• pp.89-95
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• 1987

시판 갈근으로부터 Isoflavanoid 성분인 Daidzein과 Daidzin을 분리 정제하고 이를 표준물질로 하여 시판 칡차 8종에 대한 칡성분 분석을 HPLC 방법으로 시도하여 다음과 같은 결론은 얻었다. 1. 칡차의 성분 분석법은 종래의 TLC법에 비하여 HPLC를 이용, 신속하고 정확하게 분석할 수 있었다. 2. 추출방법에 따라 성분함량이 크게 영향을 받아 Daidzein을 분석할 경우는 냉침법이, Daidzin의 분석시는 가열 추출법이 양호하였다. 3. 한국산 갈근중 Daidzein과 Daidzin은 0.08% 및 0.66% 함유되었다. 4. 시판 칡차중 고형차류는 칡의 성분이 표기량에 비하여 매우 적게 함유되거나 전혀 함유되지 않은 예도 있으며 액상차의 경우는 엑기스 고형분이 4∼5%가 함유되었다.