• 생약학회지
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• 제47권1호
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• pp.92-101
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• 2016

In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous determination of the 25 marker components, including chlorogenic acid, gallic acid, oxypaeoniflorin, homogentisic acid, methyl gallate, caffeic acid, 3,4-dihydroxybenzaldehyde, paeoniflorin, albiflorin, liquiritin, nodakenin, ferulic acid, ginsenoside Rg1, liquiritigenin, coumarin, cinnamic acid, benzoylpaeoniflorin, ginsenoside Rb1, cinnamaldehyde, paeonol, glycyrrhizin, 6-gingerol, evodiamine, rutecarpine, and spicatoside A in traditional Korean formula, Onkyung-tang. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was carried out using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization (ESI) source in the positive and negative modes. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. The correlation coefficient of all analytes in the test ranges was greater than 0.98. The limits of detection and quantification values of the 25 marker compounds were in the ranges 0.03-19.43 and 0.09-58.29 ng/mL, respectively. As a result, methyl gallate, 3,4-dihydroxybenzaldehyde, evodiamine, and rutecarpine were not detected in this sample and the concentrations of the 21 compounds except for the above 4 compounds were $33.09-3,496.32{\mu}g/g$ in Onkyung-tang decoction. Among these compounds, paeonol was detected at the highest amount as a $3,496.32{\mu}g/g$.

• 생약학회지
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• 제47권1호
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• pp.79-83
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• 2016

This study developed an HPLC analysis method for the determination of isoegomaketone (IK) and perillaketone (PK) in Perilla frutescens (L.) Britton leaves. P. frutescens ethanol extract was optimized through an HPLC analysis using a C18 column ($250{\times}4.6mml$, D, $S-5{\mu}m$, 12 nm) with gradient elution of water and acetonitrile as the mobile phase at a flow rate of 1 mL/min and a UV detection wavelength of 254 nm. The results of this method showed linearity in the calibration curve at a coefficient of correlation ($R^2$) of IK 0.9995, PK 0.9998. The limits of detection (LOD) for IK and PK were $0.234{\mu}g/mL$ and $0.952{\mu}g/mL$. The limits of quantification (LOQ) for IK and PK were $0.017{\mu}g/mL$ and $0.043{\mu}g/mL$. The inter-day precision RSDs of IK and PK in the P. frutescens were 1.25 to 2.69% and 0.36 to 1.10%, respectively, and the intra-day precision RSDs of IK and PK were 0.96 to 2.51% and 0.90 to 1.93%, respectively. The accuracies of IK and PK were 96.31 to 97.92% and 101.26 to 105.14%. In conclusion, this method was applied successfully to the detection of IK and PK in P. frutescens.

• 생약학회지
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• 제47권1호
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• pp.62-72
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• 2016

Banhasasim-tang is a well-known traditional Korean herbal formula and has been used clinically for the treatment of gastric disease, including acute and chronic gastritis, diarrhea and gastric ulcers in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was developed for the quantitative determination of the 13 marker constituents, homogentisic acid (1), 3,4-dihydroxybenzaldehyde (2), spinosin (3), liquiritin (4), baicalin (5), ginsenoside Rg1 (6), liquiritigenin (7), wogonoside (8), ginsenoside Rb1 (9), baicalein (10), glycyrrhizin (11), wogonin (12), and 6-gingerol (13) in Banhasasim-tang decoction. Separation of the compounds 1-13 was using an UPLC BEH $C_{18}$ ($100{\times}2.1mm$, $1.7{\mu}m$) column and column oven temperature was maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) formic acid in water (A) and acetonitrile (B) by gradient elution. The injection volume and flow rate were $2.0{\mu}L$ and 0.3 mL/min, respectively. Calibration curves of the compounds 1-13 were showed with $r^2$ values ${\geq}0.9908$. The limit of detection and limit of quantification values of the compounds 1-13 were 0.04-1.11 ng/mL and 0.13-3.33 ng/mL, respectively. Among the these compounds, the compounds 1-3 were not detected, while the compounds 4-13 were detected in the ranges of $3.20-107,062.98{\mu}g/g$ in Banhasasim-tang sample.

• Natural Product Sciences
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• 제26권1호
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• pp.64-70
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• 2020

Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

• 한국동물위생학회지
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• 제36권4호
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• pp.303-309
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• 2013

This study was conducted to determine the content of 7 mycotoxins (aflatoxin $B_1$, $B_2$, $G_1$, $G_2$, $M_1$, ochratoxin A and zearalenone) using LC-MS/MS in pork available on the Korean markets. The analysis was carried out using following conditions; C18 column ($2.1{\times}100mm$, $1.7{\mu}m$), mobile phase composed of $H_2O$ (0.1 mM $NH_4Ac$ 0.01% HCOOH) : Methanol (0.1 mM $NH_4Ac$ 0.01% HCOOH), binary pump at a flow rate of 0.5 mL/min and $2{\mu}L$ of injection volume, MS/MS detector with ESI positive and negative mode. The quantication of mycotoxins was based on matrix-matched calibration curves with a correlation coefficient in excess of 0.99 for the 7 mycotoxins. The dectection limits were ranged 0.74~2.13 ng/g, with mean recoveries between 73.10~97.46% except aflatoxin $B_1$ (61.31%). We also monitored mycotoxin residues in 208 pork samples. The test results, mycotoxins were not found except one sample. Ochratoxin A in one sample of the test samples was detected below the quantification limit.

• 한국버섯학회지
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• 제11권2호
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• pp.107-110
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• 2013

This study was carried out to optimize the conditions for a chemotaxonomic classification of Ganoderma species. The mycelia of Ganoderma species were extracted with 100% MeOH, and the concentrated extracts were further purified and partitioned with column chromatography (HP20) and n-BuOH, respectively. From the result of high-performance liquid chromatography (HPLC), the constituents of the samples were efficiently separated with a Chemco Pak $C_{18}$ column ($250mm{\times}4.6mm$) by linear gradient elution using water and acetonitrile as mobile phase components at a flow rate of 0.8 ml/min and detector wavelength at 210 nm. However, the samples without purification or partition were not detected the characteristic peaks. This profile could be used to classify and identify the various Ganoderma species.

• 분석과학
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• 제23권4호
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• pp.405-413
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• 2010

축산물(소의 근육 및 간)중에 잔류하는 합성 글루코코티코이드 6종 (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, flumethasone)에 대한 동시분석방법을 확립하였다. 효과적인 기기분석을 위해서 시료는 C18 고체상 카트리지를 사용하여 에틸아세테이트 용매를 사용하여 추출/정제하였다. C18 컬럼을 사용하여 분리한 후 음이온 전기분무 질량분석법의 multiple reaction monitoring 방법을 사용하여 정량 및 정성 분석을 수행하였다. 효과적이고 감도있는 HPLC-MS/MS 분석을 위해서 0.1% 포름산이 포함된 물과 아세토나이트릴이 이동상 용매로 사용되었다. 메트릭스와 약물의 종류에 따라서 검출한계(LOD)는 $0.2-0.1\;{\mu}g$/kg, 정량한계(LOQ)는 $0.8-3.4{\mu}g$/kg 이었으며, 회수율은 89.5-119.6%이었다. 확립된 기존의 방법들에 비해 6종의 글루코코티코이드의 동시분석 방법이 간소화되었고, 좋은 정확도, 정밀도 및 회수율을 나타내었으며, 축산 육류 중에 잔류하는 글루코코티코이드들 분석하는데 사용될 수 있을 것이다.

• 분석과학
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• 제30권1호
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• pp.32-38
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• 2017

In attempt to contribute in official monographs of Korean Pharmacopoeia, an HPLC method was developed and fully validated for the determination of tolperisone hydrochloride in tablets which have never been published in other forgein Pharmacopoeia. Analysis was carried out in an ODS column ($250{\times}4.6mm$ I.D., $5{\mu}m$) with common solvents include acetonitrile and ammonium hydrophosphate buffer as mobile phase. The assay was validated according to International Conference on Harmonization (ICH) guidelines. The method has good linearity in the range of $5-200{\mu}g/mL$ tolperisone. Intra-day precision varied between 0.04 and 0.10 %. Relative standard deviations of inter-day precision ranged between 0.43 and 1.24 % for peak area. The percentage recovery of the tolperisone ranged between 99.8 and 101.2 % in material. Recoveries in tablets were ranged between 98.7 and 100.8 %, thus confirmed the suitability of method for estimation of tolperisone hydrochloride in tablet dosage form.

• 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.

• 분석과학
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• 제8권3호
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• pp.299-304
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• 1995

정지상으로서 N, N'-bispalmtoyl 1, 12-diaza-3, 4:9,10-dibenzo-5, 8-cyclopentadecane (hexadecyl $NtnOenH_4$)-octadecylsilanized silicas(ODS)와 이동상으로 물을 사용하여 Ba(II), Cr(II), Fe(II) 및 Cu(II)의 흡착특성을 조사하였다. 수용액상 Ba(II), Cr(II), Fe(II) 및 Cu(II)의 결합상수와 흡착도를 조사한 결과 그 순위는 Ba(II)$NtnOenH_4$-octadecylsilanized silicas(ODS)에 흡측되는 금속이온의 농도 증가는 cation chelation mechanism에 의해 설명할 수 있었다. 또한 수용액상에서 Ba(II), Cr(II), Fe(II) 및 Cu(II)이 혼합된 용액에서 Cu(II)의 분리효율이 다른 이온들에 비해서 좋게 나타남을 알 수 있었다.