Simultaneous determination of illegal galactagogue adulterants in supplement diets by LC-MS/MS

Lee, Ji Hyun,Cho, So-Hyun,Park, Han Na,Park, Hyoung Joon,Kim, Nam Sook,Park, Sung Kwan,Kang, Hoil The Korean Society of Analytical Science 2018 분석과학 Vol.31 No.4

Recently, for successful lactation, many breastfeeding mothers seek various products, including herbal medicine, dietary supplements, and prescribed medicines, to improve milk production. As demand for galactogogues grows, it is highly possible that pharmaceutical galactogogues may be adulterated with illegal products to maximize their efficacy. For continuous control and supervision of illegal products, we developed and validated a simple and sensitive LC-MS/MS method capable of simultaneously determining five galactogogues. Chromatographic separation was conducted using an Agilent Poroshell $120SB-C_{18}$ column with a mobile phase consisting of 20 mM ammonium formate (pH 5.4) and 100 % acetonitrile. The total run time was 13 min per analyte. The proposed method was performed according to the guidelines of the International Conference of Harmonization and it produced reliable results. This method showed high sensitivity and specificity, with a limit of detection (LOD) and limit of quantitation (LOQ) of 0.01-0.82 ng/mL and 0.02-2.45 ng/mL, respectively, for the solid- and liquid-type samples. Specificity was evaluated by analyzing matrix-blank samples spiked with the target compounds at LOQ levels, which provided a good separation of all peaks without interference. Additionally, the repeatability and intermediate precision were typically <15 %, whereas the recovery was 80-120 % of the values obtained using blank samples. Thus, we concluded that this method could be used for the identification and quantification of galactogogues in food or herbal products.

Study on the spectroscopic reconstruction of explosive-contaminated overlapping fingerprints using the laser-induced plasma emissions

Yang, Jun-Ho,Yoh, Jai-Ick The Korean Society of Analytical Science 2020 분석과학 Vol.33 No.2

Reconstruction and separation of explosive-contaminated overlapping fingerprints constitutes an analytical challenge of high significance in forensic sciences. Laser-induced breakdown spectroscopy (LIBS) allows real-time chemical mapping by detecting the light emissions from laser-induced plasma and can offer powerful means of fingerprint classification based on the chemical components of the sample. During recent years LIBS has been studied one of the spectroscopic techniques with larger capability for forensic sciences. However, despite of the great sensitivity, LIBS suffers from a limited detection due to difficulties in reconstruction of overlapping fingerprints. Here, the authors propose a simple, yet effective, method of using chemical mapping to separate and reconstruct the explosive-contaminated, overlapping fingerprints. A Q-switched Nd:YAG laser system (1064 nm), which allows the laser beam diameter and the area of the ablated crater to be controlled, was used to analyze the chemical compositions of eight samples of explosive-contaminated fingerprints (featuring two sample explosive and four individuals) via the LIBS. Then, the chemical validations were further performed by applying the Raman spectroscopy. The results were subjected to principal component and partial least-squares multivariate analyses, and showed the classification of contaminated fingerprints at higher than 91% accuracy. Robustness and sensitivity tests indicate that the novel method used here is effective for separating and reconstructing the overlapping fingerprints with explosive trace.

Analytical characterization of O₃ samples prepared for investigation of tropospheric heterogeneous reactions

Kim, Mihyeon,Park, Jong-Ho The Korean Society of Analytical Sciences 2022 분석과학 Vol.35 No.5

In this study, ozone (O₃) samples were prepared for investigating the heterogeneous reactions between O₃ and tropospheric aerosols and were characterized by spectroscopic methods. O₃ generated from an ozone generator was purified by selective adsorption on refrigerated silica gel, followed by transfer to a sample bulb. The amount of UV light (λ = 256 nm) absorbed by O₃ was measured as a function of time at two different temperatures (room temperature and 50 ℃) and under different irradiation conditions. A correlation plot of 1/[O₃] versus time showed that O₃ decomposition follows the 2^nd order reaction rate under a steady-state approximation. The initial concentration of O₃, observed rate constants (k_obs), and the half-life of O₃ in the sample stored at room temperature were determined to be 2.74 [±0.14] × 10¹⁶ molecules·cm^-3, 4.47 [±0.64] × 10^-23 molecules^-1·cm³·s^-1, and 9.5 [±1.4] days, respectively. The evaluation of O₃ stability under various conditions indicated that special care should be taken to prevent the exposure of the O₃ samples to hightemperature environment and/or UV radiation. This study established a protocol for the preparation of highly purified O₃ samples and confirmed that the O₃ samples can be stored for a day after preparation for further experiments.

Silver elimination effect by sulfuric acid for Ag pre-treated activated carbon

Oh, Won-Chun The Korean Society of Analytical Sciences 2006 분석과학 Vol.19 No.2

In this study, silver pre-treated activated carbons are transformed using sulfuric acid. From the results of adsorption, each isotherm shows a distinct knee band, which is characteristic of microporous adsorbents with capillary condensation in micropores. In order to reveal the causes of the differences in adsorption capacity and specific surface area after the samples were washed with various strengths of sulfuric acid, surface morphology and external pore structure were investigated by SEM. X-ray diffraction patterns indicated that Ag-activated carbons show better performance for silver and silver compounds removal by post-treatment with acid. The FT-IR spectra of silver-activated carbon samples show that the acid post-treatment was consequently associated with the removal of silver with an increased surface functional group containing oxygen of the activated carbon. The type and quality of oxygen groups are determined on the method proposed by Boehm. For the chemical composition microanalysis of silver-activated carbons transformed by post-treatment with sulfuric acid, samples were analyzed by EDX.

A study of characteristics of cumulative deposition of fallout Pu in environmental samples

Lee, Myung Ho,Song, Byoung Chul,Jee, Kwang Yong,Park, Yeong Jae,Kim, Won Ho The Korean Society of Analytical Sciences 2006 분석과학 Vol.19 No.1

This paper describes the cumulative deposition of fallout Pu in soil and lichen at the present time and give the characteristics of fallout Pu deposits in the soil. In the soil of the forest, the accumulated depositions of $^{239,240}Pu$ were estimated to be in the range of 34.0 to $101.2Bq\;m^{-2}$ with an average value of $65.3{\pm}21.6Bq\;m^{-2}$. The average inventory of $^{239,240}Pu$ in the forest was calculated to be two times higher than that in the hill. Also, the deposited activities of $^{239,240}Pu$ in cultivated soil were significantly lower than those in the hill or forest. However, the cumulative depositions of fallout Pu in the volcanic ash soil on Cheju Island were much higher than those in the forest and hill soils. The measured activity concentrations of Pu isotopes in lichens and mosses showed large variations, due to characteristics of species and life span of lichen and moss colonies. From depth profiles, it was found that most of the fallout Pu has been accumulated in upper 10 cm layer of soil. Except for a few cases, the concentrations of $^{239,240}Pu$ in soil tended to decrease exponentially with increasing soil depth. Among parameters affecting the cumulative deposition of fallout Pu, organic substances and rainfall play an important role in the retention and relative mobility of fallout Pu in the soil. However, pH showed a weak correlation with the deposition of fallout Pu in the soil. From sequential leaching experiments, Pu was found to be associated predominantly with the "organic" and "oxy-hydroxy" fractions. Both the activity ratios of $^{238}Pu/^{239,240}Pu$ and $^{241}Pu/^{239,240}Pu$ in soils, lichens and mosses and the atomic ratios of $^{240}Pu/^{239}Pu$ in soils are close to those observed in the cumulative deposit global fallout from nuclear weapon testings. The results obtained from this research make it possible to interpret and predict the behavior of fallout Pu under natural conditions.

Characterization of composite prepared with different mixing ratios of TiO₂ to activated carbon and their photocatalytic activity

Chen, Ming-Liang,Bae, Jang-Soon,Ko, Young-Shin,Oh, Won-Chun The Korean Society of Analytical Sciences 2006 분석과학 Vol.19 No.5

In this work, pitch/activated carbon/$TiO_2$ composite were prepared by $CCl_4$ solvent method with different mixing ratios. The BET surface area of pitch/activated carbon/$TiO_2$ composite has a significantly increase with increasing activated carbon content in pitch/activated carbon/$TiO_2$ composite. The surface structure and elemental compositions of the composite were studied by SEM and EDX, respectively. The SEM results were presented to the characterization of porous texture on the pitch/activated carbon/$TiO_2$ composite. And EDX data was shown the presence of C, O, S, Ti and other elements. The structural properties of the composite were studied in XRD measurements. The $TiO_2$ crystal phases of the pitch/activated carbon/$TiO_2$ composite had lots of rutile-type structure which transforms from anatase-type with a little of anatase-type structure. The photocatalytic activities of the composite were evaluated using a photo-decomposition method under UV lamp. The pitch/activated carbon/$TiO_2$ composites were observed better photocatalytic activity than that of pristine $TiO_2$.

Synthesis of molecularly imprinted polymer (MIP) by radiation-induced polymerization and separation of ferulic acid from rice oil using MIP-packed column

Yoon, Seok-Kee,Lee, Jae-Chan,Lee, Seung-Ho,Choi, Seong-Ho,Kim, Hwa-Jung,Park, Hae-Jun,Kang, Hee-Dong The Korean Society of Analytical Sciences 2006 분석과학 Vol.19 No.3

A molecularly imprinted polymer (MIP) was synthesized by radiation-induced polymerization (RIP), where the ferulic acid was used as a template molecule, 4-vinylpyridine as a monomer and ethylene glycoldimethacrylate (EGDMA) as a cross-linking monomer. The MIP was packed in a glass column using a slurry method for use in medium pressure liquid chromatography (MPLC). The MPLC column was tested for separation and purification of ferulic acid from the rice oil. When repeated three times, the MPLC separation/purification yielded the ferulic acid with the purity higher than ~99%. The chemiluminescence of the luminal (5-amino-2,3-dihydro-1,4-phtalazinedione) measured on a potato disc slide (5.0 mm thick) was enhanced in the presence of ferulic acid, while, without the ferulic acid, the chemiluminescence of luminol on the potato slice disc was not observed, which suggests the ferulic acid obtained from the rice oil can be useful for immunoassay.

Self-assembly directed synthesis of tubular conducting polymer inside the channels of MCM-41

Showkat, Ali Md.,Lee, Kwang-Pill,Gopalan, Anantha Iyengar,Reddy, K. Raghava,Kim, Sang-Ho,Choi, Seong-Ho The Korean Society of Analytical Sciences 2006 분석과학 Vol.19 No.3

Diphenyl amine (DPA) was polymerized inside the channels of the mesoporous silica (MCM-41). MCM-41 (C) and MCM-41 (D) were prepared with cetyltrimethyl ammonium bromide (CTAB) and dodecyltrimethyl ammonium bromide (DTAB), respectively and used as hosts. Initially, the self assembly of DPA inside the pores of MCM-41 was made in ${\beta}$-naphthalene sulfonic acid (NSA) medium and subsequently poly (diphenylamine), PDPA was formed by oxidative polymerization. $N_2$ adsorption-desorption measurements of PDPA loaded MCM-41 (C) and MCM-41 (D) show variations in pore volume and surface area between them. A tubular form of poly (diphenylamine), PDPA was envisaged to form in the pores of MCM-41 and supported by high resolution transmission microscopy. The presence of PDPA inside the channel of MCM-41 was further confirmed by FTIR spectroscopy, thermogravimetric analysis (TGA), X-ray diffraction.

Acute cocaine intoxication in a body packer

Park, Mee-Jung,Lim, Mi-Ae,Chung, Hee-Sun The Korean Society of Analytical Sciences 2006 분석과학 Vol.19 No.1

A 35-year-old Perubian who suffered from grand mal seizures died in the aircraft on his way from the United States to Hongkong via Incheon international airport of Korea. While performing the autopsy, 115 packs made with double layer of transparent film and black plastic bag containing cocaine were found in the ileum and large intestine. Among of them, 3 packs were ruptured. To determine the concentration of cocaine and its metabolites, blood, urine, bile, liver, spleen, heart, kidney, brain and gastric contents were taken and toxicological analysis was performed. Gas chromatography/mass spectrometry (GC/MS) following liquid-phase extraction using chloroform:isopropanol (=9:1) and derivatization with bis(trimethylsilyl)-trifluoroacetamide (contains 1% trimethylchlorosilane) was performed. High levels of cocaine, benzoylecgonine (BE) and ecgonine methylester (EME) were found in the postmortem blood (0.96, 3.09 and $5.59{\mu}g/mL$) and urine (32.85, 145.35 and $53.17{\mu}g/mL$), respectively. Cocaine and its metabolites were also detected in all other biological specimen.

Comparative investigation of activated porous carbons treated by silver electroplating from aqueous solution

Oh, Won-Chun The Korean Society of Analytical Sciences 2006 분석과학 Vol.19 No.3

The electroplating of the Ag ions from aqueous solution on activated porous carbons was investigated over a wide range of plating time. The adsorption capacities of Ag metallic carbons were associated with their internal porosity and were related to physical properties such as surface area and pore size distribution. And, surface morphologies and quantitative analysis for the metal supported carbons are investigated by scanning electron microscopy (SEM) and energy disperse X-ray (EDX) measurements to explain the changes in adsorption properties. It is considered that the pH is an very important factor at the reason of water pollutant with increasing acidity in industrial field. The results of ICP-AES analysis showed that the residual concentration of Ag ions decreased with an increasing electroplating time. The metallic Ag-activated porous carbons electroplated showed microbicidal effects and strong antibacterial activity against six kinds of strains that were used. Finally, we confirmed that the presence of the electrolytic plated Ag-activated porous carbons is a determining factor in the HCl removal by chemical reaction, clarifying the surface chemical behavior.