• 제목/요약/키워드: Inter-calibration

검색결과 212건 처리시간 0.027초

Effective determination of nicotine enantiomers from e-liquids and biological fluids by high performance liquid chromatography (HPLC) using dispersive liquid-liquid microextraction (DLLME)

  • Song, Seunghoon;Myung, Seung-Woon
    • 분석과학
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    • 제34권4호
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    • pp.180-190
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    • 2021
  • This study compared the efficacy of chiral GC and chiral HPLC for the analysis of nicotine. To develop a suitable dispersive liquid-liquid microextraction (DLLME) method, the following parameters were optimized: pH, extraction solvent, dispersive solvent, type and quantity of salt, and laboratory temperature. The validation of the method was carried out by the established HPLC method. The LODs were 0.11 ㎍/mL and 0.17 ㎍/mL for the (S)- and (R)- enantiomers, respectively. The LOQs were 0.30 ㎍/mL and 0.44 ㎍/mL, respectively. The optimal calibration range was between 0.30-18 ㎍/mL and 0.44-4.40 ㎍/mL, respectively, and the correlation coefficient (r2) was 0.9978-0.9996. The intra-day accuracy was 79.9-110.6 %, and the intra-day precision was 1.3-12.0 %. The inter-day accuracy was 87.8-108.0 %, and the inter-day precision was 4.0-12.8 %. E-liquid and biological fluids (urine and saliva) were analyzed using the established method.

Determination of lisinopril in human plasma by liquid chromatography tendem mass spectrometry and its application to human bioavailibility study

  • Shim, Hee-Ok;Kim, Dong-Chul
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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    • pp.239.1-239.1
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    • 2003
  • This study was to develop a quantification method of lisinopril using liquid chromatography tendem mass spectrometry in human plasma. Quntitation of lisinopril by MRM(multiple reaction monitoring) in the electrospray positive mode was validated according to FDA guideline. Extraction of lisinopril and enalapril as internal standard from plasma was perfomed by means solide phase extraction. The calibration curve of lisinopril showed a good linerarity in the concentration range 2∼200ng/ml. The coefficients of variations for the inter-day and intra-day precision was less than 15%, and the inter-day and intra-day accuracy was 97.6∼101.0%. (omitted)

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순복사계의 야외 상호 비교 및 보정 (Field Intercomparison and Calibration of Net Radiometers)

  • Byung-Kwan Moon;Sang-Boom Ryoo;Yong-Hoon Youn;Jonghwan Lim;Joon Kim
    • 한국농림기상학회지
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    • 제5권2호
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    • pp.128-137
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    • 2003
  • 순복사는 지표 에너지 수지의 가장 근본적인 요소 중 하나이다. 순복사의 정확한 관측을 위해, 주기적이고 지속적인 순복사계 보정이 요구된다. 플럭스 관측에 널리 사용되는, 두 가지 타입의 대표적인 순복사계 (Q-7.1과 CNR1)의 상호 비교 및 보정 실험이 약 4개월 간격으로 두 차례 시행되었다. Q-7.1과 CNR1 간의 차이는 7.7% 이내였고, 표준 기기와의 보정 후 오차는 3.2%이내였다. 순복사계의 반응 차이와 보정 계수는 대기 상태, 특히 계절 변화에 따른 온도 차이에 따라 다르게 나타났다. 결론적으로, 주기적으로 보정된 Q-7.1은 CNR1을 대체하여 장기 관측에 사용될 수 있고, 보정 주기로는 4-6개월이 권장된다.

표준거리측정 시설을 이용한 지상라이다 성능 평가 (Performance evaluation of Terrestrial Laser Scanner over Calibration Baseline)

  • 이인수;이재원
    • 한국측량학회지
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    • 제28권3호
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    • pp.329-336
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    • 2010
  • 본 연구는 시간차방식(TOF: Time of flight)과 근적외선 파장대역(760-3000nm)을 사용하는 지상라이다를 이용해서 다양한 사용자 타깃에 대해 반사도와 거리정확도를 테스트하였다. 특별히 사용자 타깃에 대한 측점군의 반사도는 실내에서 독일 Gretag Macbeth사의 i1 분광광도계로 측정되었다. 그리고 지상라이다의 성능 평가를 위해 정밀 EDM 검기선장에서 지상라이다를 이용해서 타깃을 스캐닝 하여 기준표석간 이격거리를 측정하여 표준거리와 비교하였다. 테스트 결과로서, 약 10m 와 170m 기준표석간 이격거리에 설치된 흰색 수지 타깃을 제외하고, 실험에 이용된 다른 타깃들의 거리측정값은 기준거리와 수 mm 정확도 차이를 보였다. 향후 대기보정, 장비보정, 부가상수와 같이 거리정확도에 영향을 미치는 변수들에 대한 연구가 필요할 것으로 사료 된다.

GC/MS를 이용한 소변 중 대마 대사체 분석의 측정불확도 평가 (Uncertainty Evaluation of the Analysis of 11-Nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol in Human Urine by GC/MS)

  • 김진영;정재철;서승일;서용준;이정직;김종상;인문교
    • 약학회지
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    • 제52권6호
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    • pp.480-487
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    • 2008
  • We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH), the major metabolite of ${\Delta}^9$-tetrahydrocannabinol, in urine sample by solid-phase extraction (SPE) and GC/MS detection. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day and inter-person validation were performed using statistical analysis of several indicative factors. Measurement uncertainty associated with target analyte in real forensic samples was estimated using quality control (QC) data. Traceability of measurement was established through traceable standards, calibrated volumetric glassware and volume measuring device. The major factors of contribution to combined standard uncertainty, were calibration linearity, inter-day repeatability and inter-person reproducibility, while those associated with preparation of analytical standards and sampling volume were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method was 12.05% for THCCOOH.

고속액체크로마토그래피를 이용한 미리스틴산이소프로필증 플루르비프로펜의 정량 (Quantitation of Flurbiprofen in Isopropyl Myristate by High Performance Liquid Chromatography)

  • 김현;지상철
    • Journal of Pharmaceutical Investigation
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    • 제22권1호
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    • pp.63-68
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    • 1992
  • An HPLC procedure with UV detection has been developed for the quantitation of flurbiprofen released into isopropyl myristate used as the receptor phase in an in vitro membraneless drug diffusion cell. The drug and the internal standard (oxaprozin) were extracted from isopropyl myristate with a mixture of dimethylsulfoxide:methanol:water (2:1:1) and quantitated using a reverse phase $C_{18}$ column. The chromatograms were completely free from interfering peaks, and the relative retention times of flurbiprofen and the internal standard were 4.9 and 6.8 min, respectively. Calibration plots were linear over the concentration range of $1-200\;{\mu}g/ml$ of flurbiprofen with correlation coefficients, all higher than 0.99. The mean intra-day precision and accuracy among three replicate sets of the assay in a day were 4.26 and 4.52%, respectively, whereas the mean inter-day precision and accuracy were 3.35 and 3.64%, respectively. The mean recovery of the drug was 92.5% over the calibration range. The method was simple, reliable and accurate for the quantitation of flurbiprofen in unpurified isopropyl myristate.

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Validation, Measurement Uncertainty, and Determination of Bixin and Norbixin in Processed Foods of Animal Resources Distributed in Korea

  • Ga-Yeong Lee;Choong-In Yun;Juhee Cho;Young-Jun Kim
    • 한국축산식품학회지
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    • 제43권6호
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    • pp.949-960
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    • 2023
  • This research aimed to validate a high-performance liquid chromatography method for the quantitative determination of bixin and norbixin in various foods. The Diode Array Detector (495 nm) technique was used. Method was validated for specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy, and the measurement uncertainty was assessed. The calibration curve showed excellent linearity (r2≥0.9999) over the tested concentration range of 0.2-25 mg/L. The LOD and LOQ were 0.03-0.11 and 0.02-0.05 mg/L for bixin and norbixin, respectively. The intra-and inter-day accuracies and precisions were 88.0±1.3-97.0±0.5% and 0.2%-2.6% relative SD (RSD) for bixin and 88.2±0.8-105.8±0.8% and 0.3%-2.7% RSD for norbixin, respectively. Inter-laboratory validation for accuracy and precision was conducted in three laboratories, and these results all met the AOAC guidelines. In addition, the relative expanded uncertainty (<22%) satisfied the CODEX recommendation. Furthermore, products distributed in Korea were monitored for annatto extracts using the proposed method to demonstrate its application. The developed analytical method is reliable for quantifying bixin and norbixin in various foods.

마약남용자 11명의 타액 중 메스암페타민의 분석 (Analysis of Methamphetamine and Amphetamine in Oral Fluid of Eleven Drug Abusers)

  • 김은미;이주선;최혜영;최화경;정희선
    • 약학회지
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    • 제52권6호
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    • pp.419-425
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    • 2008
  • A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

고 에너지 광자선의 표준측정법에 대한 선량 교정 프로그램 개발 (Development of a Dose Calibration Program for Various Dosimetry Protocols in High Energy Photon Beams)

  • 신동오;박성용;지영훈;이창건;서태석;권수일;안희경;강진오;홍성언
    • Radiation Oncology Journal
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    • 제20권4호
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    • pp.381-390
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    • 2002
  • 목적 : 고 에너지 광자선에 대한 기준점에서의 물 흡수선량 계산을 절차상 또는 계산상의 오류를 피하기 위해 공기커마(혹은 조사선량) 교정정수에 토대를 두고 있는 IAEA TRS-277과 AAPM TG-21 및 최근 발표된 새로운 개념의 물 흡수선량 교정정수에 토대를 두고 있는 IAEA TRS-398과 AAPM TG-51 표준측정법에 기초한 고 에너지 광자선의 선량 교정 프로그램을 개발하고자 한다. 대상 및 방법 : 현재 국내외에서 널리 사용되고 있는 고 에너지 광자선에 대한 흡수선량 표준측정법은 IAEA TRS-277과 AAPM TG-21로서 공기커마(혹은 조사선량) 교정정수에 토대를 두고 있어 수식 체계가 복잡하고, 사용된 물리량에 대한 불확정도가 커서 선량측정의 정확성을 향상시키는데 한계가 있다. 최근 국제원자력기구와 미국의학물리학회에서는 새로운 개념의 물 흡수선량 교정정수에 토대를 두고 있는 IAEA TRS-398과 AAPM TG-51을 발표하였다. 개발된 네 종류의 선량 교정 프로그램은 이들 표준측정법에서 사용되고 있는 수식체계와 물리적인 매개변수를 엄격하게 적용하였고, 선량계에 대한 정보 및 물리적인 값에 대한 표와 그래프 값은 수치화하여 데이터베이스화하였다. 이들 프로그램은 윈도우 환경에서 사용이 용이하도록 비쥬얼 $C^{++}$ 언어를 사용하여 각각의 표준측정법에서 권고하고 있는 방법 및 절차에 따라 사용자의 편의성을 고려하여 개발하였다. 결과 : 네 종류의 표준측정법에 대하여 개발된 고 에너지 광자선에 대한 선량 교정 프로그램은 사용자가 병원에서 사용하고 있는 표준측정법을 선택하여 선량측정 절차에 따라 선량계, 선질 특성 및 측정 조건에 관한 정보와 측정 결과를 입력하고, 순차적으로 수행하도록 되어 있어 절차상 혹은 선량 계산에 있어서 사용자간의 오차 및 실수를 최소화할 수 있었다 또한 서로 다른 개념의 네 종류의 표준측정법에 대한 기준점에서의 선량값을 상호 비교할 수 있었다. 결론 : 이 프로그램은 이온함에 대한 정보와 물리적인 자료에 대한 표와 그래프 값들을 수식화하여 데이터베이스함으로써 수작업으로 각 프로토콜의 수행 절차상 혹은 사용자간의 발생할 수 있는 개인적인 실수 및 오차를 줄일 수 있었다. 또한 이 프로그램은 사용자 편의성을 고려하였고, 모든 보정계수와 물흡수선량을 정확하게 계산할 수 있기 때문에 각 표준측정법에 대한 주요한 차이점을 비교 분석할 수 있어 사용자가 적당한 표준측정법을 선택하여 수행하므로써 고 에너지 광자선 선량 교정에 이용시 매우 유익할 것으로 사료된다.

A SDR/DDR 4Gb DRAM with $0.11\mu\textrm{m}$ DRAM Technology

  • Kim, Ki-Nam
    • JSTS:Journal of Semiconductor Technology and Science
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    • 제1권1호
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    • pp.20-30
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    • 2001
  • A 1.8V $650{\;}\textrm{mm}^2$ 4Gb DRAM having $0.10{\;}\mu\textrm{m}^2$ cell size has been successfully developed using 0.11 $\mu\textrm{m}$DRAM technology. Considering manufactur-ability, we have focused on developing patterning technology using KrF lithography that makes $0.11{\;}\mu\textrm{m}$ DRAM technology possible. Furthermore, we developed novel DRAM technologies, which will have strong influence on the future DRAM integration. These are novel oxide gap-filling, W-bit line with stud contact for borderless metal contact, line-type storage node self-aligned contact (SAC), mechanically stable metal-insulator-silicon (MIS) capacitor and CVD Al process for metal inter-connections. In addition, 80 nm array transistor and sub-80 nm memory cell contact are also developed for high functional yield as well as chip performance. Many issues which large sized chip often faces are solved by novel design approaches such as skew minimizing technique, gain control pre-sensing scheme and bit line calibration scheme.

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