• Analytical Science and Technology
• /
• v.35 no.2
• /
• pp.82-91
• /
• 2022

Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquid-chromatography-tandem-mass-spectrometric method (LC-MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 ㎍/g. The intra- and inter-day deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 - 64.86 ㎍/g and 0.25 - 63.99 ㎍/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.

• Journal of Food Hygiene and Safety
• /
• v.31 no.1
• /
• pp.15-20
• /
• 2016

Malachite green was measured in 200 freshwater fish collected from local markets in Seoul using HPLC-DAD and LC-MS/MS. LC-MS/MS method was validated by linearity, accuracy, precision and limits of detection and quantification according to the CODEX's recommendation and HPLC-DAD method was applied according to the Food Code. Malachite green levels above the quantification limit of the LC-MS/MS were determined 18.5% (37) but just 1 fish was shown to contain malachite green by HPLC-DAD. Of 83 domestic fish, 21 fish were detected malachite green (25.3%). Of 117 fish from China, just 16 fish were detected malachite green (13.4%). In detection rate by species carp (35.0%), Crucian carp (30.4%), cat fish (28.0%), Korean bull head (23.8%), snake head (20.0%), eel (10.5%) and loach (7.8%) were in order. Especially, fish collected at summer were shown to contain malachite green frequently; the detection rate was 54.8%.

• Journal of the Institute of Electronics Engineers of Korea SD
• /
• v.43 no.11 s.353
• /
• pp.58-68
• /
• 2006

This work proposes a 10b 250MS/s $1.8mm^2$ 85mW 0.13um CMOS A/D Converter (ADC) for high-performance integrated systems such as next-generation DTV and WLAN simultaneously requiring low voltage, low power, and small area at high speed. The proposed 3-stage pipeline ADC minimizes chip area and power dissipation at the target resolution and sampling rate. The input SHA maintains 10b resolution with either gate-bootstrapped sampling switches or nominal CMOS sampling switches. The SHA and two MDACs based on a conventional 2-stage amplifier employ optimized trans-conductance ratios of two amplifier stages to achieve the required DC gain, bandwidth, and phase margin. The proposed signal insensitive 3-D fully symmetric capacitor layout reduces the device mismatch of two MDACs. The low-noise on-chip current and voltage references can choose optional off-chip voltage references. The prototype ADC is implemented in a 0.13um 1P8M CMOS process. The measured DNL and INL are within 0.24LSB and 0.35LSB while the ADC shows a maximum SNDR of 54dB and 48dB and a maximum SFDR of 67dB and 61dB at 200MS/s and 250MS/s, respectively. The ADC with an active die area of $1.8mm^2$ consumes 85mW at 250MS/s at a 1.2V supply.

• Economic and Environmental Geology
• /
• v.48 no.4
• /
• pp.301-312
• /
• 2015

A commercial gas field was found in the southwestern continental shelf of the Ulleung Basin, East Sea in the late 1990s. To develop additional gas field, an exploration well was drilled through the coarse infill of submarine canyon near the gas field, but it was uneconomic to develop hydrocarbons. Using newly acquired deep seismic reflection and previous well data, we have identified additional geological structure which has hydrocarbon potentials below submarine canyons in the southwestern margin of the basin. Based on the interpretation of the deep seismic reflection and well data, the sequences of the study area can be classified into the syn-rift megasequence(MS1), post-rift megasequence(MS2), syn-compressional megasequence(MS3), and post-compressional megasequence(MS4) in relation to the tectonic events. MS1, deposited simultaneously with the basin formation before the middle Miocene, is characterized by chaotic seismic facies with low- to moderate-amplitude and low frequency reflections. MS2 comprises laterally continuous, low- to moderate-amplitude reflections, showing progradational stacking patterns due to high rates of sediment supply during basin expansion in the middle Miocene. MS3 is mainly composed of continuous reflections with high amplitude and moderate- to high-frequency which are interpreted as coarse-grained sediments. The coarse-grained sediments of MS3 sequence is widely truncated by several submarine canyons which filled with fine-grained sediment of MS4 to form a stratigraphic trap of hydrocarbon. Therefore, the reservoir and seal of the hydrocarbon trap in the study area are coarse-grained sediment of MS3 and submarine canyon filled with fine-grained sediment of MS4, respectively. A flat-spot seismic anomaly, which may indicate the presence of hydrocarbon, is observed within the stratigraphic trap.

• Journal of Food Hygiene and Safety
• /
• v.37 no.2
• /
• pp.46-54
• /
• 2022

Known for its effectiveness in weight loss and diabetes prevention, Gymnema sylvestre products can be found in the US, Japanese, and Indian markets. However, the recommended dosage or safety of these products has not yet been proven. Therefore, development of an analytical method for detecting the content of Gymnema sylvestre in food products is required. Accordingly, this study proposes an analysis method that can examine Gymnema sylvestre in food using LC-ESI-MS/MS and KASP (Kompetitive Allele-Specific PCR) markers. In LC-ESI-MS/MS, a simultaneous analysis method for gymnemic acid and deacylgymnemic acid was optimized using negative ionization mode, and its validation test was completed for solid and liquid samples. In addition, KASP markers were prepared by finding the specific SNP of G. sylvestre in ITS2 and matK through DNA barcodes. The two KASP markers returned positive FAM fluorescence result when combined with G. sylvestre, and this aspect was confirmed in raw G. sylvestre as well. The applicability of the method was tested on 21 different food and healthy functional products containing G. sylvestre purchased on the internet. As a result, although there was a difference in the ratios of gymnemic acid and deacylgymnemic acid in LC-ESI-MS/MS, the index component was detected in all 21 products samples. In the KASP analysis, 9 products returned positive FAM result, and the rest of the products were found to be containing G. sylvestre extract. This study is the first study to use the dual system of LC-ESI-MS/MS and KASP for the analysis of G. sylvestre. The study has confirmed that these two methods are applicable to the examine G. sylvestre content in food products.

• Journal of IKEEE
• /
• v.25 no.2
• /
• pp.302-308
• /
• 2021

A 12-bit 10-MS/s pipeline analog-to-digital converter (ADC) is proposed for image processing applications. The proposed pipeline ADC consists of a sample and hold amplifier, three stages, a 3-bit flash analog-to-digital converter, and a digital error corrector. Each stage is operated by using a 4-bit flash ADC (FADC) and a multiplying digital-to-analog converter (MDAC). The proposed sample and hold amplifier increases the voltage gain using gain boosting for the ADC with high resolution. The proposed pipelined ADC is designed using a 180-nm CMOS process with a supply voltage of 1.8 and it has an effective number of bit (ENOB) of 10.52 bits at sampling rate of 10MS/s for a 1-V_pp differential sinusoidal analog input with frequency of 1 MHz. The measured ENOB is 10.12 bits when the frequency of the sinusoidal analog input signal is a Nyquist frequency of approximately 5 MHz.

• Mass Spectrometry Letters
• /
• v.8 no.4
• /
• pp.109-113
• /
• 2017

Single analytical procedure including extraction, liquid chromatography, and mass spectrometric analysis was evaluated for the simultaneous measurement of lysophospholipids (LPLs). LPLs, particularly, lysophosphatidic acids (LPA) and sphingosine 1-phosphate (S1P) are lipid messengers ubiquitously found in various biological matrix. The molecular species mediate important physiological roles in association with many diseases (e.g. cancer, inflammation, and neurodegenerative disease), which emphasize the significance of the simple and reliable analytical method for biomarker discovery and molecular mechanistic understanding. Thus, we developed analytical method mainly focusing on, but not limited by those lipid species S1P and LPA using reverse phase liquid chromatography-tandem mass spectrometry (RPLC-ESI-MS-MS). Extraction method was modified based on Folch method with optimally minimal level of ionization additive (ammonium formate 10 mM and formic acid). Reverse-phase liquid-chromatography was applied for chromatographical separation in combination with negative ionization mode electrospray-coupled Orbitrap mass spectrometry. The method validation was performed on human blood plasma in a non-targeted lipid profiling manner with full-scan MS mode and data-dependent MS/MS. The proposed method presented good inter-assay precision for primary targets, S1P and LPA. Subsequent analysis of other types of LPLs identified a broad range of lysophosphatidylcholines (LPCs) and lysophosphatidyl-ethanolamines (LPEs).

• Journal of Environmental Health Sciences
• /
• v.35 no.4
• /
• pp.322-333
• /
• 2009

In this study, a measurement method was evaluated for the determination of polycyclic aromatic hydrocarbons (PAHs) in the ambient atmosphere. PAHs were sampled by high-volume samplers, and were then analysed with a GC/MS system. Particulate PAHs were collected on $8"{\times}10"$ quartz fiber filter, while vapor phase PAHs were adsorbed on polyurethane foam (PUF). Target compounds included a total of 36 PAHs, which are known to be frequently detected in the urban atmosphere. It was not necessary to clean-up samples before samples were analyzed using GC/MS, and the overall performance of the method was tested by a variety of quality control and quality assurance schemes. It is generally known that the clean-up procedure can negatively affect the recovery of samples. Precision and accuracy was evaluated using SRM provided by US NIST, and the results were generally satisfactory and reliable. However, the GC/MS method appeared not to be adequate for 6-rings PAHs, such as coronene, due to its lower sensitivity. In addition, collection efficiencies for low molecular compounds, such as 2-rings PAHs, were poor because of the lower retention volume of the PUF adsorbent. As a result, it was concluded that the method based on high-volume sampling and GC/MS analysis can give very reliable data by simultaneous sampling of both particulate and vapor phases for 3-rings to 5-rings PAHs of environmental concern.

• Food Science of Animal Resources
• /
• v.34 no.6
• /
• pp.763-768
• /
• 2014

The identity of 45 Hanwo and 47 imported beef (non-Hanwoo) samples from USA and Australia were verified using the microsatellite (MS) marker and single nucleotide polymorphism (SNP) methods. Samples were collected from 19 supermarkets located in the city of Seoul and Gyeonggi province, South Korea, from 2009 to 2011. As a result, we obtained a 100% concordance rate between the MS and SNP methods for identifying Hanwoo and non-Hanwoo beef. The MS method presented a 95% higher individual discriminating value for Hanwoo (97.8%) than for non-Hanwoo (61.7%) beef. For further comparison of the MS and SNP methods, blood samples were collected and tested from 54 Hanwoo ${\times}$ Holstein crossbred cattle (first, second, and third generations). By using the SNP and MS methods, we correctly identified all of the first-generation crossbred cattle as non-Hanwoo; in addition, among the second and third generation crossbreds, the ratio identified as Hanwoo was 20% and 10%, respectively. The MS method used in our study provides more information, but requires sophisticated techniques during each experimental process. By contrast, the SNP method is simple and has a lower error rate. Our results suggest that the MS and SNP methods are useful for discriminating Hanwoo from non-Hanwoo breeds.

• Bulletin of the Korean Chemical Society
• /
• v.33 no.11
• /
• pp.3727-3734
• /
• 2012

An analytical method has been developed for the rapid determination of perfluorinated compounds (PFCs) in human serum samples. The extraction and purification of PFCs from human serum were performed by the modified method of previous report. Ten PFCs were rapidly separated within 3.3 min by C18-monolithic column liquid chromatography (LC) and detected by electrospray ionization (ESI) tandem mass spectrometry (MS/MS) in negative ion mode. The runtime of PFCs on monolithic column LC was up to 4-fold faster than that on conventional column LC. The effect of triethylamine (TEA) to the mobile phase has investigated on the overall MS detection sensitivity of PFCs in ESI ionization. Quantification was performed by LC-MS/MS in multiple-ion reaction monitoring (MRM) mode, using $^{13}C$-labeled internal standards. Method validation was performed to determine recovery, linearity, precision, and limits of quantification, followed by, the analysis of a standard reference material (SRM 1957 from NIST). The overall recoveries ranged between 81.5 and 106.3% with RSDs of 3.4 to 16.2% for the entire procedure. The calibration range extended from 0.33 to 50 $ng\;mL^{-1}$, with a correlation coefficient ($R^2$) greater than 0.995 and the limits of quantification with 0.08 to 0.46 $ng\;mL^{-1}$. This approach can be used for rapid and sensitive quantitative analysis of 10 PFCs in human serum with high performance and accuracy.