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Liquid Chromatography Quadrupole Time-Of-Flight Tandem Mass Spectrometry for Selective Determination of Usnic Acid and Application in Pharmacokinetic Study

  • Fang, Minfeng;Wang, Hui;Wu, Yang;Wang, Qilin;Zhao, Xinfeng;Zheng, Xiaohui;Wang, Shixiang;Zhao, Guifang
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1684-1688
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    • 2013
  • A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.

Measurement of Mutual Solubility of High-pressure Gaseous Fire Extinguishing Agents(HFCs) and Nitrogen (고압가스계 소화약제(HFCs계열)와 질소의 상호용해도 측정)

  • 임종성;박지영;이병권;김재덕;이윤용
    • Fire Science and Engineering
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    • v.16 no.3
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    • pp.26-31
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    • 2002
  • Bromotrifluoromethane(halon-1301) and bromochlorodifluoromethane(halon-1211) have been widely used as a clean fire extinguishing agents due to their outstanding properties. However, production and use of halon are currently being phased out under an international agreements Montreal Protocol because of global environmental concerns and HFCs have been considered as promising alter-natives for the replacement of halon since their ozone depletion potentials are low. The vapor-liquid equilibrium data are required as important basic information in evaluating the solubility of clean fire extinguishing agents and determining their optimal compositions. In this work, we chose HFCs such as HFC-22 HFC-125, and HFC-l34a for gaseous fire extinguishing agents and nitrogen as a pressurization gas for a proper jet velocity of these agents. Phase equilibria for binary mixtures of nitrogen/HFC-22, nitrogen/HFC-125, and nitrogen/HFC-l34a were measured in the temperature range from 283.15K to 303.15K. For equilibrium measurement, we used a circulation type apparatus in which both vapor and liquid phases were continuously recirculated. The experimental data were relatively well correlated with the Peng-Robinson equation of state with Wong-Sandier mixing rules.

Establishment of Analytical Method for Pencycuron in Representative Agricultural Commodities by High-Performance Liquid Chromatography (대표 농산물 중 살균제 Pencycuron의 HPLC 정밀 잔류분석법 개발)

  • Lee, Hyeri;Choi, Hoon;Kim, Byung-Joon;Kim, Eunhye;Kim, Su-Hee;Lee, Jin-Beom;Lee, Young Deuk;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.21 no.1
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    • pp.75-83
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    • 2017
  • The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

Development of validated Nursing Interventions for Home Health Care to Women who have had a Caesarian Delivery (조기퇴원 제왕절개 산욕부를 위한 가정간호 표준서 개발)

  • HwangBo, Su-Ja
    • Journal of Korean Academy of Nursing Administration
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    • v.6 no.1
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    • pp.135-146
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    • 2000
  • The purpose of this study was to develope, based on the Nursing Intervention Classification (NIC) system. a set of standardized nursing interventions which had been validated. and their associated activities. for use with nursing diagnoses related to home health care for women who have had a caesarian delivery and for their newborn babies. This descriptive study for instrument development had three phases: first. selection of nursing diagnoses. second, validation of the preliminary home health care interventions. and third, application of the home care interventions. In the first phases, diagnoses from 30 nursing records of clients of the home health care agency at P. medical center who were seen between April 21 and July 30. 1998. and from 5 textbooks were examined. Ten nursing diagnoses were selected through a comparison with the NANDA (North American Nursing Diagnosis Association) classification In the second phase. using the selected diagnoses. the nursing interventions were defined from the diagnoses-intervention linkage lists along with associated activities for each intervention list in NIC. To develope the preliminary interventions five-rounds of expertise tests were done. During the first four rounds. 5 experts in clinical nursing participated. and for the final content validity test of the preliminary interventions. 13 experts participated using the Fehring's Delphi technique. The expert group evaluated and defined the set of preliminary nursing interventions. In the third phases, clinical tests were held at in a home health care setting with two home health care nurses using the preliminary intervention list as a questionnaire. Thirty clients referred to the home health care agency at P. medical center between October 1998 and March 1999 were the subjects for this phase. Each of the activities were tested using dichotomous question method. The results of the study are as follows: 1. For the ten nursing diagnoses. 63 appropriate interventions were selected from 369 diagnoses interventions links in NlC., and from 1.465 associated nursing activities. From the 63 interventions. the nurses expert group developed 18 interventions and 258 activities as the preliminary intervention list through a five-round validity test 2. For the fifth content validity test using Fehring's model for determining lCV (Intervention Content Validity), a five point Likert scale was used with values converted to weights as follows: 1=0.0. 2=0.25. 3=0.50. 4=0.75. 5=1.0. Activities of less than O.50 were to be deleted. The range of ICV scores for the nursing diagnoses was 0.95-0.66. for the nursing interventions. 0.98-0.77 and for the nursing activities, 0.95-0.85. By Fehring's method. all of these were included in the preliminary intervention list. 3. Using a questionnaire format for the preliminary intervention list. clinical application tests were done. To define nursing diagnoses. home health care nurses applied each nursing diagnoses to every client. and it was found that 13 were most frequently used of 400 times diagnoses were used. Therefore. 13 nursing diagnoses were defined as validated nursing diagnoses. Ten were the same as from the nursing records and textbooks and three were new from the clinical application. The final list included 'Anxiety', 'Aspiration. risk for'. 'Infant behavior, potential for enhanced, organized'. 'Infant feeding pattern. ineffective'. 'Infection'. 'Knowledge deficit'. 'Nutrition, less than body requirements. altered', 'Pain'. 'Parenting'. 'Skin integrity. risk for. impared' and 'Risk for activity intolerance'. 'Self-esteem disturbance', 'Sleep pattern disturbance' 4. In all. there were 19 interventions. 18 preliminary nursing interventions and one more intervention added from the clinical setting. 'Body image enhancement'. For 265 associated nursing activities. clinical application tests were also done. The intervention rate of 19 interventions was from 81.6% to 100%, so all 19 interventions were in c1uded in the validated intervention set. From the 265 nursing activities. 261(98.5%) were accepted and four activities were deleted. those with an implimentation rate of less than 50%. 5. In conclusion. 13 diagnoses. 19 interventions and 261 activities were validated for the final validated nursing intervention set.

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Disturbance of $\alpha$-Amylase Secretion from Bacillus amyloliquefaciens Cells by the Treatment of Puromycin and Magnesium (Bacillus amyloliquefaciens에서 Puromycin 과 Magnesium에 의한 $\alpha$-Amylase 의 분비저해)

  • 안순자;김순옥;이동희;송방호
    • Microbiology and Biotechnology Letters
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    • v.17 no.5
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    • pp.412-420
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    • 1989
  • To know how the ribosomes involved in secretory protein synthesis were attached to the cytoplasmic membrane in Bacillus amyloliquefaciens, the cells were treated with puromycin combinated with magnesium at the logarithmic phase, and the variation of cell-bound and extracellular $\alpha$-amylase activity was assayed for determining the $\alpha$-amylase translocation blocking through the cytoplasmic membrane. In the abnormal $\alpha$-amylase producing mutant in which the C-terminal of the $\alpha$-amylase structure was deleted, B. umytotiquefaciens CH10-2, the $\alpha$-amylase was translocated normally through the cytoplasmic membranes, and the translocation blocking by puromycin was revealed to have a similar pattern as that in the wild type. This means that the C-terminal part of the enzyme structure may not have a signal for secretion. The cell death of the logarithmic phase cells in both strains was not affected much under 20$\mu\textrm{g}$/$m\ell$ of puromycin, however, the $\alpha$-amylase translocation was blocked markedly under less than 10$\mu\textrm{g}$/$m\ell$ of the puromycin concentration. The blocking of the enzyme secretion by puromycin may be due to the detachment of the ribosomes from cytoplasmic membranes by disturbing the nascent polypeptide synthesis. Further evidence for confirming this was that the detachment was increased in 50 mM of magnesium ion because the extracellular $\alpha$-amylase activity was decreased more under this condition. If the cells were treated with trypsin combinated with Iysozyme, the extracellular $\alpha$-amylase activity from the cultured medium was reduced markedly, however, the activity from the cells treated with trypsin only was not reduced. This means that the nascent polypeptides protruding from the cytoplasmic membrane were sensitive to the trypsin digestion, whereas the matured ones were not. Therefore, the protruding polypeptides from the cytoplasmic membranes may be truncated by trypsin before forming their final tertiary structures by folding in the cell wall layer.

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Nicardipine Hydrochloride Injectable Phase IV Clinical Trial-Study on the antihypertensive effect and safely of nicardipine for acute aortic dissection (급성대동맥해리에 대한 혈압강하요법으로서의 Nicardipine.HCI 주사액(Perdipine$^{circledR}$)의 유효성 및 안전성을 검토하기 위한 다기관 공동, 공개 제4상 임상시험)

  • Kim, Kyung-Hwan;Moon, In-Sung;Park, Jang-Sang;Koh, Yong-Bok;Ahn, Hyuk
    • Journal of Chest Surgery
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    • v.35 no.4
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    • pp.267-273
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    • 2002
  • Background: We performed a phase IV clinical trial to examine the usefulness of a continuous infusion of nicardipine hydrochloride to control hypertension in patients with acute aortic dissection. material and Method: Systolic/diastolic blood pressure, and heart rate were monitored before and after the intravenous administration of nicardipine in 31 patients with aortic diseases. The period of nicardipine administration in each patient was from 3 to 14 days. Efficacy was evaluated by determining the average amount of blood pressure reduction on the 3rd day of drug administration. The dosage of another antihypertensive agent was slowly tapered down, and ultimately replaced by the test drug. Result: 28 patients were diagnosed as acute aortic dissection, 2 patients as rupture of the aortic arch aneurysm, and 1 patient as traumatic aortic rupture. Mean age was 53.9 $\pm$ 14.9(29~89) years, and 21 patients(67.7%) were male. 14 patients(32.3%) had complications associated with underlying aortic disease: aortic insufficiency in 7, hemopericardium in 6, acute renal failure in 1, paraplegia in 1, lower extremity ischemia in 1, and hemothorax in 1. The time needed to reach the target blood pressure was within 15 minutes in 16, from 15 to 30 minutes in 10, from 30 to 45 minutes in 3 and from 45 to 60 minutes in 2, and their baseline average systolic, diastolic, and mean arterial blood pressures(mmHg) were 147$\pm$23, 82.3$\pm$ 18.6, and 104 $\pm$ 18, respectively. Average systolic, diastolic, and mean arterial blood pressures(mmHg) on the third day of nicardipine infusion were 119$\pm$ 12, 69$\pm$9, and 86$\pm$8, and they all showed statistically significant decrease(p<0.05). The average systolic, diastolic, and mean arterial blood pressure(mmHg) after the discontinuation of the nicardipine infusion were 119 $\pm$ 15, 71 $\pm$ 14, and 86$\pm$ 13, respectively. No significant difference was observed between the average pressures measured on the third day and those measured after the discontinuation of the nicardipine infusion, and no definite side effects were observed during the study period. Conclusion: Nicardipine hydrochloride was both effective and safe at controlling blood pressure in patients with acute aortic dissection.

Analysis of Fungicide Prochloraz in Platycodi Radix by GC-ECD (GC-ECD를 이용한 한약재 길경(Platycodi Radix) 중 살균제 Prochloraz의 분석)

  • Oh, Gyeong-Seok;Yoon, Myung-sub;Yang, Seung-Hyun;Choi, Hoon
    • Korean Journal of Environmental Agriculture
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    • v.40 no.4
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    • pp.353-358
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    • 2021
  • BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quantitative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were converted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were extracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was decomposed to 2,4,6-T, and then the partitioned ion-associate was finally purified by optimized aminopropyl solid-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (82.1-89.7%). Good reproducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were reasonable (r2 > 0.9986) in the range of 0.005-0.5 ㎍/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines required for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.

Analysis of Quantization Noise in Magnetic Resonance Imaging Systems (자기공명영상 시스템의 양자화잡음 분석)

  • Ahn C.B.
    • Investigative Magnetic Resonance Imaging
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    • v.8 no.1
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    • pp.42-49
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    • 2004
  • Purpose : The quantization noise in magnetic resonance imaging (MRI) systems is analyzed. The signal-to-quantization noise ratio (SQNR) in the reconstructed image is derived from the level of quantization in the signal in spatial frequency domain. Based on the derived formula, the SQNRs in various main magnetic fields with different receiver systems are evaluated. From the evaluation, the quantization noise could be a major noise source determining overall system signal-to-noise ratio (SNR) in high field MRI system. A few methods to reduce the quantization noise are suggested. Materials and methods : In Fourier imaging methods, spin density distribution is encoded by phase and frequency encoding gradients in such a way that it becomes a distribution in the spatial frequency domain. Thus the quantization noise in the spatial frequency domain is expressed in terms of the SQNR in the reconstructed image. The validity of the derived formula is confirmed by experiments and computer simulation. Results : Using the derived formula, the SQNRs in various main magnetic fields with various receiver systems are evaluated. Since the quantization noise is proportional to the signal amplitude, yet it cannot be reduced by simple signal averaging, it could be a serious problem in high field imaging. In many receiver systems employing analog-to-digital converters (ADC) of 16 bits/sample, the quantization noise could be a major noise source limiting overall system SNR, especially in a high field imaging. Conclusion : The field strength of MRI system keeps going higher for functional imaging and spectroscopy. In high field MRI system, signal amplitude becomes larger with more susceptibility effect and wider spectral separation. Since the quantization noise is proportional to the signal amplitude, if the conversion bits of the ADCs in the receiver system are not large enough, the increase of signal amplitude may not be fully utilized for the SNR enhancement due to the increase of the quantization noise. Evaluation of the SQNR for various systems using the formula shows that the quantization noise could be a major noise source limiting overall system SNR, especially in three dimensional imaging in a high field imaging. Oversampling and off-center sampling would be an alternative solution to reduce the quantization noise without replacement of the receiver system.

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Australian Case Study in Regulatory Techniques to the Security Industry Reform and Policy Implications (호주 민간경비산업 고품질 규제수단 검토 및 시사점)

  • Kim, Dae-Woon
    • Korean Security Journal
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    • no.47
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    • pp.7-36
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    • 2016
  • The security providers industry, often referred to as an industry with unconfined growth ceiling, has entered a remarkable mass-growth phase since the 1980. In the modern era, private-sector security increasingly cover functions relating to general security awareness (including counter-terrorism) in partnership with State bodies, and the scale of operations continue to accelerate, relative to the expanding roles. In the era of pluralisation of policing, there has been widening efforts pursued to develop a range of regulatory strategies internationally in order to manage such growth and development. To date, in South Korea, a diverse set of industry review studies have been conducted. However, the analyses have been conventionally confined to North America, Britain, Germany and Japan, while developments in other world regions remain unassessed. This article is intended to inform the drivers and determinants of regulatory reforms in Australia, and examine the effectiveness of the main pillars of licensing innovations. Over the past decades, the Australian regime has undergone a wave of reforms in response to emerging issues, and in recognition of the industry as a 'public good' due to underpopulation density and the resulting security challenges. The focus of review in this study was on providing a detailed review of the regulatory approach taken by Australia that has expanded police-private security co-operation since the 1980s. The emphasis was on examining the core pillars of risk management strategies and oversight practices progressed to date and evaluating areas of possible improvement in regulation relative to South Korea. Overall, this study has identified three key features of Australian regime: (1) close checks on questionable close associates (including fingerprinting), (2) power of inspection and seizure without search warrant, (3) the 'three strikes' scheme. The rise of the private security presence in day-to-day policing operations means that industry warrant some intervening government-sponsored initiative. The overall lessons learnt from the Australian case was taken into account in determining the following checks and balances that would provide the ideal setting for the best-practice arrangement: (1) regulatory measure should be evaluated against a set of well-defined indicators, such as the merits of different enforcement tools for each given risk, (2) information about regulatory impacts should be analysed by a specialist research institute, (3) regulators should be innovative in applying a range of strategies available to them by employing a mixture of compliance promotional strategies, and adjust the mix as required.

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An Empirical Analysis of the Effects of Startup' Activities of Preparatory Stage and Early Stage on Performance (창업기업의 준비 및 초기단계 활동들이 기업 성과에 미치는 영향에 관한 연구)

  • Yoon, Byeong seon;Seo, Young wook
    • Asia-Pacific Journal of Business Venturing and Entrepreneurship
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    • v.11 no.4
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    • pp.1-15
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    • 2016
  • Startups in Korea are experiencing for themselves the laws of survival through competition in the local and international market, and are performing active business movements based on these. Korea's economic growth rate is 2.6% due to the slump in the domestic demand and reduced exports brought by the MERSC incident in 2015. The Korea Development Institute has estimated the economic growth rate in 2016 to be around 3.0%. South Korea's economy is facing the crisis of low-growth solidification due to the decrease in economic growth, and it is forecasted that growth without employment and polarization will worsen. Startups in the high-tech industrial generation of a particular field wherein the market environment is rapidly changing must maintain a competitive advantage with the capabilities and functions exclusive to them. It is very important that they maintain a competitive edge by utilizing the capabilities exclusive to startup companies. Likewise, the accumulation of resources is also crucial in determining the success of a startup business. In a poor local startup ecosystem, majority of the startup companies are performing their business activities while striving for survival, rather than success. About 80% are struggling to survive and are failing to overcome the "Death Valley" faced 3-5 years after establishing the company. Since majority of the startups fail to achieve results during the initial stages of foundation, the importance of research on business activities and achievement during the early stages of establishment is being raised. In accordance to this, this research has performed an actual analysis on how the activities of startups during their preparation phase and early stages affect their achievements. A survey was done on the CEOs or executives (people in a position to make decisions) of local small and medium-sized enterprises that are considered start-ups, and 203 valid data were collected and analyzed. Results showed that the discoveries and utilized activities necessary for the businesses of startups have a significant impact on their achievement through the entrepreneur resources and external partners' cooperation; additionally, the related implications were discussed.

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