• Steel and Composite Structures
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• v.44 no.4
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• pp.473-488
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• 2022

A high-speed railway (HSR) bridge may undergo long-term deformation due to the degradation of material stiffness, or foundation settlement during its service cycle. In this study, an analytical model is set up to evaluate the influence of this long-term vertical bridge deformation on the track geometry. By analyzing the structural characteristics of the HSR track-bridge system, the energy variational principle is applied to build the energy functionals for major components of the track-bridge system. By further taking into account the interlayer's force balancing requirements, the mapping relationship between the deformation of the track and the one of the bridge is established. In order to consider the different behaviors of the interlayers in compression and tension, an iterative method is introduced to update the mapping relationship. As for the validation of the proposed mapping model, a finite element model is created to compare the numerical results with the analytical results, which show a good agreement. Thereafter, the effects of the interlayer's different properties of tension and compression on the mapping deformations are further evaluated and discussed.

• Journal of the Korean Society of Food Science and Nutrition
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• v.41 no.6
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• pp.870-874
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• 2012

The objective of this study was to determine the content of capsaicinoids in different commercial pepper powders and pepper-containing products in the Korean market. The two major capsaicinoids in the samples, capsaicin and dihydrocapsaicin, were analyzed using reversed-phase HPLC. The levels of capsaicin and dihydrocapsaicin in pepper powders and pepper-containing products ranged from 0.21 to 78.24 and 0.20 to 38.82 mg/100 g sample, respectively. Pepper powders contained generally higher amounts of capsaicin and dihydrocapsaicin than pepper- containing products. In addition, the analytical method validation parameters including accuracy, precision, and specificity were provided to ensure the validity of the extraction procedure for capsaicinoid analysis. Overall recovery from pepper powder and pepper paste was close to 100% (n=3). The results of validation parameters indicated that the present method was reliable and reproducible for the HPLC analyses of capsaicin and dihydrocapsaicin in commercial pepper products.

• Food Science of Animal Resources
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• v.35 no.4
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• pp.466-472
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• 2015

A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

• Journal of Korean Society on Water Environment
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• v.32 no.6
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• pp.649-669
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• 2016

This study explored the analytical conditions for 21 veterinary antibiotics which have been popularly sold in South Korea in 2014 but have not yet been targeted in EPA method 1694. Most of the selected antibiotics were separated by a reverse-phase C18 column with a combination of (buffered) water and organic polar solvent, which was commonly methanol and acetonitrile in the gradient elution mode. Volatile additives such as formic acid, ammonium acetate and ammonium formate were usually added to the mobile phases to minimize asymmetrical and tailing of antibiotics' peaks and to increase their ionization in mass spectrometry. The analytical methods of aminoglycoside antibiotics were distinct from those of the other antibiotics in terms of adoption of ion-pair chromatography (IPC) and hydrophilic interaction liquid chromatography (HILIC) capable of retaining and separating extremely polar compounds due to their hydrophilicity. Trifluoroacetic acid or heptafluorobutyric acid was frequently added to the mobile phase as an ion-pair reagent for the IPC. Tandem mass spectrometry was numerously applied to the detection of antibiotics using positive electrospray ionization (ESI) and the selected reaction monitoring (SRM) mode. All reviewed analytical methods had been/were validated by evaluating recovery, limits of detection and quantification, decision limit or detection capability of the methods.

• Mass Spectrometry Letters
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• v.9 no.1
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• pp.30-36
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• 2018

A quantitation method for free amino acids in human serum was developed using a stepwise-dilution method and a bimodal cation exchange (CEX)/hydrophilic interaction liquid chromatography (HILIC)-tandem mass spectrometry system equipped with an electrospray ionization source (ESI/MS/MS). This method, which was validated using quality control samples, was optimized for enhanced selectivity and sensitivity. Dithiothreitol (DTT) was used as a reducing agent to prevent the oxidation of a serum sample ($50{\mu}L$), which was then subjected to stepwise dilution using 3, 30, and 90 volumes of acetonitrile containing 0.1% formic acid. Chromatographic separation was performed on an Imtakt Intrada Amino Acid column ($50mm{\times}3mm$, $3{\mu}m$) in mixed mode packed with CEX and HILIC ligands embedded in the stationary phase. Underivatized free amino acids were eluted and separated within 10 min. As a result of the validation, the precision and accuracy for the inter- and intraday assays were determined as 2.11-11.51% and 92.82-109.40%, respectively. The lowest limit of quantification (LLOQ) was $0.5-4.0{\mu}g/mL$ and the matrix effect was 80.22-115.93%. The proposed method was successfully applied to the quantitative analysis of free amino acids in human serum.

• Analytical Science and Technology
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• v.30 no.5
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• pp.295-302
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• 2017

This study presents a method validation for extraction and quantitative analysis of levulinic acid in soy sacues using high performance liquid chromatograph-photodiode array detector (HPLC-PDA). The levulinic acid in samples were extracted with distilled water, and then purified with C18 Sep-Pak cartridge. The calibration curves showed good linearity (R > 0.999) in a relatively wide concentration range ($2.5-400{\mu}g/mL$). Mean recoveries and relative standard deviation (RSD) of levulinic acid spiked in soy sauce samples at different spiking levels ($2.5-400{\mu}g/mL$; 6 point). Recoveries were 87.58-97.26 % with RSD less than 15 %, and limit of detection (LOD) and limit of quantification (LOQ) were 0.64 and $1.64{\mu}g/mL$, respectively. According to monitoring result with the established method, levulinic acid was found in 43 of 59 domestic commercial soy sauces, soy sauce based sauces and seasoned meats. The contamination levels were 0.44-1.23 mg/mL for soy sauces, 0.03-0.83 mg/mL for soy sauce based sauces and 8.43-38.94 mg/mL for seasoned meats. The results indicated to be rapidly and accurately qualifying levulinic acid and can be used as a suitable quality control method for soy sauce and soy sauce related commodities.

• Journal of Food Hygiene and Safety
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• v.36 no.5
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• pp.376-381
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• 2021

Red beet (Beta vulgaris L.) is a root vegetable and a popular functional food ingredient of dark red-purple appearance due largely to betacyanins, principally betanine (75-95%) and its isomer, isobetanine (15-45%). This study developed an analytical method for beet red in terms of betanine and isobetanine in processed food products labeled with beet red as a food additive. High Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD) was used with a C₁₈ column. Linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision and uncertainty in measurement were calculated for method validation. Matrix-matched calibration was applied to the candy, ice cream, and cocoa product, respectively, and R² was ≥0.9998, showing a high level of linearity. The LOD and LOQ were 0.16 to 0.32 and 0.48 to 0.97 mg/L, respectively. As a result of repeated intra-day and interday experiments to validate the accuracy and precision of the analytical method, the recovery rates were 96.0-103.1% and 100.0-102.2%, respectively and the RSD% was 0.5-3.3% and 0.9-3.8%, respectively. Moreover, the measurement uncertainty was estimated to be 1.71-12.43% depending on the matrix and the measured concentration. In this study, betanine and isobetanine were quantified (8.4-3,823.4 mg/kg) by applying the developed analytical method to processed food products (n= 26; e.g., candy, ice cream, and other processed foods) labeled with beet red as a food additive.

• Bulletin of the Korean Chemical Society
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• v.32 no.5
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• pp.1547-1553
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• 2011

An effective analytical method of gas chromatography/mass spectrometry (GC/MS) was developed for the rapid determination of essential oils in the crude extract of Acorus species (Acorus gramineus, Acorus tatarinowii, and Acorus calamus). Major phenypropanoids (${\beta}$,${\alpha}$-asarone isomers, euasarone, and methyleugenol) and ${\beta}$-caryophyllene in Acorus species were used as marker compounds and determined for the quality control of herbal medicines. To extract marker compounds, various extraction techniques such as solvent immersion, mechanical shaking, and sonication were compared, and the greatest efficiency was observed with sonication extraction using petroleum ether. The dynamic range of the GC/MS method depended on the specific analyte; acceptable quantification was obtained between 10 and 2000 ${\mu}g/mL$ for ${\beta}$-asarone, 10 and 500 ${\mu}g/mL$ for ${\alpha}$-asarone, 10 and 200 ${\mu}g/mL$ for methyleugenol, and between 5 and 100 ${\mu}g/mL$ for ${\beta}$-caryophyllene. The method was deemed satisfactory by inter- and intra-day validation and exhibited both high accuracy and precision, with a relative standard deviation < 10%. Overall limits of detection were approximately 0.34-0.83 ${\mu}g/mL$, with a standard deviation (${\sigma}$)-to-calibration slope (s) ratio (${\sigma}$/s) of 3. The limit of quantitation in our experiments was approximately 1.13-3.20 ${\mu}g/mL$ at a ${\sigma}$/s of 10. On the basement of method validation, 20 samples of Acorus species collected from markets in Korea were monitored for the quality control. In addition, principal component analysis (PCA) and hierarchical cluster analysis (HCA) were performed on the analytical data of 20 different Acorus species samples in order to classify samples that were collected from different regions.

• Journal of Environmental Health Sciences
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• v.36 no.6
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• pp.510-517
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• 2010

Phthalates, such as di (2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) have been proved to be teratogenics and endocrine disruptors, metabolized rapidly and excreted in the urine. In this study, a simultaneous analytical method for 10 phthalate metabolites, MnBP, MiBP, MBzP, MCHP, MEHP, MEHHP, MEOHP, MnOP, MiNP and MiDP, in human urines, based on switching system with on-line pretreatment column using HPLC-MS/MS has been developed. This method was validated according to the guideline of bioanalytical method validation of National Institute of Toxicological Research. Limits of detection range between 0.2 and 0.9 ng/ml for 10 phthalate metabolites. The calibration curves showed linearity in the range 0.997~0.999, and the results of the intra- and inter-day validations were in the range from 0.4 to 14.7% RSD and from 0.3 to 9.4% RSD, respectively. Recoveries of phthalate metabolites varied from 87.0 to 116.1%. This analytical method showed high accuracy and stable precision for all metabolites, and seems to be suitable for biomonitoring of phthalates in human urine.

• Analytical Science and Technology
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• v.31 no.3
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• pp.107-111
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• 2018

Currently, ultraviolet-visible spectrophotometry and titration methods are used for assay tests of tramadol hydrochloride injection and raw material in the Korean Pharmacopoeia XI (KP XI). Titration has also been used in the British Pharmacopoeia (BP 2013) for the assay test of tramadol hydrochloride, and the HPLC assay for tramadol hydrochloride raw material has been used in the United States Pharmacopeia (USP 39). In this study, we developed an alternative HPLC assay method for tramadol hydrochloride injection that is up to date and specific, and employs the same method as tramadol hydrochloride capsules. Validation of the HPLC method was conducted to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of the calibration curves in the desired concentration range was good ($r^2$ > 0.9999). RSDs of intra-day precision obtained were 0.05-0.08 % and inter-day precision obtained were 0.08-0.19 %. Accuracy was obtained with recoveries in the range of 98.16 % and 100.90 %. As a result of the system's suitability, the RSD of both retention time and the peak area obtained were 0.07 %. The values of the plate number and tailing factor of tramadol hydrochloride obtained were 7076 and 1.16, respectively. Because of the intermediate precision and robustness of the developed assay, it is expected to become a valuable tool for revising the Korean Pharmacopoeia (KP XI).