• Title/Summary/Keyword: Inter-day variation

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The Rapid Determination of Gemcitabine by Reversed-phase Ultra-Performance Liquid Chromatography (역상 초고속액체크로마토그라피에 의한 gemcitabine의 빠른 농도 분석법)

  • Park, Dae-Jin;Kim, Woo-Mi
    • Journal of Life Science
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    • v.19 no.12
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    • pp.1698-1704
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    • 2009
  • Gemcitabine is an anticancer drug used to treat a variety of solid tumors. The drug is rapidly inactivated by cytidine deaminase in plasma and its hydrophilicity restricts the extent of quantification that is possible using reversed-phase liquid chromatography. In this paper, we report a rapid and precise method to analyze velocity and peak efficiency using ultra-performance liquid chromatography (UPLC) with a reversed-phase column. The retention periods of gemcitabine and 2'-deoxycytidine at 283 nm were 3.2 and 2.1 min, respectively. The assay provided highly linear results in the range of $0.1{\sim}20{\mu}g/ml$ ($r^2$ > 0.999). The coefficients of variation of the intra-day and inter-day assays were less than 10.0%. We observed that the estimated average concentrations of the intra-day and inter-day assays ranged from 97.3 to 113.5% to verify the accuracy. These results suggest that this new reversed-phase UPLC method is a rapid and reliable way of determining gemcitabine levels.

HPLC Determination of Diltiazem and Deacetyldiltiazem in Rat Plasma (HPLC를 이용한 랫트 혈장중의 딜타아젬 및 데아세틸딜티아젬의 정량)

  • Lee, Yong-Hee;Shim, Chang-Koo;Lee, Min-Hwa;Kim, Shin-Keun
    • Journal of Pharmaceutical Investigation
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    • v.22 no.4
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    • pp.317-321
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    • 1992
  • A high-performance liquid chromatographic (HPLC) method was developed for the determination of diltiazem (DTZ) and its major metabolite, deacetyldiltiazem (DAD), in rat plasma. DTZ, DAD and imipramine, the internal standard, were selectively fractionated from plasma on a $C_{18}$ reversedphase column $({\mu}-Bondapak,\;10\;{\mu}m\;silica,\;300{\times}3.9\;mm\;ID)$. The composition of the mobile phase was methanol: acetonitrile: 0.04 M ammonium bromide: triethylamine (40:24:36:0.06 in volume). The pH of the mobile phase of their method was lowered to 6.4. The eluents from the column were detected for DTZ and DAD using a UV detector at 237 nm. The recovery was >85% for DTZ and DAD, and average intra-day and inter-day coefficients of variation were <6% for DTZ and DAD at the concentration ranges of 20-1000 ng/ml. Detection limit of DTZ and DAD in plasma was 20 ng/ml with signal-to-noise ratio of 3. This method would be applicable to practical pharmacokinetic studies without detriment to the HPLC column.

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Seasonal Variation of Planktonic Foraminifera Assemblage in response to Seasonal Shift of Inter-Tropical Convergence Zone in the Northeastern Equatorial Pacific (적도수렴대의 위치변화에 따른 북동태평양 적도해역의 부유성 유공충 군집의 계절변동)

  • Lee, Yuri;Asahi, Hirofumi;Woo, Han Jun;Kim, Hyung Jeek;Lee, Seong-Joo;Khim, Boo-Keun
    • Ocean and Polar Research
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    • v.36 no.4
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    • pp.437-445
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    • 2014
  • A time-series sediment trap was operated at a water depth of 4950 m from July 2003 to May 2004 at KOMO station ($10^{\circ}30^{\prime}N$, $131^{\circ}20^{\prime}W$) in the northeastern equatorial Pacific, with the aim of understanding the temporal variation of planktonic foraminifera assemblages in response to the seasonal shift of Inter-Tropical Convergence Zone (ITCZ). A total of 22130 planktonic foraminifera specimens belonging to 30 species and 11 genera were identified, which shows a distinct seasonal variation with high values (125~288 specimens $m^{-2}day^{-1}$) in the winter to spring (December-May) and low values (16~23 specimens $m^{-2}day^{-1}$) in the fall (September-November). In addition, seasonal ecological differences of foraminifera assemblages are distinctly recognizable: omnivorous foraminifera occurred predominantly during the summer season, whereas herbivorous ones were dominant during the winter season. Such seasonal variations correspond to the seasonal shift of the ITCZ. Enhanced occurrence of herbivorous species during the winter-spring season seems a result of surface water mixing generated by the southward shift of the ITCZ. The increase in omnivorous species during the summer season may be due to the northward movement of the ITCZ caused by weakened wind speed, resulting in the intensification of water column stratification and nutrient-poor environment. A significant reduction of planktonic foraminifera specimens during the fall is attributed to heavy precipitation and reduction in light intensity.

Measurement and Interpretation of Time Variations of Particulate Matter Observed in the Busan Coastal Area in Korea

  • Kim, Cheol-Hee;Son, Hye-Young
    • Asian Journal of Atmospheric Environment
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    • v.5 no.2
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    • pp.105-112
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    • 2011
  • In order to investigate the effects of local and synoptic meteorological conditions on urban scale particulate air pollutants observed over the Busan coastal area, power spectrum analysis was applied to observed particulate matter with an aerodynamic diameter $\leq10\;{\mu}m$ ($PM_{10}$) for the period from 1 October, 1993 to 31 December, 2004. Fast Fourier Transform (FFT) analysis was used to obtain the hourly mean observed $PM_{10}$ concentrations to identify different periodicity scales of $PM_{10}$ concentrations. The results showed that, aside from the typical and well-known periodicities such as diurnal and annual variations caused by anthropogenic influences, three other significant power spectral density peaks were identified: 7-day, 21-day and 2.25-year periodicities. Cospectrum analysis indicated that the seven-day variations were closely related to the synoptic meteorological conditions such as weak wind speed, which are relevant to the stagnant high pressure system slowly passing through the Korean Peninsula. The intra-seasonal 21-day variation was negatively correlated with wind speed but was consistently positively correlated with relative humidity, which is related to aerosol formation that can be achieved as a result of the hygroscopic characteristics of aerosols. However, the quasibiennial 2.25-year variation was correlated with the frequency of Asian dust occurrence, the periodicities of which have been recorded inter-annually over the Korean Peninsula.

Development of Milk Progesterone Test(EIA) using Monoclonal Antibody and It's Application to Estrus-and Early Pregnancy Detection in Dairy Cattle (단일클론항체를 이용한 Milk Progesterone Test(EIA) 측정법의 개발과 이에 의한 소의 발정 및 임신조기진단의 정확도 향상에 관한 연구)

  • 김정우;홍승욱
    • Korean Journal of Animal Reproduction
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    • v.14 no.3
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    • pp.165-173
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    • 1990
  • A simple and sensitive microplate enzyme immunoassay(ELISA) was developed for progesterone, based on progesterone monoclonal antibody as anti-progesterone, horseradish peroxise(HRP) as enzyme-label and tetramethylbenzidine(TMB) as substrate. The assay has a sensitivity of 5pg-120pg/well and intra- and inter assay coefficients of variation for progesterone standard curve(0.1ng-3.2ng/ml) were ranged 4.4-10.6% and 5.-12.6%, respectively. They assay is performed in less than two hours and provide reliable values to differentiate among samples from day 0(A.I.), day 14 and day 19. The discriminatory levels for early pregnancy diagnosis are [>10ng(day 19) & decreasing rate <1.5 : pregnancy] and [ 7ng & decreasing rate 1.5 : non-pregnancy]. The accuracy of the pregnancy diagnosis for cows classified as positive(pregnancy) and negative(non-pregnancy) were 96% and 100%, respectively.

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Formulation of Topical Analgesic Preparation for a New Capsaicin Derivative Analgesic, DA-5018 (I) : Establishment of Skin Penetration Evaluation System and Formulation of Topical Cream (신규 Capsaicin 유도체 DA-5018을 함유한 외용진통제의 제제설계 I : 평가법 확립 및 외용크림제의 설계)

  • Cha, Bong-Jin;Lee, Eung-Doo;Kim, Won-Bae;Lee, Min-Hwa
    • Journal of Pharmaceutical Investigation
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    • v.27 no.1
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    • pp.65-69
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    • 1997
  • To formulate the topical analgesic preparation of a new capsaicin derivative, DA-5018, a skin penetration evaluation system was established and the effect of composition of formulation on skin penetration using this system was evaluated, The effect of massage on hairless mouse skin penetration and inter-day variation of this effect were investigated using test formulations(cream). In massage group, compared with non-massage group, absolute penetration amount of DA-5018 increased and this experimental system was found to be reproducible, The effects of pH of water phase, ratio of oil/water and the concentration of active ingredient in cream on skin penetration were investigated. The permeation of DA-5018 from the cream increased with increasing pH of water phase to 9. But at pH 10, the permeation of DA-5018 decreased, because of the physical instability of the cream. The permeation of DA-5018 from the cream increased with increasing the ratio of oil/water of the cream. The increase of the content of DA-5018 to 0.3% increased the permeation of DA-5018, but at high concentration(1.0%), the permeation of DA5018 decreased, due to the instability of the cream.

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Determination of Terbutaline Enantiomers in Human Urine by Capillary Electrophoresis Using $Hydroxypropyl-{\beta}-cyclodextrin$ as a Chiral Selector

  • Kim, Kyeong-Ho;Seo, Sang-Hun;Kim, Hyun-Ju;Jeun, Eun-Young;Kang, Jong-Seong;Mar, Woong-Chon;Youm, Jeong-Rok
    • Archives of Pharmacal Research
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    • v.26 no.2
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    • pp.120-123
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    • 2003
  • A method for the determination of terbutaline enantiomers in human urine by capillary elctrophoresis has been developed. Optimum resolution was achieved using 50 mM phosphate buffer, pH 2.5, containing 15 mM of hydroxypropyl-$\beta$-cyclodextrin as a chiral selector. Urine samples were prepared by solid-phase extraction with Sep-pak silica, followed by CE. The assay was linear between 2-250 ng/mL (R = 0.9998 for (S)-(+)-terbutaline and R = 0.9999 for (R)-(-)-terbutaline) and detection limit was 0.8 ng/mL. The intra-day variation ranged between 6.3 and 14.5% in relation to the measured concentration and the inter-day variation was 8.2-20.1%. It has been applied to the determination of (S)-(+)-terbutaline and (R)-(-)-terbutaline in urine from healthy volunteer dosed with racemic terbutaline sulfate.

Quantitation of abamectin by HPTLC and its pharmacokinetics after intramuscular injection in pigs (돼지에서 근육주사한 Abamectin에 대한 HPTLC 분석 및 약물동태학)

  • Park, Seung-chun;Yun, Hyo-in
    • Korean Journal of Veterinary Research
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    • v.40 no.1
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    • pp.35-41
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    • 2000
  • We established a new method to analyze abamectin using HPTLC (high performance thin layer chromatography) in order to obtain its pharmacokinetic profiles in pigs. Recovery of abamectin in pig serum after fluorescence derivatization was $80.01{\pm}3.82%$ at 0.1ppm and $83.67{\pm}3.63%$ at 10ppm, respectively. Detection reproducibility in terms of coefficient variation (c.v.) was 3.09% and 2.74% (intra-day), and 3.71% and 51.7%(inter-day), for 0.1 and 10ppm, respectively. Pharmacokinetics of abamectin was studied in five Yorkshire-Landrace mixed bred male pigs ($35.0{\pm}2.7kg$) administered intramuscularly 0.3mg/kg b.w. Pharmacokinetic profiles of abamectin in pigs were described by the 1-compartment open model with first-order absorption and first-order elimination. AUC (area under the curve) was $262.65{\pm}16.44ng{\cdot}day/ml$ and the biological elimination half-life ($t_{1/2},\;k_e$) was $5.28{\pm}0.84$ days, indicating somewhat high bioavailability and long half-life by the intramuscular route. We suggest intramucular injection of abamectin could be also used in place of the recommended route of its subcutaneous administration so far.

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Study on Simultaneous Analysis and Use of Preservatives in Mouthwashes (구강 청정제 중 보존제의 동시 분석법 확립과 사용실태에 관한 연구)

  • Jung, Sang-Mi;Moon, Tae-Jung;Kim, Jae-Dong;Lee, Gye-Won
    • Journal of Digital Convergence
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    • v.10 no.6
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    • pp.331-339
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    • 2012
  • The easy and simple simultaneous analytical method of preservatives (BA, SA, DHA, MP, EP, IPP, PP, IBP and BP) was studied by more easily changing from method used in food and drug using HPLC with scherzo SM-C18 column. All presevatives were seperated successfully in mobile phase of 50 mM ammonium formate : 0.1% phosphoric acid (50:50 v/v%) and 50 mM ammonium formate : acetonitrile (30 : 70). Retention time of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP was 7.74, 9.08, 12.57, 13.83, 21.62, 27.29, 28.20, 33.20 and 33.68 min, respectively. The calibration curves of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP were linear over the concentration range of 5~80 ${\mu}g/mL$ with correlation coefficient of above 0.999. The limit of detection (LOD) and limit of quantitation (LOQ) of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP were 0.52 and 1.58, 1.09 and 3.29, 1.00 and 3.03, 1.36 and 4.13, 1.26 and 3.83, 1.02 and 3.08, 1.11 and 3.37, 0.82 and 2.48, 0.85 and 2.59 ${\mu}g/mL$, respectively. The coefficients of variation for intra- and inter-day assay were 0.12~2.68 and 0.18~2.66%, respectively. The developed method showed good intra- and inter-day precision and accuracy. The preservatives used in mouthwashes were BA, MP and PP and were detected in 24 samples(86%) except for 4 samples and not showed significant difference in using dose of adult and children. In conclusion, the developed method can be useful for simultaneous analysis of preservatives in mouthwashes and these results suggest that could be applied to fundamental study and guideline on content of preservatives in mouthwashes.

Quantitative and Pattern Recognition Analyses for the Quality Evaluationof Herba Epimedii by HPLC

  • Nurul Islam, M.;Lee, Sang-Kyu;Jeong, Seo-Young;Kim, Dong-Hyun;Jin, Chang-Bae;Yoo, Hye-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.137-144
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    • 2009
  • In this study, quantitative and pattern recognition analyses for the quality evaluation of Herba Epimedii using HPLC was developed. For quantitative analysis, five major bioactive constituents, hyperin, epimedin A, epimedin B, epimedin C, and icariin were determined. Analysis was carried out on Capcell pak $C_{18}$ column ($250{\time}4.6$ mm, 5 ${\mu}m$) with a mobile phase of mixture of acetonitrile and 0.1% formic acid, using UV detection at 270 nm. The linear behavior was observed over the investigated concentration range (2-50 ${\mu}g/mL;\;r_2\;>$ 0.99) for all analytes. The intraand inter-day precisions were lower than 4.3% (as a relative standard deviation, RSD) and accuracies between 95.1% and 104.4%. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of one reference sample. The RSD of intra- and inter-day variation of relative retention time (RRT) and relative peak area (RPA) of the 12 selected common peaks were below 0.8% and 4.7%, respectively. The developed methods were applied to analysis of twenty Herba Epimedii extract samples. Contents of hyperin, epimedin A, epimedin B, epimedin C, and icariin were calculated to be 0$\sim$0.79, 0.69$\sim$1.91, 0.93$\sim$9.58, 0.65$\sim$3.05, and 2.43$\sim$11.8 mg/g dried plant. Principal component analysis (PCA) showed that most samples were clustered together with the reference samples but several apart from the main cluster in the PC score plot, indicating differences in overall chemical composition between two clusters. The present study suggests that quantitative determination of marker compounds combined with pattern-recognition method can provide a comprehensive approach for the quality assessment of herbal medicines.