• Mass Spectrometry Letters
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• v.14 no.3
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• pp.104-109
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• 2023

Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

• Advances in materials Research
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• v.1 no.2
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• pp.129-146
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• 2012

Polycrystalline diamond is an ideal material for parts with micro-holes and has been widely used as dies and cutting tools in automotive, aerospace and woodworking industries due to its superior wear and corrosion resistance. In this research paper, the modeling and simultaneous optimization of multiple performance characteristics such as material removal rate and surface roughness of polycrystalline diamond (PCD) with ultrasonic machining process has been presented. The fuzzy logic and taguchi's quality loss function has been used. In recent years, fuzzy logic has been used in manufacturing engineering for modeling and monitoring. Also the effect of controllable machining parameters like type of abrasive slurry, their size and concentration, nature of tool material and the power rating of the machine has been determined by applying the single objective and multi-objective optimization techniques. The analysis of results has been done using the MATLAB 7.5 software and results obtained are validated by conducting the confirmation experiments. The results show the considerable improvement in S/N ratio as compared to initial cutting conditions. The surface roughness of machined surface has been measured by using the Perthometer (M4Pi, Mahr Germany).

• Smart Structures and Systems
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• v.29 no.4
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• pp.625-640
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• 2022

Maglev rail joints are vital components serving as connections between the adjacent F-type rail sections in maglev guideway. Damage to maglev rail joints such as bolt looseness may result in rough suspension gap fluctuation, failure of suspension control, and even sudden clash between the electromagnets and F-type rail. The condition monitoring of maglev rail joints is therefore highly desirable to maintain safe operation of maglev. In this connection, an online damage detection approach based on three-dimensional (3D) convolutional neural network (CNN) and time-frequency characterization is developed for simultaneous detection of multiple damage of maglev rail joints in this paper. The training and testing data used for condition evaluation of maglev rail joints consist of two months of acceleration recordings, which were acquired in-situ from different rail joints by an integrated online monitoring system during a maglev train running on a test line. Short-time Fourier transform (STFT) method is applied to transform the raw monitoring data into time-frequency spectrograms (TFS). Three CNN architectures, i.e., small-sized CNN (S-CNN), middle-sized CNN (M-CNN), and large-sized CNN (L-CNN), are configured for trial calculation and the M-CNN model with excellent prediction accuracy and high computational efficiency is finally optioned for multiple damage detection of maglev rail joints. Results show that the rail joints in three different conditions (bolt-looseness-caused rail step, misalignment-caused lateral dislocation, and normal condition) are successfully identified by the proposed approach, even when using data collected from rail joints from which no data were used in the CNN training. The capability of the proposed method is further examined by using the data collected after the loosed bolts have been replaced. In addition, by comparison with the results of CNN using frequency spectrum and traditional neural network using TFS, the proposed TFS-CNN framework is proven more accurate and robust for multiple damage detection of maglev rail joints.

• Bulletin of the Korean Chemical Society
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• v.23 no.8
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• pp.1139-1143
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• 2002

Analysis of lysophosphatidic acids (LPAs) is of clinical importance as they can serve a potential marker for ovarian and other gynecological cancers and obesity. It is critically important to develop a highly sensitive and specific method for the early detection of gynecological cancers to improve the overall outcome of this disease. We have established a novel quantification method of LPAs in human plasma by negative ionization tandem mass spectrometry (MS-MS) using multiple reaction monitoring (MRM) mode without the conventional TLC step. Protein-bound lipids, LPAs in plasma were extracted with methanol : chloroform (2:1) containing LPA C14:0 as an internal standard under acidic condition. Following back extraction with chloroform and water, the centrifuged lower phase was evaporated and reconstituted in methanol. The reconstituted solution was directly injected into electrospray source of MS/MS. For MRM mode, Q1 ions selected were m/z 409, 433, 435, 437 and 457 which corresponds to molecular mass [M-H]- of C16:0, C18:2, C18:1, C18:0 and C20:4 LPA, respectively. Q2 ions selected for MRM were m/z 79, phosphoryl product. Using MS/MS with MRM mode, all the species of LPAs were completely separated from plasma matrix without severe interferences. This method allowed simultaneous detection and quantification of different species of LPAs in a plasma over a linear dynamic range of 0.01-25 ㎛olL-1 . The detection limit of the method was 0.3 pmol/mL, with a correlation coefficient of 0.9983 in most LPAs analyzed. When applied to the plasmas of normal and gynecological cancer patients, this new method differentiated two different groups by way of total LPA level.

• Journal of Convergence for Information Technology
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• v.11 no.2
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• pp.107-116
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• 2021

In this study, an analytical method was developed for estradiol-17��, testosterone, and progesterone, which are growth promoters as veterinary drug residues in animal food. The analytes were separated using liquid chromatography, and was injected into a mass spectrometer through the electrospray ionization(ESI) process and detected in multiple reaction monitoring(MRM) mode. As the method was validated by CODEX CAC/GL 71-2009 guideline, it met the acceptable. The analysis of beef, pork, and chicken distributed in Korea was conducted with an established method to confirm the applicability of the actual sample. It was confirmed that the developed method can be quickly and reliably in the analysis for the growth promoters identified in domestic distributed livestock products. Through subsequent research, a highly utilized analysis method will be completed if the number of growth promoters is expanded based on the method and the simultaneous analytical method is established by including all of it.

• Analytical Science and Technology
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• v.28 no.2
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• pp.86-97
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• 2015

Recently, the consumption of dietary supplements has increased because of people’s greater interest in health. Unfortunately, the sales of dietary supplements containing unauthorized substances such as drugs have also increased. We developed a rapid, accurate method for the simultaneous determination of antihistamines using liquid chromatography tandem mass spectrometry with a multiple reaction monitoring mode. The limit of detection (LOD) and limit of quantification (LOQ) of the instrument used in this method were in the ranges 0.0003-0.3 and 0.0009-0.6 µg mL⁻¹, respectively. The linearity of the method was > 0.99. The precision levels of the method were 0.1-9.8% (intra-day) and 0.3-9.6% (inter-day), and the levels of accuracy of the method were 82.7-115.0% (intra-day) and 84.3-113.0% (inter-day). The mean of recovery of the method was in the range of 83.9-117.9% and the RSD of the stability was less than 5.9%.

• Journal of Biomedical Engineering Research
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• v.44 no.6
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• pp.392-403
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• 2023

This study presents a new hybrid fNIRS-EEG system to meet the demand for a lightweight and low-cost sleep pattern monitoring device. For multiple-channel configuration, a six-channel electroencephalogram (EEG) and a functional near-infrared spectroscopy (fNIRS) system with eight photodiodes (PD) and four dual-wavelength LEDs are designed. To enhance the convenience of signal measurement, the device is miniaturized into a patch-like form, enabling simultaneous measurement on the forehead. Due to its fully integrated functionality, the developed system is advantageous for performing sleep stage classification with high-temporal and spatial resolution data. This can be realized by utilizing a two-dimensional (2D) brain activation map based on the concentration changes in oxyhemoglobin and deoxyhemoglobin during sleep stage transitions. For the system verification, the phantom model with known optical properties was tested at first, and then the sleep experiment for a human subject was conducted. The experimental results show that the developed system qualifies as a portable hybrid fNIRS-EEG sleep pattern monitoring device.

• Journal of Pharmaceutical Investigation
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• v.37 no.3
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• pp.179-186
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• 2007

A simple, sensitive and selective liquid chromatographic/tandem mass spectrometric method (LC-MS/MS) was developed and validated for doxifluridine and 5-fluorouracil (5-FU) quantification in dog heparinized plasma. Sample preparation was based on liquid-liquid extraction using a mixture of isopropanol/ethyl acetate (1/9 v/v) to extract doxifluridine, 5-FU and 5-chlorouracil (5-CU, an internal standard) from plasma. Chromatography was performed on a C-18 analytical column and the retention times were 2.7, 1.5 and 1.7 min for doxifluridine, 5-FU and 5-CU, respectively with shorter analysis time within 5 min than previously reported methods. The ionization was optimized using ESI negative mode and selectivity was achieved by tandem mass spectrometric analysis by multiple reaction monitoring (MRM) using the transformations of m/z 244.8>107.6, 129.0>42.0 and 144.9>42.1 for doxifluridine, 5-FU and 5-CU, respectively. The achieved low limit of quantification was 20.0 ng/mL and the assay exhibited linear range of 20-2000 ng/mL ($R^2>0.99957$ for doxifluridine and $R^2>0.99857$ for 5-FU), using $100{\mu}L$ of plasma. Accuracy and precision of quality control samples for both doxifluridine and 5-FU met KFDA and FDA Guidance criteria of 15% for accuracy with coefficients of variation less than 15%. This method demonstrated adequate sensitivity, specificity, accuracy, precision and stability to support the simultaneous analysis of doxifluridine and 5-FU in dog plasma samples in pharmacokinetic and bioequivalence studies.

• Bulletin of the Korean Chemical Society
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• v.33 no.1
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• pp.177-182
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• 2012

A new composition of standardized Scutellariae Radix extract (HPO12) was developed for treatment of Alzheimer's disease. For the preclinical pharmacokinetic study of HPO12, a rapid, sensitive, and selective LCMS/MS method was developed and validated for the simultaneous determination of 4 bioactive compounds, baicalein, baicalin, wogonin, and wogonoside. After extraction with ethylacetate, chromatographic analysis was performed on a Thermo $C_{18}$ column ($150mm{\times}2.1mm$, $3{\mu}m$) with a mobile phase consisting of 0.1% formic acid (A) and 0.1% formic acid in 95% acetonitrile (B) by using gradient elution at a flow rate of $250{\mu}L/min$. Analytes introduced to a mass spectrometer were monitored by multiple reaction monitoring (MRM) in positive ion mode. Using $25{\mu}L$ of plasma sample, the method was validated over the following concentration ranges: 25-5000 ng/mL for baicalein, 20-40000 ng/mL for baicalin, 1-1000 ng/mL for wogonin, and 5-10000 ng/mL for wogonoside. The intra- and inter-day precision and accuracy of the quality control samples at the 4 concentrations showed $\leq$ 13.7% relative standard deviation (RSD) and 86.6-105.5% accuracy. The method was successfully applied to determine the concentrations of baicalein, baicalin, wogonin, and wogonoside in rat plasma after intraperitoneal and oral administrations of HPO12.

• Mass Spectrometry Letters
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• v.12 no.2
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• pp.31-40
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• 2021

Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.