• Title/Summary/Keyword: internal standard method

Search Result 689, Processing Time 0.038 seconds

The Role of NMR in the Field of Quantitative Analysis

  • Lee, Sueg-Geun
    • Journal of the Korean Magnetic Resonance Society
    • /
    • v.20 no.3
    • /
    • pp.87-94
    • /
    • 2016
  • Although NMR technique has been using in many areas of chemistry, its merit on quantitative analysis seems not to acknowledge greatly because of the many inferior intrinsic aspects, particularly its sensitivity. Recently, new NMR techniques, high-field NMR, and demands for cutting edge techniques of analysis, however, seem to change the role of NMR spectroscopy in this field. This review shows the application of NMR development in quantitative analysis and will discuss the basic idea, limitations, and pitfalls. Then it will show you several successful applications applied in quantitative analysis and you will see how useful and accurate method it is.

Preliminary Research for Developing a Pattern Identification Tool for Idiopathic Pulmonary Fibrosis (특발성 폐섬유화증 변증 도구 개발을 위한 기초연구)

  • Hong, Sung-eun;Park, Ji-won;Shin, Jeong-won;Kil, Jung-eun;Kim, Kwan-il;Bu, Yung-min;Jung, Hee-jae;Lee, Beom-joon
    • The Journal of Internal Korean Medicine
    • /
    • v.43 no.3
    • /
    • pp.327-343
    • /
    • 2022
  • Objective: The purpose of this study was to develop a standard tool for identifying idiopathic pulmonary fibrosis patterns. Methods: Textbooks, published literature, and references with comments on patterns were reviewed. Using the Delphi method, we determined pattern identification based on the advice of a committee consisting of 11 Korean respiratory internal medicine professors. Results: Four pattern identifications were selected by the Delphi method: qi difficiency (氣虛), yin difficiency (陰虛), phlegm dampness (痰飮), blood stasis (瘀血). The tool was developed in a question-and-answer format containing 38 questions. Conclusions: An IPF pattern identification tool that can analyze IPF patterns for standardized diagnostics was developed with the consent of experts. Further research is needed on its reliability.

Standard Error of Empirical Bayes Estimate in NONMEM$^{(R)}$ VI

  • Kang, Dong-Woo;Bae, Kyun-Seop;Houk, Brett E.;Savic, Radojka M.;Karlsson, Mats O.
    • The Korean Journal of Physiology and Pharmacology
    • /
    • v.16 no.2
    • /
    • pp.97-106
    • /
    • 2012
  • The pharmacokinetics/pharmacodynamics analysis software NONMEM$^{(R)}$ output provides model parameter estimates and associated standard errors. However, the standard error of empirical Bayes estimates of inter-subject variability is not available. A simple and direct method for estimating standard error of the empirical Bayes estimates of inter-subject variability using the NONMEM$^{(R)}$ VI internal matrix POSTV is developed and applied to several pharmacokinetic models using intensively or sparsely sampled data for demonstration and to evaluate performance. The computed standard error is in general similar to the results from other post-processing methods and the degree of difference, if any, depends on the employed estimation options.

Study on Establishing the Indoor Noise Standard in Military Airport (군용 비행장 내 실내소음 기준 설정에 관한 연구)

  • Ko, JoonHee;Choi, NamSu;Baek, Chol;Cho, ManHee
    • Proceedings of the Korean Society for Noise and Vibration Engineering Conference
    • /
    • 2014.10a
    • /
    • pp.701-703
    • /
    • 2014
  • The intense noise generated by military aircraft hans a significant impact on ground crews and their families on airbase. For minimizing the impact of the aircraft noise on the airport, appropriate indoor noise standard is required. This paper studied to establish the indoor noise standard on the military airport. The aircraft noise was measured and analyzed the frequence characteristics. the remodeling of office for the noise mitigation was enforced to verify the appropriate internal noise standard and to select the method of reinforcement. The noise standard was classified three categories according to the dwelling, office and usage of building with flight train facilities and banishment in military airfield.

  • PDF

Development of Highly Sensitive Analytical Method for Evaluation of Evening Primrose Oil's Enhancing Effect in Prostaglandin E1(OP 1206) Biosynthesis

  • Lee, Sung-Hoon
    • Journal of People, Plants, and Environment
    • /
    • v.21 no.6
    • /
    • pp.485-492
    • /
    • 2018
  • This study aimed to develop and validate highly sensitive determination method of a prostaglandin ($PGE_1$, OP 1206) in human plasma by LC-MS/MS using column switching. Plasma stored at $-30^{\circ}C$ and treated with methanol effectively inhibited interferences synthesized post-sampling. Samples were added with internal standard and were separated by reversed-phase HPLC with a cycle time of 30min. The method was selective for OP 1206 and the regression models, based on internal standard, were linear across the concentration range 0.5-50 pg/mL with the limit of quantification of 0.5 pg/mL (limit of quantitation, LOQ) for OP 1206. The calibration curve of OP 1206 standards spiked in five individual plasma samples was linear ($r^2=0.9999$). Accuracy and precision at the concentrations of 0.5, 1.5, 5.0 and 40 pg/mL, and at the lower LOQ of 0.5 pg/mL were excellent at 20%. OP120 < 6 was stable in plasma samples for at least 24 hours at room temperature, 24 hours frozen at $-70^{\circ}C$, 24 hours in an auto sampler at $6^{\circ}C$, and for two freeze/unfreezing cycles. The validated determination method successfully quantified the concentrations of OP 1206 in plasma samples from simulated administrating a single $5{\mu}g$ OP 1206 formulation. Thus, this novel LC-MS/MS technique for drug separation, detection and quantitation is expected to become the standard highly-sensitive detection method in bioanalysis and to be applied to many low dose pharmaceutical products.

Advanced Method for Determination of Omeprazole in Plasma by HPLC

  • Kang, Won-Ku;Kim, Dong-Sup;Kwon, Dwang-Il
    • Archives of Pharmacal Research
    • /
    • v.22 no.1
    • /
    • pp.86-88
    • /
    • 1999
  • An advance d and sensitive high-performance liquid chromatographic (HPLC) method for determination of omeparzole in human plasma has been developed. After omeprazole was extracted from plasma with diethylether, the organic phase was transferred to another tube and trapped back with 0.1 N NaOH solution. The alkaline aqueous layer was injected into a reversed-phase C8 column. Lansoprazole was used as an internal standard. The mobile phase consisted of 30% of acetonitrile and 70% of 0.2 M $ KH_{2}PO_{4}$, pH 7.0. Recoveries of the analytes and internal standard were >75.48%. The coefficients of variation of intra- and inter-day assay were <5.78 and 4.59% for plasma samples. The detection limit in plasma was 2 ng/ml. The clinical applicability of this assay method was evaluated by determining plasma concentration-time courses of the respective analytes in 24 healthy volunteers after oral administration 40 mg of omeprazole. The present assay is considered to be simple, accurate, economical and suitable for the study of the kinetic disposition of omeprazole in the body.

  • PDF

Portable Piezoelectric Film-based Glove Sensor System for Detecting Internal Defects of Watermelon (수박 내부결함판정을 위한 휴대형 압전형 장갑 센서시스템)

  • Choi, Dong-Soo;Lee, Young-Hee;Choi, Seung-Ryul;Kim, Hak-Jin;Park, Jong-Min;Kato, Koro
    • Journal of Biosystems Engineering
    • /
    • v.33 no.1
    • /
    • pp.30-37
    • /
    • 2008
  • Dynamic excitation and response analysis is an acceptable method to determine some of physical properties of agricultural product for quality evaluation. There is a difference in the internal viscoelasticity between sound and defective fruits due to the difference of geometric structures, thereby showing different vibration characteristics. This study was carried out to develop a portable piezoelectric film-based glove sensor system that can separate internally damaged watermelons from sound ones using an acoustic impulse response technique. Two piezoelectric sensors based on polyvinylidene fluoride (PVDF) films to measure an impact force and vibration response were separately mounted on each glove. Various signal parameters including number of peaks, energy ratio, standard deviation of peak to peak distance, zero-crossing rate, and integral value of peaks were examined to develop a regression-estimated model. When using SMLR (Stepwise Multiple Linear Regression) analysis in SAS, three parameters, i.e., zeros value, number of peaks, and standard deviation of peaks were selected as usable factors with a coefficient of determination ($r^2$) of 0.92 and a standard error of calibration (SEC) of 0.15. In the validation tests using twenty watermelon samples (sound 9, defective 11), the developed model provided good capability showing a classification accuracy of 95%.

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

  • Park, Seok;Lee, Ye-Rie;Kim, Ho-Hyun;Lee, Hee-Joo;Kim, Yoon-Gyoon;Youm, Jeong-Rok;Han, Sang-Beom
    • Journal of Pharmaceutical Investigation
    • /
    • v.34 no.6
    • /
    • pp.513-519
    • /
    • 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.

Sacroiliac Joint/Sacrum Uptake Ratio Measured by Quantitative Sacroiliac Joint Scintigraphy (골(骨)스캔을 이용(利用)한 천장관절(薦腸關節)/천골섭취비(薦骨攝取比)의 정량적(定量的) 측정(測定))

  • Lee, Young-Yiul;Park, Seon-Yang;Lee, Myung-Chul;Choi, Sung-Jae;Cho, Bo-Youn;Choe, Kang-Won;Koh, Chang-Soon
    • The Korean Journal of Nuclear Medicine
    • /
    • v.16 no.2
    • /
    • pp.63-70
    • /
    • 1982
  • To evaluate the diagnostic usefulness and significance of quantitative sacroiliac joint scintigraphy in the assessment of sacroiliitis, we measured Sacroiliac Joint/Sacrum Uptake Ratio(SIS Ratio) by region of interest(ROI) method using $^{99m}Tc-methylene$ diphosphonate. The observed results were as follows: 1. Using ROI method, the SIS ratios for the control group of 65 persons were $1.05{\pm}0.08$(left) and $1.06{\pm}0.07$(right) which were narrower in range than those of slice method $(mean{\pm}S.D.)$. 2. The effects of age, gender and laterality on SIS ratio were not significant. 3. In left side, one of 6 patients with rheumatoid arthritis had SIS ratio in excess of 2 standard deviation of normal control group, and remainder had SIS ratios within normal limit. In right side, 3 patients had SIS ratios in excess of 2 standard deviation of normal control group, and remainder, within normal limit. 4. In both sacroiliac joint, 2 of 3 patients having sacroiliitis clinically with Reiter's syndrome whose pelvis A-P X-ray findings showed normal had high SIS ratios (left/right; 1.31/1.69, 1.90/1.80), but SIS ratio of one patient who had no evidence of sacroiliitis clinically was within normal limit. 5. In 6 patients with ankylosing spondylitis in both sacroiliac joints, 4 whose pelvis A-P Xray findings showed severe sclerotic change of sacroiliac joints had SIS ratio within normal limit or below that of normal control group, and SIS ratios of 2 patients whose pelvis A-P X-ray findings showed were increased. 6. 4 of 5 patients with low back pain of which cause could not be evaluated clinically and radiologically had SIS ratios in excess of that of normal control group. It would be concluded that quantitative sacroiliac joint scintigraphy is useful and sensitive screening method in the diagnosis as well as in the assessment clinical activity of sacroiliitis.

  • PDF

Selective Extraction and Quantification of Glutathione using Maleimide-Presenting Gold Nanoparticles

  • Oh, Hongseok;Lee, Jeongwook;Yeo, Woon-Seok
    • Bulletin of the Korean Chemical Society
    • /
    • v.35 no.10
    • /
    • pp.3047-3051
    • /
    • 2014
  • In this paper, we describe a new method for the selective extraction and quantification of glutathione (GSH) using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) and maleimide-presenting gold nanoparticles (Mal-AuNPs). Our strategy utilizes the Michael addition to selectively extract GSH, from chosen samples, onto the maleimide of Mal-AuNPs. After the extraction step, the GSH bound to the AuNPs was analyzed by MALDI-TOF MS in the presence of an internal standard which was prepared by reacting Mal-AuNPs with isotope-labeled GSH ($GSH^*$). The $GSH^*$ has the same structure as GSH but a higher molecular weight, and therefore, enables absolute quantification of GSH by comparing the mass signal intensities of the GSH- and $GSH^*$-conjugated alkanethiols. Our strategy was verified by analyzing GSH-spiked fetal bovine serum and NIH 3T3 cells.