• Title/Summary/Keyword: $MS^n$

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Validation of LC-MS/MS Method for Analysis of Paralytic Shellfish Toxins in Shellfish and Tunicates (LC-MS/MS를 이용한 패류 및 피낭류 중 마비성 패류독소 분석법의 유효성 검증)

  • Cho, Sung Rae;Kim, Dong Wook;Yu, Hean Jae;Cho, Seong Hae;Ryu, Ara;Lee, Ka Jeong;Mok, Jong Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.53 no.2
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    • pp.174-180
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    • 2020
  • The mouse bioassay has been used widely for the monitoring of paralytic shellfish toxins (PSTs) in many countries. However, this method shows low sensitivity and high limit of detection (LOD), as well as it cannot confirm toxic profiles. Recently, LC-MS/MS method was studied for the quantitative of PSTs, however, the method has any problems with unstable retention times by ionization suppression caused by high salt concentration in shellfish extracts. To establish an alternative method for PSTs analysis, we tried to original LC-MS/MS methods adding desalting operation using amorphous graphitized polymer carbon solid-phase extraction cartridges. The method validation was conducted to determine linearity, limit of detection, limit of quantification (LOQ), accuracy, and precision in quantifying PSTs. The correlation coefficients for all tested PSTs maintained over 0.999. The LODs and LOQs for all PSTs were about 0.19-1.05 ㎍/kg and 0.58-3.18 ㎍/kg, respectively. The accuracies for PSTs were 95.4-107.7% for saxitoxin group, 97.1-100.9% for gonyautoxin group, 99.0-100.8% for N-sulfocarbamoyl toxin group, and 96.8-104.6% for decarbamoyl toxin group. These results indicate that the modified LC-MS/MS method was appropriate for analyzing the PSTs in shellfish and tunicates.

Identification of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Gas Chromatography/Mass Spectrometry (GC/MS에 의한 오미자 Lignan성분의 동정)

  • Sohn, Hyun-Joo;Bock, Jin-Young
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.344-349
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    • 1989
  • Eleven lignan compounds in fruits of Schisandra chinensis BAILLON were identified by gas chromatography/mass spectrometry(GC/MS). The GC/MS conditions were as followed: the GC column used was SPB-1 fused silica capillary $(0.25mm\;id{\times}30m,Supelco)$ and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute; the MS ionization voltage was 70eV (EI mode). The compounds identified were gomisin J $(M^+;\;388)$, deoxyschizandrin$(M^+;\;416)$, gomisin N $(M^+;\;400)$, schizandrin$(M^+;\;432)$, wuweizisu C $(M^+;\;384)$, gomisin A $(M^+;\;416)$, angeloylgomisin H $(M^+;\;500)$, tigloylgomisin H $(M^+;\;500)$, angeloylgomisin Q $(M^+;\;530)$, gomisin B $(M^+;\;514)$ and benzoylgomisin H $(M^+;\;522)$, peaks of which were separated well on the GC chromatogram.

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Change of the upper airway after mandibular setback surgery in patients with mandibular prognathism and anterior open bite

  • Lee, Kyungjin;Hwang, Soon Jung
    • Maxillofacial Plastic and Reconstructive Surgery
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    • v.41
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    • pp.51.1-51.8
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    • 2019
  • Purpose: It has been reported before that the amount of pharyngeal airway space (PAS) significantly decreases following mandibular setback (MS) surgery in patients with mandibular prognathism (MP). Further, MP patients with an anterior open-bite (AOB) presentation may show a larger decrease in PAS compared with those without AOB. However, studies on postoperative PAS changes in MP patients with AOB remain rare. This study sought to evaluate changes in PAS and hyoid bone positioning following MS surgery in MP patients with and without AOB. Patients and methods: Twenty patients who underwent two jaw surgery involving MS movement were included. Patients were divided into a non-AOB group (n = 10; overbite > 2 mm) and an AOB group (n = 10; overbite < - 4 mm). Three-dimensional changes in PAS and hyoid bone positioning were compared and statistically evaluated pre- and postoperatively using computed tomography (CT). Results: The mean magnitude of MS was 6.0 ± 2.8 mm and 5.6 ± 3.2 mm in the non-AOB group and AOB group, respectively. The oropharyngeal volume and upper hypopharyngeal volume were significantly reduced after surgery in both the groups (p = 0.006 and p = 0.003), while the retroglossal cross-sectional area was significantly reduced only in the AOB group (p = 0.028). Although the AOB group showed a larger decrease in PAS, the difference was not statistically significant between the groups. The position of the hyoid bone showed significant posterior and inferior displacement only in the AOB group, while the vertical displacement of the hyoid bone showed a statistically significant difference between the two groups. Conclusion: PAS was significantly decreased after MS in both the groups, while only the AOB group presented a statistically significant reduction in the retroglossal cross-sectional area. Vertical displacement of the hyoid bone showed a statistically significant difference between the groups, while the PAS change was not. Surgeons should be aware of potential postoperative airway problems that may arise when performing MS surgeries.

Meal skipping relates to food choice, understanding of nutrition labeling, and prevalence of obesity in Korean fifth grade children

  • Kim, Hye-Young;Lee, Na-Rae;Lee, Jung-Sug;Choi, Young-Sun;Kwak, Tong-Kyung;Chung, Hae-Rang;Kwon, Se-Hyug;Choi, Youn-Ju;Lee, Soon-Kyu;Kang, Myung-Hee
    • Nutrition Research and Practice
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    • v.6 no.4
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    • pp.328-333
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    • 2012
  • This study was performed to investigate the differences in food choice, nutrition labeling perceptions, and prevalence of obesity due to meal skipping in Korean elementary school children. A national survey was performed in 2010 to collect data on food intake frequency, understanding of nutrition labeling, and body mass index from 2,335 fifth grade students in 118 elementary schools selected from 16 metropolitan local governments by stratified cluster sampling. The data were analyzed using the SAS 9.1 and SUDAAN 10.0 packages. Students who consumed three meals for 6-7 days during the past week were classified into the regular meal eating (RM) group (n = 1,476) and those who did not were placed into the meal skipping (MS) group (n = 859). The daily intake frequency of fruits, vegetables, kimchi, and milk was significantly lower in the MS group compared to that in the RM group (P < 0.001), whereas the daily intake frequency of soft drinks and instant noodles (ramyeon) was significantly higher in the MS group than that in the RM group (P < 0.05). The MS group demonstrated a significantly lower degree of understanding with regard to nutrition labeling and high calorie foods containing low nutritional value than that in the RM group. The distribution of obesity based on the percentile criteria using the Korean growth chart was different between the MS and RM groups. The MS group (8.97%) had a higher percentage of obese subjects than that in the RM group (5.38%). In conclusion, meal skipping was related to poor food choice, low perception of nutrition labeling, and a high prevalence of obesity in Korean fifth grade children.

Life Firing Test of 1 N-class Monopropellant Thruster Development Model -Part II: Pulse Mode Performance (1 N급 단일추진제 추력기 개발모델의 장기수명 연소시험 -Part II: 펄스모드 성능 특성)

  • Won, Su-Hee;Kim, Su-Kyum;Jun, Hyoung-Yoll;Lee, Jun-Hui;Park, Su-Hyang;Lee, Jae-Won
    • Journal of the Korean Society of Propulsion Engineers
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    • v.18 no.6
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    • pp.68-74
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    • 2014
  • During the life firing test of 1 N-class thruster development model, pulse mode performance and performance changes were examined. The deviation of pulse mode response time according to thruster feed pressure was relatively small and the resultant ignition delay, response time, tail-off time were 32-35 ms, 86-91 ms, 89-98 ms, respectively. For the stabilized pulse region the impulse bit revealed the outstanding reproducibility of 1.41, 1.32, 2.10% at $3{\sigma}$. During the life firing test, the impulse bit was decreased with limited amounts, therefore the pulse mode performance could be considered to be maintained. The thrust centroid was also maintained during the life firing test.

Development and validation of a qualitative GC-MS method for THCCOOH in urine using injection-port derivatization

  • Sim, Yeong Eun;Kim, Ji Woo;Kim, Jin Young
    • Analytical Science and Technology
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    • v.34 no.2
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    • pp.68-77
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    • 2021
  • Cannabis is one of the most abused drugs in Korea. The main psychoactive component in cannabis, Δ9-tetrahydrocannabinol, is metabolized to 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) and THCCOOH-glucuronide (THCCOOH-glu) in the human liver, whereby the amount of THCCOOH-glu found in urine is twice as high as that of THCCOOH. The analytical process adapted by the majority of urine drug-testing programs involves a two-step method consisting of an initial immunoassay-based screening test followed by a confirmatory test if the screening test result is positive. In this study, a qualitative gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the detection of THCCOOH in human urine, where THCCOOH-glu was converted into THCCOOH by alkaline hydrolysis. For purification of the urine extract prior to instrumental analysis, high-speed centrifugation was used to minimize interference. In addition, an injection-port derivatization method using ethyl acetate and N,O-bis(trimethylsilyl)-trifluoroacetamide containing 1 % trimethylchlorosilane was employed to reduce the time required for derivatization, and an aliquot of the final solution was injected into the GC-MS. The method was validated by measuring the selectivity, limit of detection (LOD), and repeatability. The sensitivity, specificity, precision, accuracy, Kappa, F-measure, false positive, and false negative rate were determined by comparing the GC-MS results with those obtained using the immunoassay. The LOD was determined to be 0.32 ng/mL, while the repeatability was within 9.1 % for THCCOOH. Furthermore, a comparison study was carried out, whereby the screening immunoassay exhibited a sensitivity of 86.4 % and a specificity of 100 % compared to GC-MS. The applicability of the developed method was examined by analyzing spiked urine and forensic urine samples obtained from suspected cannabis abusers (n = 221).

Rapid Identification of Staphylococcus Species Isolated from Food Samples by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

  • Kim, Eiseul;Kim, Hyun-Joong;Yang, Seung-Min;Kim, Chang-Gyeom;Choo, Dong-Won;Kim, Hae-Yeong
    • Journal of Microbiology and Biotechnology
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    • v.29 no.4
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    • pp.548-557
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    • 2019
  • Staphylococcus species have a ubiquitous habitat in a wide range of foods, thus the ability to identify staphylococci at the species level is critical in the food industry. In this study, we performed rapid identification of Staphylococcus species using Matrix-Assisted Laser Desorption/Ionization Time-of-Flight mass spectrometry (MALDI-TOF MS). MALDI-TOF MS was evaluated for the identification of Staphylococcus reference strains (n = 19) and isolates (n = 96) from various foods with consideration for the impact of sample preparation methods and incubation period. Additionally, the spectra of isolated Staphylococcus strains were analyzed using principal component analysis (PCA) and a main spectra profile (MSP)-based dendrogram. MALDI-TOF MS accurately identified Staphylococcus reference strains and isolated strains: the highest performance was by the EX method (83.3~89.5% accuracy) at species level identification (EDT, 70.3~78.9% accuracy; DT, less than 46.3~63.2% accuracy) of 24-h cultured colonies. Identification results at the genus level were 100% accurate at EDT, EX sample preparation and 24-h incubation time. On the other hand, the DT method showed relatively low identification accuracy in all extraction methods and incubation times. The analyzed spectra and MSP-based dendrogram showed that the isolated Staphylococcus strains were characterized at the species level. The performance analysis of MALDI-TOF MS shows the method has the potential ability to discriminate between Staphylococcus species from foods in Korea. This study provides valuable information that MALDI-TOF MS can be applied to monitor microbial populations and pathogenic bacteria in the food industry thereby contributing to food safety.

A Study on 10 Metabolites Separated from DNA Adduce of Blood Lymphocytes in Rats Exposed Orally with 3,3-dichlorobenzidine(DCB) by GC/MS-SIM

  • Shin, Ueon-Sang;Lee, Jin-Heon
    • Journal of Environmental Health Sciences
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    • v.28 no.4
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    • pp.6-11
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    • 2002
  • 3.3'-Dichlorobenzidine(DCB) has be shown carcinogenic in several animals, and the development of non-invasive biomonitoring method in workers exposed with it is a very important subject. DNA adduct is a good biomarker for biomonitoring about carcinogens exposure, and lymphocytes is a good non-invasive samples. So we studied to analyze metabolites in blood lymphocytes of female Sprague-Dawley rats exposed orally with DCB(20, 30, and 40 mg/kg wt.) for 3 weeks. For analysis of them, we isolated DNA adducts from blood lymphocytes by using the enzymes method in /sup 32/P-postlabeling, and measured them by using gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM). 4-aminobiphenyl and phenanthrene-d/sub 10/ were added as internal standard for blank sample. Standard metabolites of DCB were synthesized with using pyridine and acetic acid which were promoter and controller in acetylation of DCB. And they were used for calibration curve. Our results showed two kinds of metabolites in DNA adducts of blood lymphocytes. They were N-acetyl 3,3'-dichlorobenzidine(acDCB) and N,N'-diacetyl 3,3'-dichiorobenzidine(di-acDCB ). They were combined with DNA at the same time as an acetyl of it was removed. So we measured DCB and acDCB for two kinds of metabolites in DNA adducts of blood lymphocytes. Our results showed the levels of DCB were 1.46∼2.26 times more than that of acDCB. And also the levels of metabolites in 20, 30 and 40 mg/kg wt. were gradually increased with going days from 1st to 3rd week. They are 1.66, 1.38 and 0.90 times in total metabolites, 1.76, 1.49 and 1.02 times in DCB, and 1.51, 1.22 and 1.28 times in acDCB. In conclusion, the results of this study showed DCB exposed to rats formed DNA adduct in blood lymphocytes after acetylated to N-acetyl 3.3'-dichloro benzidine(acDCB) and N,N'-diacetyl 3,3'-dichlorobenzidine(di-acDCB), and they could be analyzed by us ing gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM).

The Difference of Ginsenoside Compositions According to the Conditions of Extraction and Fractionation of Crude Ginseng Saponins (추출 및 분획조건에 따른 인삼 조사포닌 중 ginsenoside 조성 차이)

  • Shin, Ji-Young;Choi, Eon-Ho;Wee, Jae-Joon
    • Korean Journal of Food Science and Technology
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    • v.33 no.3
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    • pp.282-287
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    • 2001
  • This study was carried out to investigate the difference of ginsenoside compositions in crude ginseng saponins prepared by five different methods including three new methods. Two known methods are hot methanol(MeOH) extraction/n-butanol(n-BuOH) fractionation and hot MeOH extraction/Diaion HP-20 adsorption/MeOH elution. Three new methods are hot MeOH extraction/cation AG 50W $absorption/H_2O$ elution/n-BuOH extraction, cool MeOH extraction/Diaion HP-20 adsorption/MeOH elution and direct extraction with ethyl acetate(EtOAc)/n-BuOH. Analysis of ginsenoside composition in the crude saponins by conventional HPLC/RI(Refractive Index) did not show great difference between methods except EtOAc/n-BuOH method. However, HPLC/ELSD (evaporative light scattering detector) employing gradient mobile phase afforded fine resolution of ginsenoside Rf, $Rg_1$ and $Rh_1$, and great difference of ginsenoside compositions between methods. LC/MS revealed that large amount of prosapogenins were produced during the pass through the cation exchange (AG 50W) column being strongly acidic. Six major ginsenosides such as $Rb_1,w;Rb_2,$ Rc, Rd, Re and $Rg_1$, 5 prosapogenins and one chikusetsusaponin were identified by LC/MS. A newly established HPLC method employing ODS column and gradient mobile phase of $KH_2PO_4/CH_3CN$ revealed that malonyl ginsenosides were detected only in the crude saponin obtained from cool MeOH extraction.

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Influence of Heating Conditions on the Formation of Acrylamide and Other Products in Asparagine-Glucose Model Reaction System (Model reaction system에서 가열조건이 acrylamide 및 기타 화합물들의 생성에 미치는 영향)

  • Lee Young-Guen
    • Journal of Life Science
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    • v.16 no.2 s.75
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    • pp.323-327
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    • 2006
  • The Formation of acrylamide was studied in Maillard model reaction systems based on asparagine-glucose. The mixture of asparagine and glucose in equal molar ratio, and then heated at 125, 150, 175 and $200^{\circ}C$ for 10, 20 and 30 minute, respectively. The reaction products were extracted with ethyl acetate and methanol, and then isolated and detected on FFAP capillary column and HP-5MS 5% phenyl methyl siloxane column by using GC/MS. Acrylamide was detected only from methanol extracts and on FFAP capillary column, at retention time 23.53 min., and the detection limit was 4.6 ng. Acrylamide content mainly increased with increasing temperature and processing time till $175^{\circ}C$, therefore, maximal acrylamide formation occurred at $175^{\circ}C$ for 10 minute ($116{\mu}g/g$), while, above $175^{\circ}C$, higher temperatures or prolonged processing times caused a decrease of acrylamide levels, finally disappeared at $200^{\circ}C$ for 30 minute. Three major compounds were identified as 1,3-dihydroxypropanone, 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrane-4-one and 5-hydroxymethylfurfural, and three minor compounds also as 5-methylfurfural, 2-acetylpyrrole and N,N-dimethylcyclohexamine, from ethyl acetate or methanol extracts on FFAP or HP-5MS capillary column.