• 환경위생공학
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• 제7권1호
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• pp.79-86
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• 1992

Rapid determination of chlorpyrifos and fluvalinate in mixed insecticide was established by using high performance liquid chromatography. Result were as follows : 1. On Lichrosorb${\circledR}$ RP-8(10 ${\mu}m$) Column with on fluent of acetanitrile : water=75 . 25, sufficient separation of Chlorpyrifos and Fluorinate of base was obtained. 2.410td portion the diluted solution was injected in to the cdumn, and the effluent was monitored by on UV-Detector at 270 nm. 3. Relative Standard Deviation were 0.97% (chlorpyrifos) and 0.5% (fluorinate) under analysis conditions. 4. The UV-Detector response at 270 nm were linear (Y=421.8X-2090, $R^2=0.9997$ : Chlorpyrifos, Y= 1062.7X-4017.7, $R^2=0.9998$ : Fluorinate) over a range of 30~500 ${\mu}g/ml$.

• Journal of Pharmaceutical Investigation
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• 제37권3호
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• pp.187-192
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• 2007

A reversed phase HPLC analysis of atorvastatin (AS) standard solution was performed using diclofenac (DF) as internal standard. Column oven temperature, flow rate and the composition of the mobile phase were varied in order to determine a practical system setup using a C18 column and UV detector. Two C18 columns of different length were compared regarding their influence on the AS peak shape. Based on these preliminary experiments a validation study was performed utilizing a C18 column at $62^{\circ}C$ with a mobile phase consisting of sodium phosphate buffer (0.05 M, pH 4.0), methanol and acetonitrile (40:50:10, v/v/v). The detection limit for AS was $0.1{\mu}g/ml$ and inter- and intra-day calibration curves were linear over a concentration range of $0.2-50{\mu}g/ml$. Accuracy and precision were satisfactory in the AS concentration range of $0.5-50{\mu}g/ml$.

• Bulletin of the Korean Chemical Society
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• 제20권10호
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• pp.1165-1171
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• 1999

The analysis of trace herbicides using the on-line SPE-HPLC system and a photochemical reaction was studied. 18 compounds of herbicides including eight triazines, six phenoxy acids and esters, and four other herbicides were examined. The on-line SPE-HPLC system developed for selection of eluting solvent improved chromatographic efficiency. The recoveries of herbicides were higher than 77%. With 100 mL tap water samples, the detection limits for all analytes were in the 0.1-2.3×10-10 M range. Detection was done by a UV or fluorescence spectrometer after photochemical reaction at the end of the column with 2W or 450W mercury lamp. Without a photochemical reaction, all compounds responded to 230 nm UV detector, but phenoxy acids and esters were weakly detected. However, with a photochemical reaction, these compounds were selectively detected at 320 nm wavelength of UV absorption and 400 nm emission of the fluorescence detectors. This method can be used for the analysis of environmental water containing herbicides at trace levels.

• 분석과학
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• 제19권6호
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• pp.519-528
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• 2006

본 연구에서는 뇨시료를 고체상 추출법으로 추출한 후 HPLC/DAD/ESI-MS(high-performance liquid chromatograph/diode array detector/electro-spray ionitation mass spectrometry)를 사용하여 분석하였다. 7종의 thyroid hormones의 HPLC 분리조건은 Hypersil ODS(octadecylsilica) 컬럼(4.6mm I.D., 100 mm length, particle size $5{\mu}m$)을 사용하고 ammonium formate buffer와 acetonitrile을 이동상으로 하여 기울기 용리한 결과 완전 분리가 가능하였으며, UV spectra 및 질량스펙트럼을 확인할 수 있었다. 고체상 추출법에 의한 전처리 최적 조건을 조사한 결과 시료를 pH 3으로 한 후 C18 고체상을 사용하여 4 mL의 methanol/ammonium hydroxide(9:1) 혼합용액으로 용리할 경우 회수율이 89.0-113.1%로 나타났다. HPLC/DAD를 이용하여 10-1000 ng/mL범위에서 검량선을 작성한 결과 $r^2$값은 0.992-0.998 으로 나타났으며 검출한계는 2-4 ng/mL(3.8-13.0 pmol/mL)로 계산되었다.

• 약학회지
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• 제30권6호
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• pp.311-316
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• 1986

A new UV labeling reagent was developed and used in HPLC for the determination of prostaglandin $E_2$ which have weak UV light-absorbing property. This reagent, 2-bromoacetyltriphenylene, was synthesized by the bromination of 2-acetyltriphenylene which was obtained from triphenylene by Friedel-Crafts reaction. The wave length maximum (${\lambda}_{max}^{CH_3CN}$ of this reagent was 268nm. Prostaglandin E$_2$ was extracted from prostaglandin E$_2$-$\beta$-cyclodextrin using a Sep-pak $C_{18}$ cartridge. The prostaglandin E$_2$ was labeled with 2-bromoacetyl-triphenylene in aectonitrite using 18-crown-6-ether as catalyst. Derivatized prostaglandins were separated on a reversed-phase column (Radial-pak) $\mu$-Bondapak $C_{18}$ using acetonitrile: water=60:40 as mobile phase. The effluent was monitored by UV detector at 254nm filter kit. Linearity of calibration curve was obtained between 30ng and 140ng, and the lower limit of detection was 5ng.

• Applied Biological Chemistry
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• 제41권4호
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• pp.251-256
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• 1998

The analytical method of ${\beta}-ecdysone$, the insect moulting hormone, by high performance liquid chromatograph (HPLC) with UV detector was developed using boronic ester derivatization and applied to the extracts of Ajuga iva, Silene otites and Schistocerca egg. Derivatization of yield with methyl-, butyl-, and phenyl-boronate was completed under mild conditions with 20-hydroxyecdysone. The conversion ratios of boronate were estimated to be 70% in methylboronic acid, 89% in butylboronic acid and 93% in phenylboronic acid. Phenylboronate showed a high sensitivity and demonstrated an effective separation on HPLC. The optimum temperature and reaction time for derivative formation were $25^{\circ}C$ and 20 min. respectively. ${\beta}-Ecdysone$ was effectively identified in extracts of Ajuga iva, Silene otites and Schistocerca egg by the HPLC method.

• 한국식품과학회지
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• 제32권6호
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• pp.1227-1233
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• 2000

Lycopene을 dichloromethan에 용해하고 dry ice 상에서 ozonolysis을 행하였다. Ozonolysis에 의해 생성된 산화개열산물은 silica gel chromatography를 행하여 분획하고, photodiode array detector를 이용하여 ODS-HPLC와 LC-MS를 이용하여 분석하였다. Lycopene으로부터 생성된 carbonyl 화합물로 acycloretinal, apo-14'-lycopenal, apo-12'-lycopenal, apo-10'-lycopenal, apo-8'-lycopenal 그리고 apo-6'-lycopenal이 동정되었다. Lycopene을 toluene 및 Tween 40 수용액에 용해하고 $37^{\circ}C$에서 자동산화시킨 결과, 다수의 carbonyl 화합물이 생성되었다. Lycopene의 자동산화에 의해 생성된 carbonyl 화합물의 대부분은 ozonolysis에 얻어진 산화개열산물이 나타내는 HPLC상의 거동과 분광학적 특성이 서로 잘 일치하였다. 이러한 결과는 in vitro 상의 산화적 조건하에서 lycopene 자동산화에 의해 eccentric cleavage가 생성됨을 알 수 있었다.

• 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.

• 분석과학
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• 제26권1호
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• pp.19-26
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• 2013

자외선 흡광도가 거의 없는 농작물의 생장 조절용 농약으로 사용되고 있는 지베렐린(GAs) 중 하나인 지베렐린 산($GA_3$)은 발색단이 미약해서 자외선 검출기를 이용하여 분석하기가 어려운 물질이다. 액체-액체 추출법을 이용하여 과일류로부터 지베렐린 산을 효과적으로 추출하기 위하여 시료의 pH와 추출용매에 대한 최적의 추출조건을 확립하고자 하였다. 페나실 브로마이드를 유도체화 시약으로 사용함으로써 자외선 검출기에 선택적이며 감도가 좋은 $GA_3$-유도체 화합물을 만들었으며, 최적의 유도체화 조건을 확립하기 위해서 반응온도 및 시간, 유도체화 시약의 양, 염기의 양 등을 변화시켜주는 실험이 수행되었다. 유도체화 된 $GA_3$는 C18 컬럼을 사용하여 방해물질이 없이 HPLC/UV-vis로 효과적으로 분석되었으며, HPLC/ESI-MS를 사용하여 유도체화된 화합물의 구조를 확인하였다. 사과의 경우, 검출한계(LOD)와 정량한계(LOQ)는 각각 0.008 mg/kg, 0.027 mg/kg로, 배의 경우, 검출한계(LOD)와 정량한계(LOQ)는 각각 0.003 mg/kg, 0.012 mg/kg로 낮은 검출한계와 정량한계를 보였다. 확립된 유도체화 방법은 과일류 중에 존재하는 $GA_3$의 효과적이고 편리한 분석에 응용될 수 있을 것이다.

• Biomolecules & Therapeutics
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• 제15권2호
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• pp.123-126
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• 2007

A sensitive, simple and highly selective liquid chromatography method of determination for extraction of pseudoephedrine hydrochloride from Allegra D tablet was developed. The chief benefit of the present method is the minimal sample preparation, as the procedure is only filtering through pore syringe filter. Two drugs (pseudoephedrine hydrochloride, fexofenadine) were separated on a C$_{18}$ column and analyzed by high performance liquid chromatography (HPLC). The method had a chromatographic run time of 8.0 min. 1 ml of pseudoephedrine hydrochloride solution (1 mg/ml) was filtered through 0.22 um pore syringe filter. 50 ul of filtering solution was injected to HPLC pump and we knew the retention time (1.85 min) of separating of pseudoephedrine hydrochloride using UV detector at 280 nm. We used C$_{18}$ column (4.6 mm${\times}$250 mm), mobile phase solution (<0.05 mol/L NaH$_2$PO$_4$, 2 ml/L H$_3$PO$_4$>/CH$_3$CN / sodium dodesyl sulfate = 60 ml / 40 ml / 1 g). We separated psedoephedrine hydrochloride at run time of 1.85 min from Allegra D tablet solution (1 mg/ml) filtered through 0.22 um pore syringe filter using UV detector at 280 nm. Flow rate was set at 1.0 ml/min and the column temperature was set at 40$^{\circ}C$. Psedoephedrine hydrochloride solution (1 mg/ml) separated from Allegra D tablet was filtered through 0.22 um pore syringe filter and injected 50 ul. We confirmed the peak of psedoephedrine hydrochloride at same retention time and the separating solution was freeze-dried. In conclusion, A simple isocratic reverse-phase HPLC method has been developed that provides excellent separation of pseudoephedrine from Allegra D tablet.