• Analytical Science and Technology
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• v.26 no.1
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• pp.19-26
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• 2013

Gibberllic acid ($GA_3$) is one of gibberellins (GAs) that are a class of plant growth hormones that exert profound and diverse effects on plant growth and development. $GA_3$ is essentially non-UV absorbing and is difficult to assay by UV-detector. For effective extraction of gibberellic acid from fruits by using liquid-liquid extraction, optimized pH and extraction solvent were established. The selective and sensitive derivative of $GA_3$ for HPLC/UV-vis was derivatized using phenacyl bromide, and the experimental factors, including reaction time, reaction temperature and amount of derivatizing reagent and base were investigated for the effective synthesis. The derivatized $GA_3$ with phenacyl bromide was effectively analyzed by HPLC/UV-vis. The structure of derivatized $GA_3$ was confirmed by HPLC/ESI-MS. For apple, LOD and LOQ were 0.008 mg/kg and 0.027 mg/kg, respectively. For pear, LOD and LOQ were 0.003 mg/kg, 0.012 mg/kg, respectively. The established method can be applied to more effective analysis of $GA_3$ from plant and food.

• Analytical Science and Technology
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• v.31 no.2
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• pp.71-77
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• 2018

Detection of bloodstains is a very important process in scientific investigations, and luminol is often used for the detection of bloodstains that are not visible. Recently, new preparation methods of blood detection reagents based on luminol (BloodFlareA, B) were developed and reported to have higher active persistence and to be more economical than conventional blood detection reagent, BlueStar forensic. In this paper, we tested the specificity and effect of the BloodFlares (A and B) on DNA and compared them with those of BlueStar forensic. False positive results for the BloodFlares were not observed in semen, saliva, vaginal fluids, urine, sweat, and nasal discharge, but were observed in $CuSO_4$, $FeSO_4$, and bleach solutions, and the observed patterns were similar to those of BlueStar forensic. The effect on DNA was determined by analyzing the DNA yield, degradation index, and DNA profiling. Based on these results, we concluded that the BloodFlares based on luminol do not affect DNA stability and are applicable in forensics.

• Analytical Science and Technology
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• v.28 no.1
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• pp.26-32
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• 2015

The consistency and homogeneity of repetitive printing of artificial fingerprint were evaluated using a visual minutiae comparison method and an Automated Fingerprint Identification System (AFIS). The standard latent fingerprint pattern was prepared by the printing of a master digital fingerprint pattern with an inkjet printer cartridge case filled with artificial sweat. The master digital fingerprint pattern was prepared with a scanning of an inked fingerprint pattern of a living subject. The intensities of the master digital fingerprint pattern were adjusted by changing the 'output level' values of the Adobe Photoshop CS 5 software. Number of standard latent fingerprint patterns were printed and then developed with conventional latent fingerprint developing methods; ninhydrin treatment method and 1,2-indandion(1,2-IND)/$ZnCl_2$ treatment method. The ridge details of the latent fingerprint patterns developed with the reagents were visually compared with the inked fingerprint pattern and could confirm that the minutiae of both patterns are visually identical. The ridge detail of the inked fingerprint and reagent developed standard latent fingerprint patterns were compared with an AFIS. The average number of minutiae searched by the AFIS was $52.4{\pm}2.4$ (range = 48~56) for 50 ninhydrin developed latent fingerprint patterns, and $50.2{\pm}1.9$ (range = 47~53) for 50 1,2-IND/$ZnCl_2$ developed latent fingerprint patterns. These low standard deviation values over 50 repetitive printing demonstrated that the 50 standard latent patterns were printed with consistent and homogeneous manner.

• Analytical Science and Technology
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• v.23 no.6
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• pp.511-517
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• 2010

Dissolution procedure of vanadium pentoxide, which is widely used as a catalyst for production of sulfuric acid or an oxide reaction of the numerous organic compounds, was investigated. Reagent of vanadium pentoxide was completely dissolved in aqua regia-$H_2O_2$-HF solution, but plate type of vanadium pentoxide sample was not clearly dissolved with mixed acids. Thus, in order to establish the dissolution procedure for plate type of vanadium pentoxide, the solubility of vanadium pentoxide was investigated through comparison of acid treatment-fusion and microwave digestion methods. The optimized acid for dissolution of vanadium compound was found to be mixing acids of aqua regia, $H_2O_2$ and HF. Acid-fusion and microwave digestion methods have a similar property in the solubility of vanadium compound, but the latter was more quick and convenient procedure. The content of vanadium pentoxide was found to be $97.9{\pm}0.9%$ using an inductively coupled plasma atomic emission spectrometer after dissolution of a sample with the microwave digestion system.

• Journal of the Korean Chemical Society
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• v.53 no.6
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• pp.717-726
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• 2009

Multivariate models were developed for the simultaneous spectrophotometric determination of copper (II), nickel (II) and zinc (II) in water with 1-(2-thiazolylazo)-2-naphthol as chromogenic reagent in the presence of Triton X-100. To overcome the drawback of spectral interferences, principal component regression (PCR) and partial least square (PLS) multivariate calibration approaches were applied. Performances were validated with several test sets, and their results were then compared. In general, no significant difference in analytical performance between PLS and PCR models. The root mean square error of prediction (RMSEP) using three components for $Cu^{2+}$, $Ni^{2+}$ and $Zn^{2+}$ were 0.018, 0.010, 0.011 ppm, respectively. Figures of merit such as sensitivity, analytical sensitivity, limit of detection (LOD) were also estimated. High reliability was achieved when the proposed procedure was applied to simultaneous determination of $Cu^{2+}$, $Ni^{2+}$ and $Zn^{2+}$ in synthetic mixture and tap water.

• Analytical Science and Technology
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• v.17 no.6
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• pp.481-488
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• 2004

Solvent extraction of Ni(II) into a chloroform by using salen[N,N'-Bis (salicylidene)-ethylenediamine] as a ligand has been studied. Salen was synthesized from ethylenediamine and salicylaldehyde by simple condensation reaction in an ethanol. Salen formed a 1 : 1 complex with Ni(II) and its extraction constant was $10^{5.12}$. For the determination of Ni(II) in sea water samples, some experimental conditions such as pH of solution, amount of salen, acid type and concentration for back extraction, extraction time, and influence of foreign ions were optimized by using a synthetic sea water. The sea water of which the composition was similar to a natural sea water was synthesized in this laboratory. Trace Ni(II) was extracted into the chloroform in the weak basic solution above pH 8. And the nickel could be quantitatively extracted with the concentration of salen higher than $1.2{\times}10^{-4}mol/L$. This concentration was more than 180 times of Ni(II) in the solution with a mole ratio. Real samples of Korean coastal sea water were analyzed under optimized conditions. Even though Ni(II) was not detected in these samples. Recoveries more than 98% were obtained in the samples which 40 ng/mL of Ni(II) was spiked. And detection limit of proposed method was 1.3 ng/mL. From these results, it could be known that salen of this type would be applied for the determination of trace metals as an organic chelating reagent.

• Analytical Science and Technology
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• v.17 no.4
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• pp.322-336
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• 2004

The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride (TFAA), pentafluoroacetic anhydride (PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry (GC/MS) technique use negative ion chemical ionization (NCI), positive ion chemical ionization (PCI) and electron impact (EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at $50^{\circ}C$ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.

• Analytical Science and Technology
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• v.34 no.6
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• pp.251-258
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• 2021

Knives are most frequently used as weapons in violent crimes. Criminals leave behind knife sheaths made of paper and tape at crime scenes. It is difficult to develop fingerprints using tape attached to a porous surface, resulting in the need to explore effective techniques for identifying fingerprints as well as the distribution of fingerprints on each surface, when evidence such as paper knife sheaths are found. In this study, 50 knife sheaths were prepared. The cyanoacrylate fuming (CA fuming) method was applied to develop fingerprints on the non-adhesive side of the tape, and a dual-purpose 1,2-indanedione/Zn (1,2-IND/Zn) reagent was used to separate tape from paper while simultaneously developing fingerprints on the paper. The fingerprints on the adhesive side of the tape were developed using Wet Powder Black^®. Using the R statistical analysis program (The R Foundation for Statistical Computing), we used a heat map to indicate the location of fingerprints developed from each surface. More fingerprints were detected at the ends than in the center of the adhesive side of the tape, and although the non-adhesive sides of tape and paper did not present clear distribution patterns, many fingerprints were developed that had sufficient clarity for personal identification. The results of this study may be applicable for processing evidence when paper sheaths are found at crime scenes.

• Clean Technology
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• v.28 no.4
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• pp.323-330
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• 2022

Microfluidic paper-based analytical devices (μPADs) have recently been in the spotlight for their applicability in point-of-care diagnostics and environmental material detection. This study presents a double-sided printing method for fabricating 3D-μPADs, providing simple and cost effective metal ion detection. The design of the 3D-μPAD was made into an acryl stamp by laser cutting and then coating it with a thin layer of PDMS using the spin-coating method. This fabricated stamp was used to form the 3D structure of the hydrophobic barrier through a double-sided contact printing method. The fabrication of the 3D hydrophobic barrier within a single sheet was optimized by controlling the spin-coating rate, reagent ratio and contacting time. The optimal conditions were found by analyzing the area change of the PDMS hydrophobic barrier and hydrophilic channel using ink with chromatography paper. Using the fabricated 3D-μPAD under optimized conditions, Ni²⁺, Cu²⁺, Hg²⁺, and pH were detected at different concentrations and displayed with color intensity in grayscale for quantitative analysis using ImageJ. This study demonstrated that a 3D-μPAD biosensor can be applied to detect metal ions without special analysis equipment. This 3D-μPAD provides a highly portable and rapid on-site monitoring platform for detecting multiple heavy metal ions with extremely high repeatability, which is useful for resource-limited areas and developing countries.

• Analytical Science and Technology
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• v.20 no.4
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• pp.323-330
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• 2007

A simple and rapid HPLC method with fluorescence detection(FLD) for quantitation of penciclovir in human plasma using a monolithic column was developed and validated. Penciclovir and ganciclovir(internal standard, I.S.) were separated on a Chromolith column RP-18e ($4.6{\times}100mm$) with a mobile phase consisting of a mixture of (A) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (3/97, pH 2.5) and (B) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (50/50, pH 2.5) at a flow gradient of $1.6{\sim}4.0mL/min$. The retention times of penciclovir and internal standard were less than 4.0 min. Calibration curve was linear ($R^2=0.9994$) over a concentration range of $0.1{\sim}5{\mu}g/mL$. Intra-day precision, accuracy and inter-day precision were 1.36~8.55 %, 92.8~100.0 % and 0.93~5.62 %, respectively with a limit of quantitation at $0.1{\mu}g/mL$. The present HPLC-FLD method is sensitive, precise and accurate. The method described herein has been successfully used for the bioequivalence study of a famciclovir formulation product after oral administration to healthy Korean volunteers.