• Title/Summary/Keyword: simultaneous recovery

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Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample

  • Kim, Nam Sook;Yoo, Geum Joo;Kim, Kyu Yeon;Lee, Ji Hyun;Park, Sung-Kwan;Baek, Sun Young;Kang, Hoil
    • Analytical Science and Technology
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    • v.32 no.2
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    • pp.35-47
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    • 2019
  • In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

Analysis of Co-movement and Causality between Supply-Demand Factors and the Shipping Market: Evidence from Wavelet Approach (웨이블릿 분석을 통한 수요-공급요인과 해운시황의 연관성 분석)

  • Jeong, Hoejin;Yun, Heesung;Lee, Keehwan
    • Journal of Korea Port Economic Association
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    • v.38 no.3
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    • pp.87-104
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    • 2022
  • Considering the complex structure and high volatility in the shipping market, it is important to investigate the connectedness amongst influencing factors. This study explores the dynamic relationship between supply-demand factors and shipping freight indices. We choose Capesize and Panamax in the bulk carrier market and use quarterly data of GDP, world fleet, BCI, and BPI from 1999 to 2021. Applying the wavelet analysis and wavelet Granger causality test, the simultaneous examination of co-movement and causality between two factors and the shipping market in both the time and frequency domains is achieved. We find that co-movement and causality vary across time and frequencies, thereby existing dynamic relationships between variables. Second, compared to multiple coherencies using demand and supply factors together, partial coherencies indicate noticeable causalities. It implies that analyzing demand and supply factors separately is essential. Finally, shipping freight indices show a high correlation with the demand factor in a good market and with the supply factor in a bad market. Generally, GDP positively leads shipping freights in the recovery phase while the world fleet negatively leads shipping freights in the downturn. The research is meaningful in that the rarely-applied wavelet analysis is adopted in the shipping market and that it gives a reasonable ground to explain the role of supply and/or demand factors in different phases of the market cycle.

A sensitive analytical method for determination of 3-monochloropropane-1,2-diol and 1,3-dichloropropan-2-ol in various foods by gas chromatography with mass spectrometer (가스크로마토그래피/질량분석기를 이용한 식품 중 클로로프로판올 화합물 분석)

  • Kim, Eunju;Park, Sungkug;Choi, Dongmi
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.543-552
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    • 2008
  • This paper described the relatively sensitive and simultaneous analytical method for 3-monochloropropane-1,2-diol (3-MCDP, $C_3H_7ClO_2$, MW. 110) as well as 1,3-dichloropropan-2-ol (1,3-DCP, $C_3H_6Cl_2O$, MW. 128) in various foods. Food samples were homogenized in 5M NaCl solution, mixed with aluminum oxide and eluted with dichloromethane. The extracted chloropropanols were concentrated by rotary evaporator and $N_2$ blow serially were derivatized with HFBA (Heptafluorobutyric anhydride, $C_8F_{14}O_3$, MW. 410) and were determined by GC/MS using isotope dilution method. The characteristic molecular ions at m/z 253, 275, 289, 291, and 453 for HFBA derivatives of 3-MCPD (MW. 502) and 110, 275, and 277 for HFBA derivatives of 1,3-DCP (MW. 325) were chosen in selected ion mode. The method validation data showed sufficiently good properties of LOD (0.003 mg/kg), LOQ (0.010 mg/kg), linearity ($R^2{\geq}0.999$ at 0.010~1.000 mg/kg), and recovery rate (${\approx}97%$). The levels of chloropropanols in soy sauce, sauces, processed meat products, fishery products, and seasonings (n=56/157) determined by the presented method were 0.0~0.3 mg/kg.

University Hospital Nurses' Experience of a Music-Based Online Burnout Prevention Program: A Qualitative Case Study (대학병원 간호사의 소진예방을 위한 비대면 음악기반 심리정서지원 프로그램 참여경험 연구)

  • Yun, Juri;Lee, Jin Hyung
    • Journal of Music and Human Behavior
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    • v.21 no.2
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    • pp.135-157
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    • 2024
  • In this study, the authors developed and implemented an online music-based support program to prevent burnout among university hospital nurses. This study involved 40 nurses from three university hospitals who shared their subjective experiences after participating in 8 music-based non-simultaneous online sessions. The responses were collected as qualitative data and analyzed using the qualitative content analysis method. The analysis identified 66 meaning units, 10 themes, and 3 categories, which included: 'Recovery of physical and psychological stability', 'Self-care and acceptance', and 'Rediscovery of pride and meaning as a nurse'. This study is significant for exploring the experiences of university hospital nurses who participated in a remotely implemented music-based psycho-emotional support program, with respect to burnout prevention. For future directions, we suggest a more in-depth exploration of specific burnout factors and an expansion of research through the diversification of research methods to refine programs aimed at alleviating nurse burnout.

Practical Applications of DNA Marker-Assisted Selection and OPU-Derived IVF Embryo Transfer for the Production of High Quality Meat in Hanwoo I. Collection of Follicular Oocytes with Ultrasound-Guided Transvaginal Ovum Pick-Up from DNA Marker-proved Hanwoo (유전자 분석을 통하여 선발된 한우로부터 초음파 유래 체외수정란 이식에 의한 고품질 한우 생산기술의 실용화 I. DNA 검정우에서 초음파기기를 이용한 난포란의 채란에 관한 연구)

  • 박희성;이지삼;진종인;박준규;홍승표;이명열;정장용
    • Journal of Embryo Transfer
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    • v.16 no.3
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    • pp.183-191
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    • 2001
  • This study was designed to establish the superior method for IVF embryos from DNA marker-proved Hanwoo cattle. DNA markers related to marbling score were identified using DNA fingerprinting with Ml3 probe and restriction enzyme Hae III. Oocytes were aspirated from unstimulated. immature ovarian follicles using a combined method of rectal ovarian-palpation and transvaginal ultrasound-guidance(6.5MHz) under local abesthesia. The aspirated oocytes were washed twice with fresh D-PBS containing 5% FBS and were rewashed 4 to 5 times with TCM-199 containing 5% FBS. A morphological grade of I to IV was assigned to each oocyte. Data were analysed using the GLM procedure of SAS. Mean number of follicles identified on ultrasound was 5.5 $\pm$2.9 in right and 4.3 $\pm$2.8 in left ovaries, respectively. The highest follicles(16.6$\pm$2.6) were found in 5101 cow compared to others. Recovery rate of follicular oocytes in individual cow was highest in 5101 cow with 89.3% in > 2mm and 94.0% in $\leq$ 2mm follicles. Total recovery rate was significantly(P<0.01) higher in $\leq$ 2mm(85.7%, 130/154) than > 2mm follicles(74.2%, 201/271). Significantly more oocytcs of Grade IV were recovered from > 2mm follicles. Mean number follicles recovered was 4.8$\pm$3.7. 3.0$\pm$3.4 and 0.3$\pm$0.6 in $\leq$2mm, 2~6mm and $\geq$6mm follicles. respectively. Our results imply that the more fertilizablc oocytes can be recovered from invisible-immature follicles by the combination of simultaneous rectal ovarian-palpation and ultrasound-guided approach in Hanwoo cattle.

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Development of Analytical Methods of Spinosad in Agricultural Commodities by HPLC with UV Detector and Monitoring (HPLC-UVD를 이용한 농산물 중 스피노사드 분석법 개선 및 잔류실태 조사)

  • Kim, Hee-Yun;Choi, Sun-Hee;Chung, So-Young;Choi, Hee-Ju;Kim, Yong-Hoon;Cho, Min-Ja;Seo, Eun-Chae;Han, Kyoung-Jin;Choi, Jae-Chun;Park, Hee-Ok;Ha, Sang-Chul;Shin, Il-Shik;Eom, Ji-Yoon
    • Korean Journal of Food Science and Technology
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    • v.43 no.2
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    • pp.125-133
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    • 2011
  • The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

Simultaneous Separation and Determination of $^{l4}C\;and\;^3H$ in Spent Resins from PWR Nuclear Power Plants (가압경수로형 원전에서 발생된 폐수지의 $^{14}C$$^3H$ 동시 분리 및 측정)

  • Park, Soon-Dal;Kim, Jung-Suck;Kim, Jong-Goo;Han, Sun-Ho;Jee, Kwang-Yong
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.5 no.3
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    • pp.179-188
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    • 2007
  • In this work $^{14}C\;and\;^3H$ distribution characteristics of spent resins from nuclear power plants(NPPs), pressurized water reactors(PWRs), was investigated. It was found that the recovery percent of $^{14}C$ by the wet oxidation-acid stripping was $81%{\sim}100%$ for the added activity range of $^{14}C,\;0.72\;Bq{\sim}460\;Bq$, and it was not affected by the kinds of stripping acids, 3N-HCl, $3\;N-HNO_3\;and\;3\;N-H_2SO_4$. And the recovery percent of $^3H$ by distillation using the same apparatus was $81%{\sim}101%$ for the added activity range of $^3H,\;0.60\;Bq{\sim}435\;Bq$. Among the tested stripping acids, 3\;N-HCl, $3\;N-HNO_3\;and\;3\;N-H_2SO_4$, only the trapped $^3H$ solution by distillation in $3\;N-H_2SO_4$ was compatible with the 3H scintillator, Ultimagold XR. Neither of the $^{14}C\;and\;^3H$ trapping solutions from the spent ion exchange resin samples by the wet oxidation-3 $N-H_2SO_4$ stripping contained gamma nuclides. However, some gamma nuclides, $^{60}Co,\;^{134}Cs,\;^{137}Cs\;and\;^{54}Mn$, were found in the trapped $^3H$ solutions of the spent resins by the wet oxidation-3 N-HCl stripping. It was the same for the $^3H$ trapping solutions of the spent resins by Sample Oxidizer(PACKARD MODEL 307). Meanwhile only two nuclides, $^{134}Cs,\;and\;^{134}Cs$, were found in the $^{14}C$ trapping solutions of the spent resins by Sample Oxidizer(PACKARD MODEL 307). It was found that most of the $^{14}C$ in the spent resins existed as inorganic carbon form, more than about 70% of the total $^{14}C$ content. Among the analyzed 30 spent ion exchange resin samples, the average concentration of $^{14}C$ and $^3C$ for the high radioactive samples, 8 samples, was $19000\;Bq/g{\pm}41000\;Bq/g,\;670\;Bq/g{\pm}460\;Bq/g$ and that for the low radioactive samples, 22 samples, was $4.2\;Bq/g{\pm}4.3\;Bq/g,\;6.0\;Bq/g{\pm}5.3\;Bq/g$, respectively. And the average $^{14}C/^3H$ ratio for the high radioactive samples, was higher, 28, than that of low radioactive samples, 0.70. Some linear relationship trend was found between the activity concentrations of $^{14}C\;and\;^3H$.

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Validation of a Rapid Quantitative Method for the Residues of Nitrofuran Metabolites in Loach by Accelerated Solvent Extraction and HPLC Triple Quadrupole Mass Spectrometry

  • Ryu, Eun Chae;Han, Yun-jeong;Park, Seong-soo;Lim, Chul-joo;Choi, Sunok;Park, Se Chang
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.85-93
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    • 2016
  • A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Kim, Ji-Young;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.124-134
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    • 2019
  • An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

Recent Progress in Air-Conditioning and Refrigeration Research : A Review of Papers Published in the Korean Journal of Air-Conditioning and Refrigeration Engineering in 2016 (설비공학 분야의 최근 연구 동향 : 2016년 학회지 논문에 대한 종합적 고찰)

  • Lee, Dae-Young;Kim, Sa Ryang;Kim, Hyun-Jung;Kim, Dong-Seon;Park, Jun-Seok;Ihm, Pyeong Chan
    • Korean Journal of Air-Conditioning and Refrigeration Engineering
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    • v.29 no.6
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    • pp.327-340
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    • 2017
  • This article reviews the papers published in the Korean Journal of Air-Conditioning and Refrigeration Engineering during 2016. It is intended to understand the status of current research in the areas of heating, cooling, ventilation, sanitation, and indoor environments of buildings and plant facilities. Conclusions are as follows. (1) The research works on the thermal and fluid engineering have been reviewed as groups of flow, heat and mass transfer, the reduction of pollutant exhaust gas, cooling and heating, the renewable energy system and the flow around buildings. CFD schemes were used more for all research areas. (2) Research works on heat transfer area have been reviewed in the categories of heat transfer characteristics, pool boiling and condensing heat transfer and industrial heat exchangers. Researches on heat transfer characteristics included the results of the long-term performance variation of the plate-type enthalpy exchange element made of paper, design optimization of an extruded-type cooling structure for reducing the weight of LED street lights, and hot plate welding of thermoplastic elastomer packing. In the area of pool boiling and condensing, the heat transfer characteristics of a finned-tube heat exchanger in a PCM (phase change material) thermal energy storage system, influence of flow boiling heat transfer on fouling phenomenon in nanofluids, and PCM at the simultaneous charging and discharging condition were studied. In the area of industrial heat exchangers, one-dimensional flow network model and porous-media model, and R245fa in a plate-shell heat exchanger were studied. (3) Various studies were published in the categories of refrigeration cycle, alternative refrigeration/energy system, system control. In the refrigeration cycle category, subjects include mobile cold storage heat exchanger, compressor reliability, indirect refrigeration system with $CO_2$ as secondary fluid, heat pump for fuel-cell vehicle, heat recovery from hybrid drier and heat exchangers with two-port and flat tubes. In the alternative refrigeration/energy system category, subjects include membrane module for dehumidification refrigeration, desiccant-assisted low-temperature drying, regenerative evaporative cooler and ejector-assisted multi-stage evaporation. In the system control category, subjects include multi-refrigeration system control, emergency cooling of data center and variable-speed compressor control. (4) In building mechanical system research fields, fifteenth studies were reported for achieving effective design of the mechanical systems, and also for maximizing the energy efficiency of buildings. The topics of the studies included energy performance, HVAC system, ventilation, renewable energies, etc. Proposed designs, performance tests using numerical methods and experiments provide useful information and key data which could be help for improving the energy efficiency of the buildings. (5) The field of architectural environment was mostly focused on indoor environment and building energy. The main researches of indoor environment were related to the analyses of indoor thermal environments controlled by portable cooler, the effects of outdoor wind pressure in airflow at high-rise buildings, window air tightness related to the filling piece shapes, stack effect in core type's office building and the development of a movable drawer-type light shelf with adjustable depth of the reflector. The subjects of building energy were worked on the energy consumption analysis in office building, the prediction of exit air temperature of horizontal geothermal heat exchanger, LS-SVM based modeling of hot water supply load for district heating system, the energy saving effect of ERV system using night purge control method and the effect of strengthened insulation level to the building heating and cooling load.