• 제목/요약/키워드: Quantitation

검색결과 629건 처리시간 0.025초

HPLC Determination and Steady-State Bioavailability Study of Levodropropizine Sustained-release Tablets in Dogs

  • Yan, Lin;Li, Tongling;Zhang, Rongqin;Xu, Xiaohong;Zheng, Pengcheng
    • Archives of Pharmacal Research
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    • 제29권6호
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    • pp.514-519
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    • 2006
  • A simple HPLC method using UV detection was developed and validated for the determination of levodropropizine (LDP) In dog plasma. The sample was prepared for injection using a liquid-liquid extraction method with 1-phenypiperazine as the internal standard. The mobile phase was methanol - diethylamine solution (0.05 M) (20:80, v/v, pH adjusted to 3.0 with $H_3PO_4$) with a detection wavelength of 240 nm. The limit of quantitation (LOQ) of LDP in a biological matrix was determined to be 25.25 ng/mL. The calibration curve was linear across the concentration range of 25.25 to 2020 ng/mL. The intra-day and inter-day precision values (CV%) were within 7% and accuracy (R.E. %) was within 6% of the nominal values for medium (252.5 ng/mL) and high (2020 ng/mL) LDP concentrations. For the LDP concentration at the LOQ, the intra-day and inter-day precision and accuracy were within 20% and 10%, respectively. The average absolute recovery for LDP was 70.28%. This method was successfully used to analyze plasma samples in a steady-state bioavailability study of a newly developed sustained-release LDP tablets (SR) using immediate-release tablets (IR) as the reference. The relative bioavailability of the SR was determined to be $106.3\;{\pm}\;12.8%$ (n=6). The $C_{max}$ of the SR was significantly lower (p<0.05), and the $t_{max}$ was significantly longer than that of the IR (p<0.05). The results of ANOVA and two one-sided tests indicated that the SR exhibited acceptable sustained release properties and was bioequivalent to the IR.

Penicillium islandicum에 의한 황변미독(黃變米毒) Luteoskyrin의 생성(生成) (Formation of Luteoskyrin by Penicillium islandicum)

  • 김용화;이서래
    • 한국식품과학회지
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    • 제10권1호
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    • pp.46-51
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    • 1978
  • 황변미독(黃變米毒)의 일종인 luteoskyrin의 동정(同定) 및 정량법(定量法)을 검토한 후 변질미에서 분리된 Pen. islandicum의 luteoskyrin 생성능(生成能)을 추구한 결과는 다음과 같다. 1) Luteoskyrin은 0.5 N oxalic acid impregnated silicagel G plate로서 acetone : n-hexane : water(6:3:1.5, upper layer)를 전개용매로하는 TLC방법에서 분리(分離)가 가장 좋았다. 분리된 황색물질의 최대흡수파장(吸收波長)은 426, 448nm이었으며 chromatogram을 태양광선에 $2{\sim}3$시간 노출시 자색(紫色)으로 변하였다. 2) Luteoskyrin의 정량법으로서 TLC전개(展開)후 용출비색법(溶出比色法)에서는 4 ppm, densitometry에서는 0.1 ppm이 검출한계(檢出限界)이었다. 미곡 중의 허용량(許容量)을 3.68 ppm이하로 정설할 경우 곡류시료 중 luteoskyrin의 검색(檢索)에는 densitometry가 적합할 것이다. 3) Pen. islandicum에 의한 luteoskyrin 생성능은 Czapek 액체배지에서는 균계체(菌系體) 1g당 11mg, 가압살균한 쌀에서는 1g당 40mg이었다.

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Gamma-PF 보드를 이용한 아날로그 감마카메라의 디지털화 연구 (A Study of Digitalizing Analog Gamma Camera Using Gamma-PF Board)

  • 김희중;소수길;봉정균;김한명;김장휘;주관식;이종두
    • 대한의용생체공학회:의공학회지
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    • 제19권4호
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    • pp.351-360
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    • 1998
  • 아날로그 감마카메라에 비해 디지털 카메라는 Q.C가 편리하고, Calibration과 조작이 매우 쉬운 장점들을 갖고 있어 영상 질을 향상시킬 뿐만 아니라 진단의 정확도를 높일 수 있다. 더욱이, 디지털 카메라로 획득한 디지털 영상은 PACS(Picture Archiving and Communication System) 뿐만 아니라 원격진료에도 활용될 수 있다. 그러나, 많은 병원들이 아직도 아날로그 카메라를 사용하고 있고 이들을 디지털 카메라로 대체하기는 어려운 상황에 있다. 본 연구는 아날로그 감마카메라를 디지털화 할 수 있는지의 가능성을 보는 것이었다. 카메라를 디지털화 한 후 균일도 계수능력 등의 물리적 특성을 측정하였다. 임상에서의 사용 가능성을 보기 위해 아날로그 시스템과 디지털 시스템을 동시에 연결하여 임상 데이터들을 획득하였다. 이들의 결과는 임상환경에서 아날로그 카메라를 디지털화 하 수 있다는 가능성을 보여주었다.

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LC-ESI-MS/MS를 이용한 생체시료 중 브롬화피나베리움의 고감도 분석 및 이를 이용한 생체이용률 평가 (Sensitive Determination of Pinaverium Bromide in Human Plasma by LC-ESI-MS/MS : Applicability to Oral Bioavailability Determination)

  • 박석;이예리;김호현;이희주;김윤균;염정록;한상범
    • Journal of Pharmaceutical Investigation
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    • 제34권6호
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    • pp.513-519
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    • 2004
  • A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

Production and Characterization of a Monoclonal Antibody Against Enrofloxacin

  • Chusri, Manaspong;Wongphanit, Pitikarn;Palaga, Tanapat;Puthong, Songchan;Sooksai, Sarintip;Komolpis, Kittinan
    • Journal of Microbiology and Biotechnology
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    • 제23권1호
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    • pp.69-75
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    • 2013
  • Enrofloxacin is a fluoroquinolone antibiotic approved for the treatment of infections in animals. Because of the side effects to consumers of animal products, the maximum residue limits (MRLs) of enrofloxacin in animal tissues for consumption are regulated. In this study, a monoclonal antibody (mAb) against enrofloxacin was prepared and characterized for the development of a direct competitive enzyme-linked immunosorbent assay (ELISA). The obtained mAb, Enro44, was highly specific for enrofloxacin and had a 50% inhibition concentration ($IC_{50}$) of 1.99 ng/ml in a competitive ELISA, and the limit of detection (LOD) was 0.50 ng/ml. The cross-reactivity of the mAb with other quinolones and fluoroquinolones was lower than 0.01%. The subclass of the mAb Enro44 was identified as IgG1. The antigen (Ag)-captured direct competitive ELISA using the mAb Enro44 was tested on different spiked samples, including chicken muscle, cattle milk, and cattle urine, and the assay demonstrated recoveries of 82-112%, 80-125%, and 78-124%, respectively. Furthermore, the quantitation of enrofloxacin obtained from the ELISA and from high-performance liquid chromatography (HPLC) was in good agreement, with the linear regression coefficient between 0.933 and 1.056. The cDNAs encoding a heavy-chain Fd fragment (VH and CH1) and a light chain of the mAb Enro44 were cloned and sequenced. Taken together, the results obtained reveal a potential use of this mAb in an ELISA for the detection of enrofloxacin in food samples. The information of amino acid sequence of this mAb will be useful for further modification and production of the mAb in a bioreactor.

교반막대추출법(SBSE)과 GC/MS를 이용한 수중의 Geosmin과 2-MIB의 분석 (Analysis of Geosmin and 2-MIB in Water by Stir Bar Sorptive Extraction (SBSE) and GC/MS)

  • 이화자;강임석
    • 대한환경공학회지
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    • 제31권1호
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    • pp.64-69
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    • 2009
  • 수돗물에서 geosmin과 2-MIB에 의한 곰팡이와 흙냄새는 소비자들에 대한 수돗물불신의 주된 요인이다. 따라서 geosmin과 2-MIB의 조기 검출 및 분석방법은 이취미 문제를 예방하는데 있어서 중요한 부분이다. 본 연구에서는 교반막대 추출법 (SBSE)과 GC/MS를 이용하여 geosmin과 2-MIB의 분석방법에 대하여 살펴보았다. 용매를 사용하지 않고 시료를 추출하는 SBSE 방법을 최적화하여 수중의 geosmin과 2-MIB를 분석하는데 적용하였다. 실험 결과 SBSE 방법은 간단하고 신속한 분석이 가능하여 소량(10~20 mL)의 시료를 사용하여 한 번에 많은 시료를 동시에 분석할 수 있었다. 그리고 SBSE 방법은 높은 회수율과 재현성을 보였다. 검출한계는 1~2 ng/L 이었으며 정량한계는 3~6 ng/L 이었다. 무엇보다도 SBSE는 수중의 geosmin과 2-MIB를 분석하는 데에 매우 신뢰성이 있고 실용적인 방법이라고 판단된다.

Uptake of Mitochondrial DNA fragment into Boar Spermatoza for Sperm-Mediated Gene Transfer

  • Kim, Tae-Shin;Yang, Cao;Cheong, Hee-Tae;Yang, Boo-Keun;Lee, Sang-Young;Park, Choon-Keun
    • Reproductive and Developmental Biology
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    • 제30권3호
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    • pp.189-194
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    • 2006
  • Sperm-mediated gene transfer(SMGT) can be used to transfer exogenous DNA into the oocyte at fertilization. The main objective of this study was to assess efficiency of transferring mitochondrial DNA(mtDNA) fragment into boar spermatozoa in either presence or absence of liposome and quality of transfected spermatozoa. The mtDNA of chicken liver was isolated and purified by phenol and alkaline lysis extraction, and it was inserted to plasmid. The genome of transfected spermatozoa treated with DNase I was purified by alkaline lysis, and then amplified by the PCR analysis. After electrophoresis, DNA quantitation of each well was calculated by comparison of the band intensity with standard. As a result, exogenous DNA was composed of mtDNA fragment(1.2 kb) and plasmid(2.7 kb). On the other hand, efficiency of transfection by liposome($9.0{\pm}0.34ng/{\mu}l$) in SMGT was higher than that by DNA solution($6.9{\pm}0.53ng/{\mu}l$). However, there was no significant difference. Transfering exogenous DNA into spermatozoa was completed within 90 min of incubation. In another experiment, there were significant (p<0.05) differences between transfected spermatozoa using both DNA solution and DNA/liposome completes with unheated spermatozoa for viability ($70.8{\pm}1.80$ and $68.0{\pm}2.16%$ vs. $83.3{\pm}1.69%$, respectively) and motility($78.7{\pm}1.59$ and $79.3{\pm}2.14%$ vs. $86.7{\pm}1.59%$, respectively). This study indicates that exogenous mtDNA can be efficiently transferred into boar spermatozoa regardless of the presence of liposome, and transfected spermatozoa can also use insemination and in vitro fertilization to generate transgenic pig.

기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법 (Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry)

  • 나윤철;장윤석;김해동;홍종기
    • 분석과학
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    • 제17권1호
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    • pp.29-36
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    • 2004
  • 본 연구에서는 토양중에 존재하는 폴리브롬화 디페닐에테르 (polybrominated diphenyl ethers, PBDEs)를 동위원소희석법을 이용한 기체크로마토그래피/질량분석기-선택이온검색법에 의해 검출하는 분석방법을 소개하였다. 토양 중 PBDEs는 속실렛 장치로 추출하고 실리카와 플로리실 흡착제를 이용한 고체상 추출법을 비교하였다. 정제 후 추출물은 기체크로마토그래피/질량분석기-선택이온검색방법으로 분석하였으며, 동위원소로 치환된 4종의 PBDEs를 내부표준물질로 이용한 동위원소 희석법으로 8종의 PBDEs를 정량하였다. 속실렛추출 후 플로리실과 실리카 카트리지를 통한 회수율은 각각 30.8~110.8%, 44.4~110.7%이었다. 이 분석법의 검출한계는 0.04~0.3 ng/g로 나타났다.

Analysis of erectile dysfunction drugs and their analogues in counterfeit drugs and herbal medicines by LC-ESI-MS/MS

  • Lee, Ji Hyun;Jeong, Ji Hye;Park, Hyoung-Joon;Do, Jung Ah;Heo, Seok;Cho, Sooyeul;Yoon, Chang-Yong
    • 분석과학
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    • 제29권4호
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    • pp.155-161
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    • 2016
  • Distribution of various illegal or counterfeit drugs of seven approved erectile dysfunction drugs and their analogues has been increased, causing health problems such as cardiovascular disorder, tachycardia, headache, or vision disturbance. We used liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) to determine the erectile dysfunction drugs and their analogues in various counterfeit drugs. Eleven erectile dysfunction drugs and their analogues were detected, with sildenafil and its analogues being the most counterfeited compounds (73.8 %), followed by tadalafil and its analogues (25.4 %). The limits of detection (LOD) and the limits of quantitation (LOQ) of liquid-type and solid-type negative samples ranged from 0.1 to 3.3 ng/mL or ng/g and from 0.3 to 10.0 ng/mL or ng/g, respectively. The recoveries ranged from 84.3 to 112.3 % and 83.2 to 110.2 %, respectively. The contents of sildenafil and tadalafil in the various counterfeit drugs ranged from 21.0 to 947.5 mg/g and from 0.2 to 170.2 mg/g, respectively.

Quantitative Analysis of Bayesian SPECT Reconstruction : Effects of Using Higher-Order Gibbs Priors

  • S. J. Lee
    • 대한의용생체공학회:의공학회지
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    • 제19권2호
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    • pp.133-142
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    • 1998
  • Bayesian SPECT 영상재구성에 있어서 정교한 형태의 사전정보를 사용할 경우 bias 및 variance와 같은 통계적 차원에서의 정량적 성능을 향상시킬 수 있다. 특히, "thin plate" 와 같은 고차의 smoothing 사전정보는 "membrane"과 같은 일반적인 다른 사전 정보에 비해 bias를 개선시키는 것으로 알려져 있다. 그러나, 이와 같은 장점은 영상재구성 알고리즘에 내재하는 hyperparameters의 값을 최적으로 선택하였을 경우에만 적용된다. 본 연구에서는 thin plate와 membrane의 두가지 대표적인 사전정보를 포함하는 영상재구성 알고리즘의 정량적 성능에 대해 집중 고찰한다. 즉, 알고리즘에 내재하는 hyperparameters 가 통계적 차원에서 bias와 variance에 어떠한 영향을 미치는지 관찰한다. 실험에서 Monte Carlo noise trials를 사용하여 bias와 variance를 계산하며, 각 결과를 ML-EM 및 filtered backprojection으로부터 얻어진 bias 및 variance와 비교한다. 결론적으로 thin plate와 같은 고차의 사전정보는 hyperparameters의 선택에 민감하지 않으며, hyperparameters 값의 전 범위에 걸쳐 bias를 개선시킴을 보인다. 걸쳐 bias를 개선시킴을 보인다.

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