• 제목/요약/키워드: G7 calibration

검색결과 177건 처리시간 0.024초

LC-MS/MS를 이용한 천왕보심단(天王補心丹)의 함량분석 및 항산화 효능 연구 (Quantitative Determination and Antioxidant Effects of Cheonwangbosimdan)

  • 서창섭;김온순;신현규
    • 생약학회지
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    • 제45권4호
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    • pp.300-314
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    • 2014
  • An ultra-performance liquid chromatography-electrospray ionization-mass spectrometer (UPLC-ESI-MS) method was established for the simultaneous quantification of eighteen marker compounds in traditional Korean formula, Cheonwangbosimdan (CWBSD). In addition, we evaluated the antioxidant effects of CWBSD. Eighteen marker components were separated on a UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) and kept at $45^{\circ}C$ by gradient elution with 0.1% (v/v) formic acid in water and acetonitrile as mobile phase. The flow rate was 0.3 mL/min and the injection volume was $2.0{\mu}L$. The antioxidant activities of CWBSD were assessed by measuring free radical scavenging activities on 2,2'-azinobis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The calibration curves of all analytes showed good linearity (correlation coefficient ${\geq}0.9937$) within the test ranges. The limits of detection and quantification for the 18 marker compounds were 0.01-4.71 ng/mL and 0.03-14.13 ng/mL, respectively. The contents of the 18 compounds in CWBSD extract ranged from none to $1701.00{\mu}g/g$. The CWBSD showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction ($RC_{50}$) against ABTS and DPPH radicals were $149.42{\mu}g/mL$ and $339.24{\mu}g/mL$.

Analysis of antibiotic residues in milk from healthy dairy cows treated with bovine mastitis ointment using ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry

  • Park, Eun-Kee;Ryu, Yong-Jae;Cha, Chun-Nam;Yoo, Chang-Yeul;Kim, Suk;Lee, Hu-Jang
    • 대한수의학회지
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    • 제56권4호
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    • pp.233-239
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    • 2016
  • This study was conducted to analyze penicillin G (PEG), streptomycin (STR) and neomycin (NEO) residues in milk of healthy lactating cows. Milk samples were collected from all four quarters of 12 dairy cows 2−7 days after intramammary infusions of an ointment containing PEG, STR and NEO once (n = 4; group I) or twice (n = 4, group II) daily. Ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry was used to determine the antibiotic residues in the samples. The correlation coefficient ($r^2$) of the calibration curves for all antibiotics was > 0.999 and the limits of detection and quantification were $0.002-0.005{\mu}g/mL$ and $0.007-0.02{\mu}g/mL$, respectively. Recovery rates were ranged from 75.5 to 92.3%. In group I, PEG, STR and NEO residues were detected in milk at 2, 3 and 2 days post-treatment, respectively, which were below the maximum residue limit (MRL). In group II, PEG, STR and NEO residues were detected in milk at 2, 3 and 3 days post-treatment, respectively, which were bellow the MRL. These results suggest that a 3-day for milk withdrawal period after the ointment treatment might be sufficient for reduction of the antibiotic residues below the MRL.

표준백금저항온도계를 이용한 온도측정능력 상호비교 (Inter-comparison of temperature measurement capability using standard platinum resistance thermometers)

  • 감기술;강주식;이용재;이광복;김용규;박승남
    • 센서학회지
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    • 제18권1호
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    • pp.86-94
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    • 2009
  • Temperature measurement capability was inter-compared using the transfer standard platinum resistance thermometers(SPRT) among four laboratories of KRISS. The transfer SPRTs were primarily calibrated at the triple point of water and Ga melting point, then used at inter-comparison experiment. Temperature difference of calibration value between temperature laboratory and length laboratory at $20^{\circ}C$ was -0.7 mK and +2.4 mK at density laboratory. Temperature measured near $20^{\circ}C$, $25^{\circ}C$ and $30^{\circ}C$ at fluid flow laboratory was deviated by $34.2{\sim}80.4\;mK$ from the calibration values of the transfer SPRT. Ga melting points was inter-compared among three laboratories, and the difference of Ga melting points against the standard Ga melting point of temperature laboratory were $0.03{\sim}0.54\;mK$ at length laboratory and 0.02 mK at density laboratory.

Use of Near-Infrared Spectroscopy for Estimating Lignan Glucosides Contents in Intact Sesame Seeds

  • Kim, Kwan-Su;Park, Si-Hyung;Shim, Kang-Bo;Ryu, Su-Noh
    • Journal of Crop Science and Biotechnology
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    • 제10권3호
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    • pp.185-192
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    • 2007
  • Near-infrared spectroscopy(NIRS) was used to develop a rapid and efficient method to determine lignan glucosides in intact seeds of sesame(Sesamum indicum L.) germplasm accessions in Korea. A total of 93 samples(about 2 g of intact seeds) were scanned in the reflectance mode of a scanning monochromator, and the reference values for lignan glucosides contents were measured by high performance liquid chromatography. Calibration equations for sesaminol triglucoside, sesaminol($1{\rightarrow}2$) diglucoside, sesamolinol diglucoside, sesaminol($1{\rightarrow}6$) diglucoside, and total amount of lignan glucosides were developed using modified partial least square regression with internal cross validation(n=63), which exhibited lower SECV(standard errors of cross-validation), higher $R^2$(coefficient of determination in calibration), and higher 1-VR(ratio of unexplained variance divided by variance) values. Prediction of an external validation set(n=30) showed a significant correlation between reference values and NIRS estimated values based on the SEP(standard error of prediction), $r^2$(coefficient of determination in prediction), and the ratio of standard deviation(SD) of reference data to SEP, as factors used to evaluate the accuracy of equations. The models for each glucoside content had relatively higher values of SD/SEP(C) and $r^2$(more than 2.0 and 0.80, respectively), thereby characterizing those equations as having good quantitative information, while those of sesaminol($1{\rightarrow}2$) diglucoside showing a minor quantity had the lowest SD/SEP(C) and $r^2$ values(1.7 and 0.74, respectively), indicating a poor correlation between reference values and NIRS estimated values. The results indicated that NIRS could be used to rapidly determine lignan glucosides content in sesame seeds in the breeding programs for high quality sesame varieties.

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UHPLC를 이용한 볏짚 사일리지와 동계사료작물의 오크라톡신과 제랄레논 분석법 최적화 (Optimization of Analytical Methods for Ochratoxin A and Zearalenone by UHPLC in Rice Straw Silage and Winter Forage Crops)

  • 함현희;문혜연;이경아;이수형;홍성기;이데레사;류재기
    • 한국초지조사료학회지
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    • 제36권4호
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    • pp.333-339
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    • 2016
  • 조사료에서 오크라톡신 A (OTA) 및 제랄레논(ZEA)의 단성분 분석법을 최적화하기 위하여 곰팡이 독소에 오염되지 않은 볏짚 사일리지, 이탈리안 라이그라스, 청보리, 호밀을 대상으로 각 시료 별로 OTA는 50, 250, $5,000{\mu}g/kg$, ZEA는 300, 1,500, $3,000{\mu}g/kg$의 농도로 스파이킹하고 면역친화성 컬럼을 이용하여 독소를 정제한 후 UHPLC-FLD를 이용하여 분석하였다. 분석 결과 표준용액의 검량선은 OTA가 결정계수 0.9999, ZEA가 0.9995로 높은 직선성을 나타냈으며, 검출 및 정량한계는 OTA가 각각 $0.1{\mu}g/kg$, $0.3{\mu}g/kg$, ZEA는 각각 $5{\mu}g/kg$, $16.7{\mu}g/kg$을 나타냈다. 유효성 및 정밀성 검정결과 OTA는 볏짚이 회수율 84.23~95.33%, 상대표준편차 (RSD) 2.59~4.77%, 이탈리안 라이그라스는 회수율 79.02~95%, RSD 0.86~5.83%, 청보리는 회수율 74.93~97%, RSD 0.85~9.19%, 호밀은 회수율 77.99~96.67%, RSD 0.33~6.26%를 나타냈으며, ZEA는 볏짚이 회수율 109.6~114.22%, RSD 0.67~7.15%, 이탈리안 라이그라스는 회수율 98.01~109.44%, RSD 1.65~4.81%, 청보리는 회수율 98~113.53%, RSD 0.25~5.85%, 호밀은 회수율 90.44~108.56%, RSD 2.5~4.66%를 나타내어 유럽연합에서 제시한 기준을 만족하였다. 따라서 본 연구에서 제시한 분석법은 국내의 볏짚 등 조사료 4종에서 OTA와 ZEA의 분석에 활용할 수 있음을 시사하였다.

기체크로마토그래피/질량분석기에 의한 수질, 토양 및 저질 시료중의 benzophenone 분석법에 관한 연구 (Determination of benzophenone in water, soil and sediment by gas chromatography/mass spectrometry)

  • 전희경;최해연;류재천
    • 분석과학
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    • 제18권2호
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    • pp.147-153
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    • 2005
  • 본 연구는 GC/MS를 이용하여 수질, 토양 및 저질 시료 중의 benzophenone (BP)을 분석하는 방법을 확립하고자 하였다. BP는 수질 시료 (100 mL)에서 n-hexane으로 추출하였으며, 토양 및 저질 시료 (10 g)에서는 먼저 메탄올로 추출한 후 hexane으로 다시 추출하여 농축시켜 분석하였다. 수질 시료 중의 BP 회수율은 71.4% 이상이었으며 토양에서의 회수율은 86.5-94.7%를 보였고 재현성은 19.8% 이하였다. 검정곡선은 상관계수 ($r^2$) 값이 수질과 토양 모두에서 0.998이상의 좋은 직선성을 보여주었다. 수질 시료의 경우 43지역 중 3지역의 수질에서 30-200 ng/L 농도 범위로 BP가 검출되었으며 토양과 저질 시료에서는 모든 지역에서 검출되지 않았다. 이 분석방법은 환경 중에 미량으로 존재하는 BP의 분석과 모니터링에 유용하게 사용할 수 있는 적합한 방법이라 사료된다.

LC-ESI-MS/MS를 이용한 계지탕 중 주요 성분 분석 (Quantitative Determination of the Bioactive Marker Components in Gyeji-tang Using LC-ESI-MS/MS)

  • 서창섭;하혜경
    • 생약학회지
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    • 제49권1호
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    • pp.76-83
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    • 2018
  • A traditional herbal formula, Gyeji-tang has been used to treat the early colds, headache, chills, and fever in Asian countries. In this study, we were performed simultaneous determination of the 14 bioactive marker compounds, gallic acid, spinosin, paeoniflorin, albiflorin, liquiritin apioside, liquiritin, 6'''-feruloylspinosin, liquilitigenin, coumarin, cinnmamic acid, benzoylpaeoniflorin, cinnamaldehyde, glycyrrhizin, and 6-gingerol in Gyeji-tang using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS). Analytical column was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) and maintained at $45^{\circ}C$ with a flow rate of 0.3 mL/min. The mobile phase consists of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was conducted using multiple reaction monitoring in the positive and negative modes by a Waters ACQUITY TQD LC-MS/MS system. The calibration curves of 14 bioactive marker compounds showed linearity with correlation coefficients ${\geq}0.9798$. The limits of detection and quantification values were in the range of 0.11-6.66 ng/mL and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the established LC-MS/MS method, the amounts of tested 14 compounds in the lyophilized Gyeji-tang sample were detected up to $85.7{\mu}g/g$. These results may be useful for quality assessment of a traditional herbal formulas.

LC-MS/MS를 이용한 반하사심탕 물 추출물 중 13종 성분의 함량분석 (Quantitative Determination of the Thirteen Marker Components in Banhasasim-Tang Decoction Using an Ultra-Performance Liquid Chromatography Coupled to Electrospray Ionization Tandem Mass Spectrometry)

  • 서창섭;신현규
    • 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.

관성 센서 데이터를 활용한 3 DoF 이미지 스티칭 향상 (Enhancement on 3 DoF Image Stitching Using Inertia Sensor Data)

  • 김민우;김상균
    • 방송공학회논문지
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    • 제22권1호
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    • pp.51-61
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    • 2017
  • 본 논문은 수평을 유지하여 촬영해야 한다는 기존 이미지 스티칭을 이용한 영상 정합 과정의 단점을 극복하기 위하여, 스마트폰의 가속도 센서와 자기장 센서 데이터를 사용하여 3가지 자유도(3 DoF)에 강인한 이미지 스티칭 방법을 제안한다. 이미지를 붙이는 작업인 이미지 스티칭은 크게 이미지 특징점 추출, 추출된 특징점에서 매칭에 필요한 참인 점(inlier)을 선별, 참인 점을 호모그래피(homography) 행렬로 변환, 호모그래피 행렬을 사용하여 이미지를 왜곡(warping), 왜곡된 이미지와 다른 이미지를 합하는 과정으로 이루어져 있다. 본 논문에서는 일반적으로 사용하는 SIFT, SURF 등의 알고리즘뿐만 아니라 MPEG에서 표준화한 MPEG-7 CDVS(Compact Descriptor for Visual Search) 표준의 특징점 추출 알고리즘을 사용하여 이미지의 특징점을 추출한다. 또한 각 알고리즘의 특징점 추출시간, 추출된 특징점 개수, 선별된 참인 점의 개수를 비교하고, 스티칭 정확도를 판단하여 본 연구에서 활용한 데이터에 어느 알고리즘이 효율적인지 살펴본다.

UPLC-MS/MS를 이용한 작약감초탕 물 추출물 중 11종 성분의 함량분석 (Quantitative Analysis of the Eleven Marker Components in Traditional Korean Formula, Jakyakgamcho-Tang Decoction Using an Ultra-Performance Liquid Chromatography Coupled to Electrospray Ionization Tandem Mass Spectrometry)

  • 서창섭;신현규
    • 약학회지
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    • 제60권2호
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    • pp.64-72
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    • 2016
  • Jakyakgamcho-tang is a well-known traditional herbal medicine and has been used for the treatment of mainly pains in oriental medicine. In this study, analytical method for the quantitative determination of the eleven marker components, gallic acid (1), oxypaeoniflorin (2), paeoniflorin (3), albiflorin (4), liquiritin (5), isoliquiritin (6), ononin (7), liquiritigenin (8), benzoylpaeoniflorin (9), paeonol (10), and glycyrrhizin (11) in Jakyakgamcho-tang decoction was performed using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer. The analytical column for separation of the compounds 1~11 was used 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) aqueous formic acid (A) and acetonitrile (B) by gradient elution. The flow rate was 0.3 ml/min and injection volume was $2.0{\mu}l$. Correlation coefficient in the calibration curves of the compounds 1~11 were showed a good linearity with more than 0.99. The limit of detection and limit of quantification values of the compounds 1~13 were detected in the ranges 0.06~18.43 ng/ml and 0.18~58.29 ng/ml, respectively. Among the compounds 1~11, the compounds 10 were not detected in this sample, while the ten compounds, 1~9 and 11, were detected $44.05{\sim}19,289.05{\mu}g/g$ in Jakyakgamcho-tang extract.