• 한국연초학회지
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• 제32권2호
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• pp.70-76
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• 2010

A simple and sensitive automatic amino acid analyzer method for the determination of free amino acids in tobacco was described. Sample preparation consisted of a single step of extraction with 0.1 mol HCl at ambient temperature in 60 min by sonication, followed by filtration of an aliquot. Automated amino acid analyzer was used to construct a post-column ninhydrin reaction unit to monitor amino acids separated by liquid chromatography using a series of eluting buffers. By optimization of sample preparation, separation of 19 amino acids was achieved. Limits of quantitation was 0.01 mg/g, coefficients of variation ranged from 0.5 % to 8.9 % and recoveries range from 85 % to 106 %. The method was applied to the analysis of amino acids contents of tobacco leaves in different varieties.

• Mass Spectrometry Letters
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• 제9권4호
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• pp.110-114
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• 2018

Since accumulation of chemicals in deciduous teeth can occur from the second trimester of fetal development to shedding, a deciduous tooth has been considered as an attractive biomatrix for estimating individual chemical exposures recently. Therefore, detection of organic chemicals from teeth has received an increasing attention in exposomics research. Most previous studies on organic chemical analysis of teeth not only focused on a few targeted chemicals but also ignored potential contaminants from an enamel surface or a dental pulp. Recently, our group started developing a multi-class organic analysis method for deciduous teeth and tried to find a proper incubation condition of tooth materials. Our results showed that incubation with methanolic HCl provided the best performance among tested.

• Applied Microscopy
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• 제50권
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• pp.15.1-15.6
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• 2020

Sample preparation including dehydration and drying of samples is the most intricate part of scanning electron microscopy. Most current sample preparation protocols use critical-point drying with liquid carbon dioxide. Very few studies have reported samples that were dried using chemical reagents. In this study, we used hexamethyldisilazane, a chemical drying reagent, to prepare plant samples. As glandular trichomes are among the most fragile and sensitive surface structures found on plants, we used Millingtonia hortensis leaf samples as our study materials because they contain abundant glandular trichomes. The results obtained using this new method are identical to those produced via critical-point drying.

• 약학회지
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• 제45권1호
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• pp.34-38
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• 2001

The Phellodendri Cortex of Phellodendron amurense (Rutaceae) is known to contain a number of isoquinoline alkaloid, and berberine, palmatine, jateorrhizine, phellodendrine and magnoflorine are the major constituents of protoberberine alkaloids. For the determination of protoberberine alkaloids from Phellodendri Cortex and berberine chloride from the preparation, the new spectrophotometric method was developed with a simple and selective sample clean-up using thiocyanatocobaltate[II] complex ion. Samples were extracted with 0.1 mM hydrochloric acid, potassium biphthalate reagent, thiocyanatocobaltate reagent and 1.2-dichloroethane for 60 min. The absorbance of protoberberine alkaloid complexes in 1.2-dichloroethane solution was measured at 625 nm. Calibration curve for berberine was linear over the concentration range of 0.05~0.30 mg/ml 1.2-dichloroethane. The method proved to be rapid, simple and reliable for the determination of protoberberine alkaloids from Phellodendri Cortex and berberine chloride from the preparation.

• 약학회지
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• 제33권4호
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• pp.241-245
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• 1989

A new application of high performance liquid chromatography for the determination of capsaicin and dihydrocapsaicin in cataplasma preparation was investigated. Optimum conditions for a good separation and detection were determined; 0.93 volt, acetonitrile: $H_3PO_4$ sol (pH 2.8), sample size; $7\;{\mu}l$. Recovery rates of capsaicin and dihydrocapsaicin from mixed artificial preparations were 99.9% and 98.4% respectively. Also reproducibility tests showed that the coefficient of variation was 1.59% for capsaicin and 1.14% for dihydrocapsaicin. There was no interference with cataplasma preparation containing thymol, dl-camphor and the commonly encountered excipients or additives such as gelatine, glycerine. This method was rapid, accurate and it gave higher sensitivity than other method.

• 한국연초학회지
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• 제27권1호
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• pp.107-114
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• 2005

The uncertainty of measurement in quantitative analysis of ammonia by continuous-flow analysis method was evaluated following internationally accepted guidelines. The sources of uncertainty associated with the analysis of ammonia were the weighing of sample, the preparation of extracting solution, the addition of extracting solution into the sample, the reproducibility of analysis and the determination of water content in tobacco, etc. In calculating uncertainties, Type A of uncertainty was evaluated by the statistical analysis of a series of observation, and Type B by the information based on supplier's catalogue and/or certificated of calibration. It was shown that the main source of uncertainty was caused by the volume measurement of 1 mL and 2 mL, the purity of ammonia reference material in the preparation of standard solution, the reproducibility of analysis and the determination of water content of tobacco. The uncertainty in the addition of extraction solution, the sample weighing, the volume measurement of 50 mL and 100 mL, and the calibration curve of standard solution contributed relatively little to the overall uncertainty. The expanded uncertainty of ammonia determination in burley tobacco at $95\%$ level of confidence was $0.00997\%$.

• Bulletin of the Korean Chemical Society
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• 제27권9호
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• pp.1315-1322
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• 2006

The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.

• Mass Spectrometry Letters
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• 제7권1호
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• pp.26-29
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• 2016

Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 μL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corticosteroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r² value was obtained in calibration standard range. Effective accuracy and precision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.

• Mass Spectrometry Letters
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• 제4권2호
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• pp.25-29
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• 2013

Proteomics for biomarker validation needs high throughput instrumentation to analyze huge set of clinical samples for quantitative and reproducible analysis at a minimum time without manual experimental errors. Sample preparation, a vital step in proteomics plays a major role in identification and quantification of proteins from biological samples. Tryptic digestion a major check point in sample preparation for mass spectrometry based proteomics needs to be more accurate with rapid processing time. The present study focuses on establishing a high throughput automated online system for proteolytic digestion and desalting of proteins from biological samples quantitatively and qualitatively in a reproducible manner. The present study compares online protein digestion and desalting of BSA with conventional off-line (in-solution) method and validated for real time sample for reproducibility. Proteins were identified using SEQUEST data base search engine and the data were quantified using IDEALQ software. The present study shows that the online system capable of handling high throughput samples in 96 well formats carries out protein digestion and peptide desalting efficiently in a reproducible and quantitative manner. Label free quantification showed clear increase of peptide quantities with increase in concentration with much linearity compared to off line method. Hence we would like to suggest that inclusion of this online system in proteomic pipeline will be effective in quantification of proteins in comparative proteomics were the quantification is really very crucial.

• Journal of Biosystems Engineering
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• 제29권4호
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• pp.323-328
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• 2004

A surface plasmon resonance (SPR) sensing system, which belonged to a family of thin film refractometry-based sensors, was fabricated to measure the alcohol contents in alcoholic beverages. In this study, a SPR owe was obtained by a photodiode array with 128 pixels and transformed into a refractive index which was calculated by means of the first moment of values below a baseline of 0.85. When the sensing system was applied to Soju, Cheonju, Igwaduju and Tacju highly linear relationships between the refractive index by SPR and the contents of alcohol were obtained. That is, the coefficients of determination in their linear models were 0.992, 0.933, 0.918 and 0.954, respectively. Meanwhile, the effect of sample preparations on the accuracy of measurement was analyzed. As for Soju and Tacju, the best calibration equations were obtained when no sample preparation was applied. The best calibration models for measurement of Cheonju and Igwaduju were obtained through the samples filtered by $C_{18}$ disks.