• 약학회지
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• 제52권6호
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• pp.446-451
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• 2008

A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of chlorogenic acid (1), sweroside (2), luteolin-7-O-glucoside (3), (E)-aldosecologanin (4) and 3,5-dicaffeoylquinic acid (5) from Lonicera joponica flower buds. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, 4.6${\times}$150 mm) with the column temperature $25^{\circ}C$. The mobile phase was composed of (A) water with 0.1% formic acid and (B) acetonitrile with 0.1% formic acid using a gradient elution, the flow rate was 0.3 ml/min. Detection wavelength was set at 250 nm. All calibration curves showed good linear regression ($r^2$>0.994) within test ranges. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.05${\sim}$1.95% and 0.15${\sim}$2.26%, respectively, and the overall recoveries of 97.71${\sim}$103.65% for the five compounds analyzed. The verified method was successfully applied to quantitative determination of the three types (phenolic compounds, iridoids and flavonoids) of bioactive compounds in 21 commercial L. japonica flower buds samples from different markets in Korea and China. The analytical results demonstrated that the contents of the five analytes vary significantly with sources.

• 대한화학회지
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• 제55권4호
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• pp.626-632
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• 2011

폭심(phoxim)은 널리 사용되고 있는 구충제인 동물용의약품이다. 본 논문에서는 소와 돼지 근육에 잔류하는 폭심을 분석하기 위해서, 실리카 고체상과 아세토니트릴을 사용하여 추출/정제하였다. 분석을 위해서 LC/ESI-MS/MS 방법이 사용되었다. HPLC에서 $C_{18}$ 컬럼($2.1{\times}100\;mm$, $3.5\;{\mu}m$)이 사용되었으며, 이동상으로는 0.1% formic acid와 물이 사용되었다. 소(0.0048~2.0 mg/kg)와 돼지(0.0055~2.0 mg/kg)에 소량첨가하여 얻은 검정곡선은 좋은 직선성($r^2$=0.995)을 나타내었다. 소와 돼지의 매트릭스에 대해서 0.0048~0.2 mg/kg범위에서 68.2~106.9%의 정확도를 나타내었으며, LOD는 0.0014~0.0017 mg/kg, LOQ는 0.0048~0.0055 mg/kg범위에 있었으며, 11.2%의 상대표준편차를 나타내었다.

• 한국식품과학회지
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• 제47권2호
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• pp.170-175
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• 2015

본 연구에서는 국산배의 기능학적 우수성 증명을 위해 국산배로부터 생리활성 화합물을 밝히고자 하였다. 이에 배 과피 MeOH 추출물을 용매분획하여 얻은 EtOAc-산성획분을 대상으로 Sephadex LH-20 column chromatography와 ODS-HPLC를 이용하여 순차적으로 정제를 행하여 2종의 화합물을 단리하였다. 단리된 화합물 1과 2는 MS 및 NMR 분석을 통하여 각각 quercetin 3-O-${\beta}$-Dglucopyranoside(화합물 1)와 3,5,6,7,8,3',4'-heptahydroxyflavan [(-)-dulcisflavan, 화합물 2)]으로 동정되었다. 단리된 화합물 1은 동양배로부터, 그리고 화합물 2는 배로부터 처음 동정된 화합물이다. 본 연구결과가 국산배의 기능학적 우수성 증명을 위한 기초자료로 활용되길 기대한다.

• Journal of Pharmaceutical Investigation
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• 제34권6호
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• pp.513-519
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• 2004

A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

• Journal of Microbiology and Biotechnology
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• 제27권9호
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• pp.1639-1648
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• 2017

Curcumin is a natural polyphenolic compound, widely acclaimed for its antioxidant, anti-inflammatory, antibacterial, and anticancerous properties. However, its use has been limited due to its low-aqueous solubility and poor bioavailability, rapid clearance, and low cellular uptake. In order to assess the effect of glycosylation on the pharmacological properties of curcumin, one-pot multienzyme (OPME) chemoenzymatic glycosylation reactions with UDP-${\alpha}-{\text\tiny{D}}$-glucose or UDP-${\alpha}-{\text\tiny{D}}$-2-deoxyglucose as donor substrate were employed. The result indicated significant conversion of curcumin to its glycosylated derivatives: curcumin 4'-O-${\beta}$-glucoside, curcumin 4',4"-di-O-${\beta}$-glucoside, curcumin 4'-O-${\beta}$-2-deoxyglucoside, and curcumin 4',4"-di-O-${\beta}$-2-deoxyglucoside. The products were characterized by ultra-fast performance liquid chromatography, high-resolution quadruple-time-of-flight electrospray ionization-mass spectrometry, and NMR analyses. All the products showed improved water solubility and comparable antibacterial activities. Additionally, the curcumin 4'-O-${\beta}$-glucoside and curcumin 4'-O-${\beta}$-2-deoxyglucoside showed enhanced anticancer activities compared with the parent aglycone and diglycoside derivatives. This result indicates that glycosylation can be an effective approach for enhancing the pharmaceutical properties of different natural products, such as curcumin.

• 대한환경공학회지
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• 제35권2호
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• pp.75-83
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• 2013

본 연구는 기존의 고상추출(SPE) 과정을 분석장비인 LC/MSD에 on-line으로 연결함으로써 cartridge의 건조를 막아 target 물질의 손실을 최대한 억제하였으며 11종의 PFCs에 대해 실제 matrix가 있는 낙동강 원수를 이용한 실험에서 $80.4{\pm}5.2%{\sim}109.5{\pm}1.4%$ 범위의 높은 회수율을 구할 수 있었다. 낙동강에서의 PFCs 분포를 조사한 결과 하수처리장 방류수의 영향을 받는 지역(진천천과 금호강 하류)은 고농도의 PFCs가 검출되었으며, 낙동강 하류의 매리원수에서는 검출농도가 급격히 감소하여 PFOA만 8.0 ng/L의 농도로 검출되었다. 외국의 PFCs 검출현황을 보고한 연구결과들과 비교해 볼 때 낙동강 지류에서는 비교적 높은 농도로 PFCs가 검출되어 안심할 수 있는 수준은 아니었으며, 낙동강 본류의 경우도 여러 지역의 상수원으로 이용되기 때문에 주기적인 모니터링이 필요한 것으로 나타났다.

• 분석과학
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• 제29권4호
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• pp.155-161
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• 2016

Distribution of various illegal or counterfeit drugs of seven approved erectile dysfunction drugs and their analogues has been increased, causing health problems such as cardiovascular disorder, tachycardia, headache, or vision disturbance. We used liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) to determine the erectile dysfunction drugs and their analogues in various counterfeit drugs. Eleven erectile dysfunction drugs and their analogues were detected, with sildenafil and its analogues being the most counterfeited compounds (73.8 %), followed by tadalafil and its analogues (25.4 %). The limits of detection (LOD) and the limits of quantitation (LOQ) of liquid-type and solid-type negative samples ranged from 0.1 to 3.3 ng/mL or ng/g and from 0.3 to 10.0 ng/mL or ng/g, respectively. The recoveries ranged from 84.3 to 112.3 % and 83.2 to 110.2 %, respectively. The contents of sildenafil and tadalafil in the various counterfeit drugs ranged from 21.0 to 947.5 mg/g and from 0.2 to 170.2 mg/g, respectively.

• Natural Product Sciences
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• 제16권2호
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• pp.116-122
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• 2010

A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of five representative metabolites of the iridoid and phenolic classes from Rehmannia glutinosa. The optimal chromatographic conditions were obtained on an ODS column (5 mm, $4.6{\times}250\;mm$) with the column temperature at $25^{\circ}C$. The mobile phase was composed of water and acetonitrile using a gradient elution with the flow rate 0.3 mL/min. Detection wavelength was set at 205 nm. All calibration curves showed good linear regression ($r^2$ > 0.997) within test ranges. Limits of detection (LOD) and quantitation (LOQ) values were lower than 0.123 and $0.373\;{\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.09 - 0.76% and 0.16 - 1.41%, respectively, and the overall recoveries of 99.03 - 102.67% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytic method. The verified method was successfully applied to the quantitative determination of five representative metabolites in twenty-one commercial Rehmannia glutinosa samples from different markets in Korea and China. The analytical results showed that the contents of the five analytes vary significantly with sources.

• Toxicological Research
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• 제26권2호
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• pp.101-108
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• 2010

Halogenated organic compounds, such as 1-bromobutane (1-BB), have been used as cleaning agents, agents for chemical syntheses or extraction solvents in workplace. In the present study, immunotoxic effects of 1-BB and its conjugation with glutathione (GSH) were investigated in female BALB/c mice. Animals were treated orally with 1-BB at 375, 750 and 1500 mg/kg in corn oil once for dose response or treated orally with 1-BB at 1500 mg/kg for 6, 12, 24 and 48 hr for time course. S-Butyl GSH was identified in spleen by liquid chromatography-electrospray ionization tandem mass spectrometry. Splenic GSH levels were significantly reduced by single treatment with 1-BB. S-Butyl GSH conjugates were detected in spleen from 6 hr after treatment. Oral 1-BB significantly suppressed the antibody response to a T-dependent antigen and the production of splenic intracellular interlukin-2 in response to Con A. Our present results suggest that 1-BB could cause immunotoxicity as well as reduction of splenic GSH content, due to the formation of GSH conjugates in mice. The present results would be useful to understand molecular toxic mechanism of low molecular weight haloalkanes and to develop biological markers for exposure to haloalkanes.

• 한국식품과학회지
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• 제38권1호
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• pp.140-142
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• 2006

이전의 연구 결과에 나타난 바 있는 막걸리 중 ochratoxin A의 낮은 회수율(<50%)은 시료 내 본 곰팡이독소의 추출 혹은 전처리 과정의 개선이 필요함을 지적하였다. 본 연구에서 막걸리 시료의 균질화에 이용되던 추출 용액을 PBS 용액 대신 3% sodium bicarbonate 용액으로 채택할 경우, 80% 이상의 첨가된 ochratoxin A가 회수되어 그 검출이 용이해졌다. 한편 개선된 해당 분석법의 막걸리 시료에 대한 적용 가능성을 알아보기 위하여 국내 시판 중인 살균막걸리 30점을 대상으로 분석한 결과 밀 막걸리 2점에서 ochratoxin A가 검출되었고(0.8, 2.1 ppb), 그 결과를 다시 HPLC-ESI-MS로 확정하였다. 본 연구를 통해 수행된 개선된 시료 전처리 방법(3% sodium bicarbonate)과 병행된 IAC 및 HPLC-FD 분석법은 막걸리를 대상으로 한 ochratoxin A의 오염 조사에 유효한 분석법임이 확인되었다.