• Journal of Pharmaceutical Investigation
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• 제9권4호
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• pp.1-7
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• 1979

The analytical method of phenobarbital and mephobarbital in the pharmaceutical preparation were investigated by the partition chromatographic method. The influence of 13 kinds of excipients and various kinds of ingredients such as 8 kinds of antipyretics and 5 kinds of antacids on the partition chromatographic analysis of phenobarbital and mephobarbital in the preparation were investigated. The results were not affected by materials with the exception of caffeine, aspirin and sulpyrin.

• Journal of Pharmaceutical Investigation
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• 제24권4호
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• pp.201-215
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• 1994

Recent development in the immunochemical technique has resulted in a new ultrasensitive analytical method known as liposome immunoassay (LIA). Liposome is a key element in performing liposome immunoassays, specifically designed to participate in immune reactions. A variety of markers can be encapsulated in liposomes and used as quantitative indicators of reactions. Liposome immunoassay based on agglutination, complement-mediated Iysis, cytolysin-mediated Iysis, detergent-mediated Iysis or destabilization of the liposomal membrane have been reviewed. The quantity of markers released from liposomes should be proportional to the concentration of the analytes. Therefore, liposomal agglutination and Iysis which are essential to liposomal Iysis are critically reviewed to provide a better understanding of liposome immunoassay. Based on the literature review of recent advances in liposome immunoassay for bioactive substances, this assay method may provide a convenient, specific and highly sensitive method for detecting and measuring trace amount of clinically relevant substances in the future.

• Journal of Applied Biological Chemistry
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• 제57권1호
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• pp.89-93
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• 2014

We aim to develop a simple method for simultaneous and quantitative determination of benzoic acid, caffeic acid and chlorogenic acid in seeds of Eriobotrya japonica. In addition, antibacterial effect of these three phenolic acids was examined. A basic method is performed on the high performance liquid chromatography system coupled to an UV-detector (230 nm) and reverse phase C-18 column ($4.6{\times}150mm$, $5{\mu}m$). Each phenolic acid was confirmed via liquid chromatography-mass spectrometry (MS)/MS system under the multiple-reaction monitoring with negative-ion electrospray ionization (ESI(-)) mode. It is demonstrated that the method was could be applied to samples for an analytical study of the phenolic acids. On the other hand, three phenolic acids in seeds of E. japonica exhibited antibacterial effect against several pathogenic bacteria. Of these, benzoic acid was found to have stronger antibacterial effect.

• 한국축산식품학회지
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• 제32권2호
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• pp.247-251
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• 2012

This study was carried out to investigate the applicability of the detection of central nervous system tissues (CNST) in beef by-products in retail market. Beef by-products including large intestine, brain, spinal cord, liver, lung, spleen and heart were purchased and tested for the presence of CNST using an ELISA method. The ELISA test was evaluated and showed a high correlation coefficient by a standard curve (R value = 0.999). Based on the analytical instruction, the positive indication of the CNST contamination of brain and spinal cord was detected above 0.1% but large intestine, liver, lung, spleen, and heart was negative. Result suggests that the ELISA method is applicable to a real meat system and may provide a method to ensure confidence for consumer against bovine spongiform encephalopathy (BSE).

• 한국정밀공학회지
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• 제12권9호
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• pp.52-58
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• 1995

Conventional measurement methods for non-destructive testing(NDT) in nuclear power plants and other industrial plants have been performed as the methods of contact with objects to be inspect, but those methods have been taken relatively much time to be inspected. Holographic interferometry which is a non-contact optical measurement method using a coherent light can overcome these demerit, and also has an advantage that the quantitative measurement of small deformation for large areas can be accomplished at a time with high precision. In this paper the comparisons of the experimental results form holographic interferometry with those from the finite element method(FEM) and the analytical solutions of the elastic equation are discussed.

• 분석과학
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• 제30권5호
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• pp.226-233
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• 2017

In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of $17{\beta}$-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of $17{\beta}$-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the $17{\beta}$-estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.

• 분석과학
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• 제37권2호
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• pp.98-113
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• 2024

The current investigation entails the characterization of five degradation products (DPs) formed under different stress conditions of loteprednol using liquid chromatography-tandem mass spectrometry (LC-MS/MS). In addition, this study developed a stable high-performance liquid chromatography (HPLC) method for evaluating loteprednol along with impurities. The method conditions were meticulously fine-tuned which involved the exploration of the appropriate solvent, pH, flow of the mobile phase, columns, and wavelength. The method conditions were carefully chosen to successfully resolve the impurities of loteprednol and were employed in subsequent validation procedures. The stability profile of loteprednol was exposed to stress degradation experiments conducted under five conditions, and DPs were structurally characterized by employing LC-MS/MS. The chromatographic resolution of loteprednol and its impurities along with DPs was effectively achieved using a Phenomenex Luna 250 mm C18 column using 0.1 % phosphoric acid, methanol, and acetonitrile in 45:25:30 (v/v) pumped isocratically at 0.8 mL/min with 243 nm wavelength. The method produces an accurate fit calibration curve in 50-300 ㎍/mL for loteprednol and LOQ (0.05 ㎍/mL) - 0.30 ㎍/mL for its impurities with acceptable precision, accuracy, and recovery. The stress-induced degradation study revealed the degradation of loteprednol under basic, acidic, and photolytic conditions, resulting in the formation of seven distinct DPs. The efficacy of this method was validated through LC-MS/MS, which allowed for the verification of the chemical structures of the newly generated DPs of loteprednol. This method was appropriate for assessing the impurities of loteprednol and can also be appropriate for structural and quantitative assessment of its degradation products.

• 한국산업보건학회지
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• 제17권1호
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• pp.21-30
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• 2007

To establish the Fourier-transform infra-red spectrophotometry (FTIR) direct-on-filter(DOF) technique as a useful analytical method for quartz in respirable dust samples, influence of the interference should be corrected. This study was designed to compare three methods of correction for cristobalite when quantifying the content of quartz, including the least square, the optimum choice and the spectral subtraction methods. Respirable dust, created in a dust chamber containing the standard material of quartz, cristobalite was collected using a cyclone equipped with a 25 mm, $0.8{\mu}m$ pore size DM filter as a collection medium. The quartz weights overestimated about 100% when mixed of cristobalite by measure using 799 cm-1 absorption peak of quartz. The quartz weights appeared over estimated by optimum choice, spectral subtraction and least square method in mixtures of 33% cristobalite were 90.3%, 60.1% and about 4.3%, respectively. The least square method have been adopted to correction methods of cristobalite and satisfactory results have been obtained. The results of this study suggest that, when correcting for effect of cristobalite on quantitative analysis of quartz in respirable dust by FTIR direct-on-filter method, the least square method produce the most unbiased results compared with those of other correction methods.

• 대한핵의학회지
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• 제3권1호
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• pp.19-32
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• 1969

Radioisotope renography was carried out in 564 cases consisting of 150 normal controls, 140 hypertensives, 102 hypertensive nephropathys, 62 chronic renal diseases, non-functioning kidneys. It was aimed to study which parameter of the renogram is most applicable to any definite disease of the kidney. The analytical methods adopted were; Tobe, Spencer, Krueger, Matchida and Takeuchi. In the non-functioning kidney groups, the hemograms and serum nitrogen series were also studied to evaluate the relationships between the renograms and renal anemia. The parameters were; time of maximum amplitude (Tmax), half-time of maximum amplitude ($T\frac{1}{2}$), Kac value calculated from these two parameters in Tobe's method, slopes of Band C phase, B/A and B/C values in Spencer's method, total concentration (T.C.), minute concentration (M.C.) and minute excretion (M.E.) in Krueger's method, Matchida's K value and Takeuchi's renal function Index (R.F.I.). Following were the results: 1. In general, marked differences in the patterns of the renogram were observed between the normal controls and nephropathys. In Tobe's method, each parameter showed statistically significant delay or decrease in patients with hypertensive nephropathys and chronic renal diseases. In Spencer's method, slopes of B and C phase and B/C, also showed the statistically significant decrease in patients with hypertension, hypertensive nephropathys and chronic renal diseases. In Krueger's method, M.C. and ME showed the statistically significant differences between the control and patients with hypertension, hypertensive nephropathys and chronic renal diseases, In Matchida's method, K value showed the statistically significant differences between the control and patients with hypertensive nephropathys and chronic renal diseases. 2. It appeared, therefore, that Tobe's $T\frac{1}{2}$, Kac value, Spencer's slopes of Band C phase, B/A, B/C values, Krueger's T.C., M.C., and M.E. values, Matchida's K value are useful for the differentiation of various renal diseases, however, qualitative analysis of the renogram with one or two parameters is not accurate. 3. In bilateral non-functioning kidney groups, a positive correlation between anemia and nitrogen retention was observed, although the quantitative assessment of the degree of non-functioning was impossible.

• 대한본초학회지
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• 제30권3호
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• pp.19-24
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• 2015

Objectives : HPL-1, a novel herbal medicine which is composed of five herbs such as Kalopanacis Cortex, Chaenomelis Fructus, Raphani Semen, Atractylodis Rhizoma and Pulvis Aconiti Tuberis Purificatum, was developed for treatment of osteoarthritis. This study is aimed to develop analytical method for consistent quality control of HPL-1 and validate chromatographic method. Methods : Chromatographic analysis was performed using ultra-high performance liquid chromatography - diode array detector (UHPLC-DAD) equipped with RP-amide column, column oven, and auto sampler. Marker compounds [protocatechuic acid, chlorogenic acid, liriodendrin, 3,5-dicaffeoylquinic acid, ${\beta}$-D-(3-O-sinapoyl)-fructofuranosyl-$\alpha$-D-(6-O-sinapoyl)glucopyranoside and benzoylmesaconine] were separated by step gradient elution of acetonitrile and 0.1% phosphoric acid/water. The method validation was evaluated by quantitative validation parameters of linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ) according to KFDA guideline.Results : An optimized method for six marker compounds in HPL-1 was established by UHPLC-DAD. The correlation coefficient (R²) with each calibration curve was greater than 0.99. The LOD and LOQ were within the range of 0.008-0.090 and $0.023-0.274{\mu}g/mL$, respectively. The relative standard deviation (RSD) of intra- and inter-day variability were less than 4.0%. The result of recovery test was range from 93.3-106.3% with RSD < 4.0%.Conclusions : These results suggest that the quantitative UHPLC method is precise, accurate, effective for quality evaluation of HPL-1. The method may also contribute to improve quality of crude drug preparations used for treatment of various diseases.