• 제목/요약/키워드: % RSD

검색결과 528건 처리시간 0.029초

국내 수집 매실유전자원의 청매실 함유 유기산 함량의 연차 변이 (Year-dependent variations of organic acid contents in pre-matured fruits of 175 Korean Prunus mume landraces.)

  • 곽보경;엄소영;;강희경;이영상
    • 한국자원식물학회:학술대회논문집
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    • 한국자원식물학회 2018년도 추계학술대회
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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.

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HPLC 분석법을 이용한 이중탕(理中湯) 제제의 품질평가 (Quality Assessment of Ijung-tang Preparations Using a HPLC Analysis)

  • 하우람;박진형;윤동인;이장천;김정훈
    • 대한본초학회지
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    • 제31권3호
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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.

HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구 (Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC)

  • 오보영;배준현;강준길;김연두
    • 대한화학회지
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    • 제43권6호
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    • pp.663-669
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    • 1999
  • HPLC/UV 및 GC/FPD 법을 사용하여 환경수에 존재하는 Diazinon, EPN, Fenitrothion, Phosalon 및 Phosmet 등 5종의 유기인계 잔류농약을 분석하였다. 전처리 과정으로 고체상추출법(SPE)과 용매추출법(LLE)을 각각 적용한 결과, 회수율과 재현성에 있어, HPLC/UV에서는 용매추출법(LLE)보다 고체상추출법(SPE)이 더 우수하였고, GC/FPD에서는 고체상추출법(SPE)보다 용매추출법(LLE)이 더 우수하였다. 또 수돗물 및 하천수(와룡천)에 일정량의 유기인계 농약을 가하여 만든 합성시료중 각 성분을 분석한 결과, SPE-HPLC/UV 법에서는 회수율이 101%, % RSD는 4.3∼8.7이었고, LLE-GC/FPD 법에서는 회수율이 100%, % RSD는 3.2∼9.5이었다. 이 결과는 두 방법 모두 유기인계 잔류농약 분석에 이용할 수 있는 우수한 방법임을 제시하고 있다.

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Determination of Herbicide Propisochlor in Soil, Water and Rice by Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) Method Using by UPLC-ESI-MS/MS

  • Wu, Xiaohu;Xu, Jun;Liu, Xingang;Dong, Fengshou;Wu, Yanbing;Zhang, Ying;Zheng, Yongquan
    • Bulletin of the Korean Chemical Society
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    • 제34권3호
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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.

부유 - 분광광도법에 의한 지르코늄의 극미량 측정 (Determination of Trace Amounts of Zirconium by Flotation - Spectrophotometric Method)

  • Pourreza, N.;Parham, H.;Shiri, S.
    • 대한화학회지
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    • 제54권3호
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    • pp.283-286
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    • 2010
  • 지르코늄의 부유-분광 광도의 측정에 대한 감도가 좋고 재현성 있는 방법이 기록되었다. 그 방법은 지르코늄과 자일렌오렌지(XO)착물 형성에 기초하였고 그것은 격렬한 진탕에 의해 수용액 상과 n-헥산의 표면에 떠있게 된다. 수용액과 n-헥산을 폐기함에 따라 분리된 깔대기의 벽에 있던 흡착된 착물은 작은 부피의 메탄올 용액으로 해리되어진다. 그리고 그것의 흡광도는 429 nm에서 측정되었다. PH, HCl, XO의 농도, n-헥산 부유 용매의 부피, 지속시간과 진탕시간과 같은 다른 변수의 효과가 연구되었다. 보정곡선은 0.9991의 상관계수를 갖는 지르코늄의 7 ~ 120 ng/mL의 범위에서 선형이었다. 검출한계(LOD)는 58 ng/mL이었다. 지르코늄의 50과 110 ng/mL 의 7개의 분할척정에 대한 상대표준편차(RSD)는 4.4와 3.0%였다. 이 방법은 물샘플에서 지르코늄의 측정에 성공적으로 적용되었다.

HPLC-PDA을 이용한 이진탕 중 6종 성분의 동시분석 (Simultaneous Analysis of Six Compounds in Yijin-tang by HPLC-PDA)

  • 김성실;김정훈;신현규;서창섭
    • 대한한의학방제학회지
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    • 제21권1호
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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.

Evaluation of the Immune-Stimulating Activity of Samul-tang, a Traditional Korean Herbal Medicine, Standardized by HPLC-PDA

  • Seo, Chang-Seob;Ha, Hye-Kyung;Jung, Da-Young;Lee, Ho-Young;Shin, Hyeun-Kyoo
    • 대한한의학회지
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    • 제32권3호
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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.

Magnetic Sector SIMS의 Sample Holder 위치에 따르는 RSF (Relative Sensitivity Factor) 변화 검증

  • 홍성윤;이종필;홍태은;윤명노;민경열;이순영
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 1999년도 제17회 학술발표회 논문개요집
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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.

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UHPLC를 이용한 새로운 한약제제 HPL-1의 품질관리법 개발 (Development of Quality Control Method for a Novel Herbal Medicine, HPL-1 using UHPLC)

  • 김세건;라마칸타라미차네;이경희;정현주
    • 대한본초학회지
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    • 제30권3호
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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.

가구 형태별 여자 노인의 식사 및 건강상태 (Diet and Health Status of Elderly Women According to the Family Type)

  • 최미경;강명화;김미현
    • 대한지역사회영양학회지
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    • 제21권3호
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    • pp.256-264
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    • 2016
  • Objectives: This study aimed to evaluate the diet and health status of elderly women according to the family type. Methods: A total of 307 elderly women participated in this study were divided into one of three groups according to their family type: residing with spouse (RSP; n=88), residing with son or daughter (RSD; n=119), and residing alone (RAL; n=100). Chisquare test was used to assess dietary habits and health status of the subjects by the family types. Results: Results demonstrated significant associations between eating regular meals, person preparing meals, coffee intake, and bone fracture experience and family type. Among the three groups, the RSP and RAL groups had a higher percentage for preparing meals by themselves (p<0.001) than the RSD group. The RAL group had a lower percentage for eating regular meals (p<0.01) but a higher percentage for bone fracture experience (p<0.05) than the other groups. There were no significant differences in monthly allowance, self-estimated health status, physical activity, exercise, drinking, and dietary habits such as frequency of consumption of dairy, beans, eggs, fish, meat, fruits, and vegetables among the three groups. Conclusions: The results showed that elderly women residing alone without a son, daughter, or spouse had more diet-related and health problems such as irregular meals and high bone fracture experience. These findings suggested that elderly women residing alone need more attention and support.