• Title/Summary/Keyword: lR Curve

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Electrospray Tandem Mass Spectrometry for the Quantification and Bioavailability Test of Gliquidone in Human Plasma (Electrospray Tandem Mass를 이용한 혈중 글리퀴돈의 정량법 개발 및 생체이용률시험)

  • Moon Chul-Jin;Lee Eun-Hee;Yang Song-Hyun;Moon Hae-Ran
    • YAKHAK HOEJI
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    • v.49 no.3
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    • pp.212-216
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    • 2005
  • A rapid, sensitive and selective electrospray tandem mass spectrometric (ESI-LC/MS/MS) method for the quantitation of gliquidone in human plasma was developed. A bioavailability study of gliquidone tablet (30 mg gliquidone, Boehringer Ingelheim Korea Co.) was performed using the validated ESI-LC/MS/MS method. The dose of 30 mg of gliquidone (1 tablet) was orally administered to 9 healthy Korean subjects. After administration, blood was taken at 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 5, 7, 9, 12, 24, and 33 hour. The validation data were as follows; the standard curve was linear ($r^2$=0.999) over the concentration range of $10\~1000 ng/ml$. The coefficient of variation for intra- and inter-day assay were $8.30\~18.86$, and $2.19\~12.92\%$, respectively. The lower limit of quantification for gliquidone was 10 ng/ml. The pharmacokinetic parameters obtained were as follows; $AUC_t$ was 3861.17$\pm$1328.61 ng-hr/ml, $C_{max}$ was 831.02$\pm$227.99 ng/ml, $T_{max}$ was $2.94{\pm}0.77 hr,\;K_e$, was 0.19$\pm$0.06 1/hr, and $t_{l/2}$ was 4.47$\pm$3.52 hr. Based on the validated analytical method and pharmacokinetic parameters, a standard guideline of the bioavailability test of gliquidone dosage forms was prepared successfully and could be used for the bioequivalence test of gliquidone preparation.

Free Volume in Polyers Note II。: Positron Annihilation lifetime Spectroscopy and Applications

  • G. Consolati;M. Pegoraro;L. Zanderighi
    • Korean Membrane Journal
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    • v.1 no.1
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    • pp.25-37
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    • 1999
  • positron annihilation Lifetime Spectroscopy has been extensively applied in recent years to investigate the free volume in polymers owing to the capability of the electron-positron bound system (positronium) to probe the typical size of sub-nanometric cavities among the macromolecular chains. In this paper we show recent results obtained through this technique in some amorphous polymeric mem-branes(olyurethanes. PUs and polytrimethilsylilpropine PTMSP) after a brief survey of the general features of the annihilation process as well as of the experimental apparatus. Lifetime of o-ps decay({{{{ tau _3}}}}) in PUs increases going from sub {{{{ TAU _g}}}} to over {{{{ TAU _g}}}} temperatures following a sigmoid curve. The coefficient of dilatation of the free volume fraction is shown to be the sum of two contributes due to the variation with T of the number of holes and of their mean volume. PAL spectrum of PTMSP freshly prepared shows four lifetime components: {{{{ tau _3}}}} and {{{{ tau _4}}}}: only are useful for free volume study. Two kinds of holes of different equivalent radius are reported ({{{{ gamma _s}}}} 4.60 nm and {{{{ gamma _1}}}} 0.754) The equivalent volume does not change in a range of 100 K. however the physical aging increases density and decreases oxygen permeability while {{{{ gamma _s}}}} goes down to 0.374 and r1 to 0.735 The number of holes obtained from the intensities{{{{ IOTA _3}}}} and {{{{ IOTA _4}}}} of PAL spectra decreases with aging 21.7% and 3.5% for large and small holes respectively.

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The estimated drying schedule of Fagaceae four species grown in Kangwon-Do (강원도산(江原道産) 참나무과(科) 4 수종(樹種)의 추정건조(推定乾燥)스케쥴)

  • Park, Jong-Su;Kim, Su-Chang
    • Journal of Forest and Environmental Science
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    • v.10 no.1
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    • pp.38-48
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    • 1994
  • This study was carried out to estimate drying schedule of Fagaceae four species grown in Kangwon-Do by oven-drying at $100^{\circ}C$ which aimed to elucidate the characteristics such as current moisture content, drying process, initial check, collapse and internal check during drying. The results were summerized as follows ; Current moisture content of each board showed a rapid drying curve with the hight initial moisture content of board and species with the high initial moisture content took long to do drying. Appearance of checks for Quercus variabilis were extremely severe and estimated schedule was $T_5-C_2$. The shrinkage rate of grain direction was in the order of tangential direction > radial direction > longitudial direction and the shrinkage rate of oven-drying at $100^{\circ}C$ was bigger than normal shrinkage rate.

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Determination of Uric Acid by Chemiluminescence Measurement Using Tris(2,2'-bipyridine)ruthenium(II)-Octylphenylpolyglycol Ether System

  • Kim, Young-Sang;Park, Jeung-Hee;Choi, Yoon-Seok
    • Bulletin of the Korean Chemical Society
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    • v.25 no.8
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    • pp.1177-1181
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    • 2004
  • The determination of uric acid in urine samples was studied by a chemiluminescence measurement using tris (2,2'-bipyridine)ruthenium(II)-octylphenylpolyglycolether [Ru$(bpy)_3^{2+}$ -OPE] system. The oxidized uric acid by Ce(IV) excited Ru$(bpy)_3^{2+}$ to emit a chemiluminescence in this system so that the intensity was stoichio-metrically dependent upon the concentration of uric acid. In a reaction cell, a luminescent reagent, oxidant, surfactant and sulfuric acid were flowed into and mixed with a taken sample. Experimental conditions were optimized to obtain the maximum intensity of chemiluminescence. Each reactant solution of more than the following concentration gave a good result: $2\;{\times}\;10^{?4}$ M Ru$(bpy)_3^{2+}$ , 0.01 M Ce(IV), 6% OPE, and 0.33 M $H_2SO_4$. Any interferences were not shown in this process by the investigation of concomitant constitutes such as albumin, creatine, lactic acid, glucose, urea, $Cl^?,\; Mg^{2+},\;Ca^{2+}$ and so on. The linearity of a calibration curve was good with r = 0.998, the relative standard deviation of the slope was 3.3% and the detection limit was 5.6ng/mL. The recoveries of 80 to 91% were obtained from the standard spiked samples. The values were little bit low, but this procedure could be considered to be reliable for the determination of trace uric acid in urine samples.

Development of a Simultaneous Analytical Method for Diquat, Paraquat and Chlormequat in Animal Products Using UPLC-MS/MS

  • Cho, Il Kyu;Rahman, Md. Musfiqur;Seol, Jae Ung;Noh, Hyun Ho;Jo, Hyeong-Wook;Moon, Joon-Kwan
    • Korean Journal of Environmental Agriculture
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    • v.39 no.4
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    • pp.368-374
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    • 2020
  • BACKGROUND: The residual analysis of polar pesticides has remained a challenge. It is even more difficult to simultaneously analyze multiple polar pesticides. Diquat, paraquat, and chlormequat are typical examples of highly polar pesticides. The existing methods for the analysis of diquat, paraquat and chlormequat are complex and time consuming. Therefore, a simple, quick and effective method was developed in the represent study for simultaneous analysis of diquat, paraquat and chlormequat in animal products, meat and fat using UPLC-MS/MS. METHODS AND RESULTS: Sample extraction was carried out using acidified acetonitrile and water and re- extracted with acidified acetonitrile and combine the extracts followed by centrifugation. The extract was then cleaned up with a HLB cartridge after reconstitution with acidic acetonitrile and water. The method was validated in quintuplicate at three different concentrations. The limits of detection (LOD) and quantification (LOQ) were 0.0015 and 0.005 mg/L, respectively. Matrix suppression effect was observed for all of the analytes. A seven point matrix matched calibration curve was constructed for each of the compound resulted excellent linearity with determination coefficients (R2) ≥ 0.991. Accuracy and precision of the method was calculated from the recovery and repeatability and ranged from 62.4 to 119.7% with relative standard deviation less than 18.8%. CONCLUSION: The recovery and repeatability of the developed method were in the acceptable range according to the Codex Alimentarius guideline. The developed method can be applied for the routine monitoring of diquat, paraquat, and chlormequat in animal products, meat and fat.

Protection provided by a commercial modified-live porcine reproductive and respiratory syndrome virus (PRRSV) 1 vaccine (PRRSV1-MLV) against a Japanese PRRSV2 field strain

  • Joel Miranda;Salvador Romero;Lidia de Lucas;Fumitoshi Saito;Mar Fenech;Ivan Diaz
    • Journal of Veterinary Science
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    • v.24 no.5
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    • pp.54.1-54.13
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    • 2023
  • Background: Porcine reproductive and respiratory syndrome virus (PRRSV) vaccines do not provide full cross-protection, mainly due to the virus genetic variability. Despite this, vaccines based on modified-live PRRSV (PRRSV-MLV) reduce the disease impact. Objectives: To assess the efficacy of two commercial vaccines-one based on PRRSV1 (PRRSV1-MLV) and another on PRRSV2 (PRRSV2-MLV)-against a Japanese PRRSV2 field strain. Methods: Two groups of three-week-old piglets were vaccinated (G1: PRRSV1-MLV; G2: PRRSV2-MLV) and two were kept as non-vaccinated (INF and CTRL). One month later, G1, G2, and INF were challenged with a PRRSV2 field strain. Results: After the challenge, clinical signs were only observed in INF. Moreover, the highest rectal temperatures and values for the area under the curve (AUC) were observed in INF. Regarding viral detection, both AUC and the proportion of positive samples in blood were higher in INF. In G1, viremic animals never reached 100%. At necropsy (21 d after the challenge), differences for titers among groups were only found in tonsils (G1 < G2 and INF). One animal (belonging to G1) was negative in all tissues. Regarding humoral responses, G1 and G2 seroconverted after vaccination, as detected in the corresponding enzyme-linked immunosorbent assay. Specific neutralizing antibodies (NA) against PRRSV1-MLV were already detected at 14 d after vaccination in G1, showing a significant booster after the challenge, while PRRSV2-MLV NA were detected in G2 at the end of the experiment. Conclusions: Despite genetic differences, PRRSV1-MLV has been demonstrated to confer partial protection against a Japanese PRRSV2 strain, at least as good as PRRSV2-MLV.

IPMN-LEARN: A linear support vector machine learning model for predicting low-grade intraductal papillary mucinous neoplasms

  • Yasmin Genevieve Hernandez-Barco;Dania Daye;Carlos F. Fernandez-del Castillo;Regina F. Parker;Brenna W. Casey;Andrew L. Warshaw;Cristina R. Ferrone;Keith D. Lillemoe;Motaz Qadan
    • Annals of Hepato-Biliary-Pancreatic Surgery
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    • v.27 no.2
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    • pp.195-200
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    • 2023
  • Backgrounds/Aims: We aimed to build a machine learning tool to help predict low-grade intraductal papillary mucinous neoplasms (IPMNs) in order to avoid unnecessary surgical resection. IPMNs are precursors to pancreatic cancer. Surgical resection remains the only recognized treatment for IPMNs yet carries some risks of morbidity and potential mortality. Existing clinical guidelines are imperfect in distinguishing low-risk cysts from high-risk cysts that warrant resection. Methods: We built a linear support vector machine (SVM) learning model using a prospectively maintained surgical database of patients with resected IPMNs. Input variables included 18 demographic, clinical, and imaging characteristics. The outcome variable was the presence of low-grade or high-grade IPMN based on post-operative pathology results. Data were divided into a training/validation set and a testing set at a ratio of 4:1. Receiver operating characteristics analysis was used to assess classification performance. Results: A total of 575 patients with resected IPMNs were identified. Of them, 53.4% had low-grade disease on final pathology. After classifier training and testing, a linear SVM-based model (IPMN-LEARN) was applied on the validation set. It achieved an accuracy of 77.4%, with a positive predictive value of 83%, a specificity of 72%, and a sensitivity of 83% in predicting low-grade disease in patients with IPMN. The model predicted low-grade lesions with an area under the curve of 0.82. Conclusions: A linear SVM learning model can identify low-grade IPMNs with good sensitivity and specificity. It may be used as a complement to existing guidelines to identify patients who could avoid unnecessary surgical resection.

Inhibitory Effects of Ethanolic Extracts from Aster glehni on Xanthine Oxidase and Content Determination of Bioactive Components Using HPLC-UV (섬쑥부쟁이 에탄올 추출물의 잔틴산화효소 저해 효능 및 HPLC-UV를 이용한 유효성분의 함량 분석)

  • Kang, Dong Hyeon;Han, Eun Hye;Jin, Changbae;Kim, Hyoung Ja
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.11
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    • pp.1610-1616
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    • 2016
  • This study aimed to establish an optimal extraction process and high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method for determination of 3,5-dicaffeoylquinic acid (3,5-DCQA) as a part of materials standardization for the development of a xanthine oxidase inhibitor as a health functional food. The quantitative determination method of 3,5-DCQA as a marker compound was optimized by HPLC analysis using a Luna RP-18 column, and the correlation coefficient for the calibration curve showed good linearity of more than 0.9999 using a gradient eluent of water (1% acetic acid) and methanol as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 320 nm. The HPLC-UV method was applied successfully to quantification of the marker compound (3,5-DCQA) in Aster glehni extracts after validation of the method with linearity, accuracy, and precision. Ethanolic extracts of A. glehni (AGEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 30, 50, 70, and 80% ethanol for 3, 4, 5, and 6 h, respectively. Among AGEs, 70% AGE at $70^{\circ}C$ showed the highest content of 3,5-DCQA of $52.59{\pm}3.45mg/100g$ A. glehni. Furthermore, AGEs were analyzed for their inhibitory activities on uric acid production by the xanthine/xanthine oxidase system. The 70% AGE at $70^{\circ}C$ showed the most potent inhibitory activity with $IC_{50}$ values of $77.01{\pm}3.13{\sim}89.96{\pm}3.08{\mu}g/mL$. The results suggest that standardization of 3,5-DCQA in AGEs using HPLC-UV analysis would be an acceptable method for the development of health functional foods.

Significance of Serum Ferritin in Multiple Trauma Patients with Acute Respiratory Distress Syndrome (다발성 외상 환자에서 발생되는 급성 호흡 곤란 증후군의 예측 인자로서 혈청 페리틴의 의의)

  • Ji, Yae-Sub;Kim, Nak-Hee;Jung, Ho-Geun;Ha, Dong-Yeup;Jung, Ki-Hoon
    • Journal of Trauma and Injury
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    • v.20 no.2
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    • pp.57-64
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    • 2007
  • Purpose: Clinically, acute respiratory distress syndrome (ARDS) occurs within 72 hours after acute exposure of risk factors. Because of its high fatality rate once ARDS progresses, early detection and management are essential to reduce the mortality rate. Accordingly, studies on early changes of ARDS were started, and serum ferritin, as well the as injury severity score (ISS), which has been addressed in previous studies, thought to be an early predictive indicator for ARDSMethods: From March 2003 to March 2005, we investigated 50 trauma patients who were admitted to the intensive care unit in Dongguk University Medical Center, Gyeongju. The patients were characterized according to age, sex, ISS, onset of ARDS, time onset of ARDS, serum ferritin level (posttraumatic $1^{st}\;&\;2^{nd}$ day), amount of transfused blood, and death. Abdominal computed topography was performed as an early diagnostic tool to evaluate the onset of ARDS according to its diagnostic criteria. The serum ferritin was measured by using a $VIDAS^{(R)}$ Ferritin (bioMeriux, Marcy-1' Etoile, France) kit with an enzyme-linked fluorescent assay method. For statistical analysis, Windows SPSS 13.0 and MedCalc were used to confirm the probability of obtaining a predictive measure from the receiver operating characteristics (ROC) curve. Results: The ISS varied from 14 to 66 (mean: 33.8) whereas the onset of ARDS could be predicted with the score above 30 (sensitivity: 90.0%, specificity: 60.0%, p<0.05). On the posttraumatic $1^{st}$ day, the serum ferritin levels were measured to be from 31 mg/dL to 1,200 mg/dL (mean: 456 mg/dL), and the onset of ARDS could be predicted when the value was over 340 mg/dL (sensitivity: 80.0%, specificity: 65.0%, p<0.05). On the posttraumatic $2^{nd}$ day, the serum ferritin levels were measured to be from 73 mg/dL to 1,200 mg/dL (mean: 404 mg/dL), and the onset of ARDS could be predicted when the value was over 627 mg/dL (sensitivity: 60.0%, specificity: 92.5%, p<0.05). The serum ferritin levels and the ISS were significantly higher on the posttraumatic $1^{st}$ and $2^{nd}$ day in the ARDS group, suggesting that they are suitable indices predicting the onset of ARDS, however relationship between the serum ferritin levels and the ISS was not statistically significant. Conclusion: In this study, we discovered increasing serum ferritin levels in multiple- trauma patients on the posttraumatic $1^{st}$ & $2^{nd}$ day and concluded that both the serum ferritin level and the ISS were good predictors of ARDS. Although they do not show statistically significant relationship to each other, they can be used as independent predictive measures for ARDS. Since ARDS causes high mortality, further studies, including the types of surgery and the methods of anesthesia on a large number of patients are essential to predict the chance of ARDS earlier and to reduce the incidence of death.

Determination of finasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 finasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.345-351
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    • 2011
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.