• Toxicological Research
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• v.31 no.3
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• pp.299-305
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• 2015

An HPLC analytical method was validated for the quantitative determination of biogenic amines in agricultural products. Four agricultural foods, including apple juice, Juk, corn oil and peanut butter, were selected as food matrices based on their water and fat contents (i.e., non-fatty liquid, non-fatty solid, fatty liquid and fatty solid, respectively). The precision, accuracy, recovery, limit of detection (LOD) and quantification (LOQ) were determined to test the validity of an HPLC procedure for the determination of biogenic amines, including tryptamine, ${\beta}$-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine, in each matrix. The LODs and LOQs for the biogenic amines were within the range of 0.01~0.10 mg/kg and 0.02~0.31 mg/kg, respectively. The relative standard deviation (RSD) of intraday for biogenic amine concentrations ranged from 1.86 to 5.95%, whereas the RSD of interday ranged from 2.08 to 5.96%. Of the matrices spiked with biogenic amines, corn oil with tyramine and Juk with putrescine exhibited the least accuracy of 84.85% and recovery rate of 89.63%, respectively, at the lowest concentration (10 mg/kg). Therefore, the validation results fulfilled AOAC criteria and recommendations. Subsequently, the method was applied to the analysis of biogenic amines in fermented agricultural products for a total dietary survey in Korea. Although the results revealed that Korean traditional soy sauce and Doenjang contained relatively high levels of histamine, the amounts are of no concern if these fermented agricultural products serve as condiments.

• Proceedings of the Plant Resources Society of Korea Conference
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• 2018.10a
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• pp.115-115
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• 2018

매실나무(Prunus mume)의 풋과일인 매실은 피로회복, 소화촉진, 살균 및 항균작용 등 다양한 생리활성을 갖고 있다. 본 연구는 국내 수집 매실 유전자원 172점의 핵심 기능성 물질인 유기산의 함량 특성을 평가하고자 2017년과 2018년 2년간 청매실을 수확하여 옥살산(OA), 사과산(MA), 구연산(CA)의 함량을 HPLC를 이용하여 분석하고 그 연차 변이를 평가하였다. 전체 유전자원 매실의 2년간 총유기산(TA) 함량은 평균 5.5% (최소 3.9%-최대 7.8%)이었으며, MA와 CA 및 OA의 평균 함량은 각각 2.7%, 2.8%, 0.1%였다. 대상 자원 내 유기산별 함량 변이는 CA (RSD=30%)가 MA (RSD=21%)보다 높게 나타났다. 2018년산 매실은 2017년산에 비교할 때 MA와 OA는 함량이 낮아 연차 변이가 인정되었으나 CA는 차이가 없었다. 비록 연차 변이는 있었으나 유전자원별 함량은 MA와 CA 및 TA에서 모두 2017년산과 2018년산간 정의 상관이 인정되어 유기산 함량이 높고 낮은 자원의 특성은 유지됨을 알 수 있었다. 대상 유전자원 중 TA함량이 가장 높았던 자원은 구산매, 용흥흥매, 상금백옥매 등이었으며, 함량이 낮은 자원은 한산매, 지곡매 등이었다. 상기 결과를 통해 매실 유기산 함량관련 국내 매실 유전자원의 유전적 다양성과 연차 변이의 영향을 평가할 수 있었다.

• The Korea Journal of Herbology
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• v.31 no.3
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• pp.29-35
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• 2016

Objectives : Ijung-tang (IJT) is a traditional herbal formula and has been used to treat digestive diseases such as abdominal pain, vomiting, and diarrhea. IJT consists of four herbal medicines, Ginseng radix, Atractylodis rhizoma alba, Zingiberis rhizoma, and Glycyrrhizae radix et rhizoma, containing various bioactive compounds. Quality assesment of IJT preparations was performed by analytical method for determining marker compounds.Methods : Determination of seven marker compounds in IJT preparations was quantitatively conducted by high-performance liquid chromatography equipped with a diode-array detector. The marker compounds were separated on a reversed-phase C18 column and the analytical method was successfully validated. Chemometric analysis was performed to compare IJT water extracts and commercial IJT granules.Results : Limit of detection and limit of quantification values were in the ranges of 0.093-2.649 μg/mL and 0.283-8.027 μg/mL, respectively. Precisions were 0.30-3.87% within a day and 0.23-2.35% over three consecutive days. Recoveries of the marker compounds ranged from 87.35-107.05%, with relative standard deviation (RSD) values < 6.15%. Repeatabilities were < 1.20% and < 1.71% of RSD value for retention time and absolute peak area, respectively. The results from quantitative analysis showed that the quantities of seven marker compounds of IJT samples varied, as were found in principal component analysis and hierarchical clustering analysis.Conclusions : The analytical method developed in the present study was precise and reliable to simultaneously determine marker compounds of IJT. Therefore, it can be used for the quality assessment of IJT preparations.

• Journal of the Korean Chemical Society
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• v.43 no.6
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• pp.663-669
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• 1999

For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

• Bulletin of the Korean Chemical Society
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• v.34 no.3
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• pp.917-921
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• 2013

A simple, quick and reliable analytical method for the confirmation and quantification of propisochlor was developed. The propisochlor was extracted from water, soil and rice (stalks, rice and hull) matrices using acetonitrile, and cleaned up with primary secondary amine and determined by UPLC-MS/MS. The LODs of propisochlor ranged from 0.03 ${\mu}g/kg$ to 0.12 ${\mu}g/kg$, while the LOQs ranged from 0.1 ${\mu}g/kg$ to 0.4 ${\mu}g/kg$ in different matrixes. The mean recoveries of propisochlor at three levels (0.005, 0.01 and 0.05 mg/kg) were in the range of 73.7-94.9% with intra-day relative standard deviations (RSD) of 1.1-13.9% and inter-day $RSD_R$ of 3.3-12.7%. This method is suitable for routine analysis of propisochlor under field conditions. The half-lives of propisochlor in rice stalks, water and soil were 1.7, 1.5 and 2.3 days in Hunan, 5.7, 1.0 and 1.9 days in Anhui and 4.8, 1.0 and 3.1 days in Guangxi.

• Journal of the Korean Chemical Society
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• v.54 no.3
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• pp.283-286
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• 2010

A sensitive and reproducible method for the flotation-spectrophotometric determination of zirconium is reported. The method is based on the complex formation zirconium and xylenol orange (XO) which is floated in the interface of aqueous phase and n-hexane by vigorous shaking. By discarding the aqueous solution and n-hexane, the adsorbed complex on to the wall of a separating funnel was dissolved in a small volume of methanol solvent and its absorbance was measured at 429 nm. The effect of different parameters such as pH, concentrations of HCl, and XO, and volume of n-hexane flotation dissolvent, standing and shaking time were studied. The calibration curve was linear in the range of 7-120 ng $mL^{-1}$ of zirconium with a correlation coefficient of 0.9991. The limit of detection (LOD) was 5.8 ng $mL^{-1}$. The relative standard deviation (RSD) for seven replicate measurements of 50 and 110 ng $mL^{-1}$ of zirconium were 4.4 and 3.0%, respectively. The method was successfully applied to the determination of zirconium in water samples.

• Herbal Formula Science
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• v.21 no.1
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• pp.71-79
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• 2013

Objectives : Yijin-tang has been used in the treatment of gastrointestinal diseases such as irritable bowel syndrome, gastritis, and gastric ulcer. In this study, a high-performance liquid chromatography (HPLC) method was established for simultaneous analysis of six compounds, liquiritin, glycyrrhizin, hesperidin, 6-gingerol, homogentisic acid, and 3,4-dihydroxybenzaldehyde in Yijin-tang, a traditional Korean herbal medicinal preparation. Methods : A Gemini C18 column was used for the separation of six constituents at $40^{\circ}C$. The mobile phase using gradient elution consist of two solvent systems, 1.0% acetic acid in water (A) and 1.0% acetic acid in acetonitrile (B). The flow-rate was 1.0 mL/min and injection volume was $10{\mu}g$. The detector was a photodiode array (PDA) detector set at 254 nm and 280 nm. Results : The calibration curves of six compounds showed good linearity in various concentration ranges ($R^2{\geq}0.9997$). The limits of detection (LOD) and limits of quantification (LOQ) were 0.028-$0.192{\mu}g/mL$ and 0.093-$0.540{\mu}g/mL$, respectively. The RSD (%) of the intra and inter day validations were 0.03-0.84% and 0.05 -1.00%, respectively. Recovery was 96.14-01.90% and RSD (%) was less than 1.5%. Conclusions : The established simultaneous analysis methods will help management to improve the quality of Yijin-tang.

• The Journal of Korean Medicine
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• v.32 no.3
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• pp.25-34
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• 2011

Objectives: We performed simultaneous determination of five constituents by HPLC in Samul-tang (SMT). Additionally, we investigated the immune-stimulatory potential of SMT on specific cellular and humoral immune responses in ovalbumin (OVA)-immunized mice. Methods: Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 190-400 nm, were used for quantification of the five components of SMT. Mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. C57BL/6 mice were immunized intraperitoneally with OVA/alum ($100{\mu}g/200{\mu}g$) on days 1, 8, and 15. The extract of SMT (1000 mg/kg) was given to mice orally for 21 days (from day 1 to day 21). At day 22, OVA-, lipopolysaccharide (LPS)- and concanavalin A (Con A)-stimulated splenocyte proliferation and OVA-specific and total antibodies were measured in plasma. Results: Calibration curves were acquired with $r^2$>0.9999, and the relative standard deviation (RSD, %) for intra- and inter-day precision were both less than 3.5%. The recovery was in the range of 95.69-115.12%, with an RSD less than 6.0%. The contents of five components in SMT were 1.08-15.30 mg/g. SMT significantly enhanced Con A-induced splenocyte proliferation in OVA-immunized mice (p<0.01). Also, SMT significantly enhanced OVAspecific IgG, IgG1 and total IgM levels in plasma compared with the OVA-immunized group. Conclusions: The established method will be applied for the quantification of major components and immunestimulating activity in OVA-immunized mouse model of SMT.

• Proceedings of the Korean Vacuum Society Conference
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• 1999.07a
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• pp.192-192
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• 1999

SIMS(Secondary Ion Mass Spectrometry)는 다른 표면 분석장비와 비교하여^g , pp m,^g , pp b 단위의 미량분석이 가능한 장비로서, 특히 depth Profiling을 위한 dynamic SIMS는 Mass Spectrometer의 종류에 따라 Quadrupole SIMS (Q-SIMS)와, Magnetic Sector SIMS (M-SIMS)로 분류된다. 한편, Q-SIMS와 달리 M-SIMS의 경우, Transmission을 높여 주기 위해 Sample Holder에 수 keV의 bias를 걸어 주는데, 이로 인하여 분석 원소에 대한 Sensitivity가 향상되어 지는 반면, RSF의 변화와 같은 분석상의 Artifact가 발생하게 된다. 일반적으로 Q-SIMS의 경우에는 RSF의 RSD(Relative Standard Deviation)가 1%이내에서 보고되고 있지만 M-SIMS에 있어서는 이러한 Deviation이 M-SIMS보다 크게 나타난다. 이 차이는 주로 Sample Holder와 Immersion Lens 사이에 형성되는 Magnetic Field의 왜곡과 Spectrometer의 문제로부터 발생한다. 본 논문에서는 Sample Holder의 종류 및 holder so window 위치에 따라 RSF의 차이를 측정하고 그 data를 RS/1 통계 Package를 이용하여 계량적으로 검증하였으며, 그 차이의 원인과 대책을 제시하고자 한다. 실험에 사용된 Sample은 Si(100) p-type Wafer에 Boron을 이온 주입하여 제작하였다. 이온 주입 장비는 Varian E-500HP이며, 5.0E13 ions/cm2의 dose양을 80keV의 Energy로 각각 7도와 22도의 Tilt와 Twist Angle로 이온 주입을 하였다. SIMS분석에 사용된 Sample Holder는 각각 3 Hole, 9 Hole Type HOlder이며, 분석은 Cameca IMS-6f를 사용하여 B에 대한 Matrix Peak으로 28Si++를 얻었다. 실험 결과 3 Hole Type Sample Holder의 경우 RSF의 RSD는 5.84%, 9Hle Type Sample Holder의 경우는 14.3%로 나타났으나 분석 Window의 위치에 따르는 Grouping을 실시한 결과, 3 Hole Type Sample Holder의 경우 1.2%, 9Hole Type Sample Holder의 경우 9.8%로 RSF의 변화가 감소하였다. 이러한 Deviation은 Sample Holder를 Mount시킬 때 세 개의 Screw를 이용하여 Immersion Lens와의 평형을 잡아주기 때문에 발생하며, 이 Munting을 정확히 해줌으로써 RSF의 변화를 줄일 수 있으나, 실제로 완벽한 Mounting이 불가능하기 때문에 RSF를 일정하게 하기 위해서는 Sample Holder so Window의 취치를 일정하게 설정한 후 분석을 실시해야 한다고 판단된다.

• The Korea Journal of Herbology
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• v.30 no.3
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• pp.19-24
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• 2015

Objectives : HPL-1, a novel herbal medicine which is composed of five herbs such as Kalopanacis Cortex, Chaenomelis Fructus, Raphani Semen, Atractylodis Rhizoma and Pulvis Aconiti Tuberis Purificatum, was developed for treatment of osteoarthritis. This study is aimed to develop analytical method for consistent quality control of HPL-1 and validate chromatographic method. Methods : Chromatographic analysis was performed using ultra-high performance liquid chromatography - diode array detector (UHPLC-DAD) equipped with RP-amide column, column oven, and auto sampler. Marker compounds [protocatechuic acid, chlorogenic acid, liriodendrin, 3,5-dicaffeoylquinic acid, ${\beta}$-D-(3-O-sinapoyl)-fructofuranosyl-$\alpha$-D-(6-O-sinapoyl)glucopyranoside and benzoylmesaconine] were separated by step gradient elution of acetonitrile and 0.1% phosphoric acid/water. The method validation was evaluated by quantitative validation parameters of linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ) according to KFDA guideline.Results : An optimized method for six marker compounds in HPL-1 was established by UHPLC-DAD. The correlation coefficient (R²) with each calibration curve was greater than 0.99. The LOD and LOQ were within the range of 0.008-0.090 and $0.023-0.274{\mu}g/mL$, respectively. The relative standard deviation (RSD) of intra- and inter-day variability were less than 4.0%. The result of recovery test was range from 93.3-106.3% with RSD < 4.0%.Conclusions : These results suggest that the quantitative UHPLC method is precise, accurate, effective for quality evaluation of HPL-1. The method may also contribute to improve quality of crude drug preparations used for treatment of various diseases.