• 제목/요약/키워드: mobile phase optimization

검색결과 37건 처리시간 0.02초

Optimization of the experimental conditions for determination of roxithromycin in bulk and dosage forms

  • Jeong, Kyung Min;Lee, Cheong Hoon;Kim, Su Hyun;Lee, Jeongmi
    • 분석과학
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    • 제30권1호
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    • pp.39-48
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    • 2017
  • Roxithromycin (RXT), which is an antibiotic used to treat respiratory tract and urinary infections, is official in Korean Pharmacopoeia (KP) and is marketed in various dosage forms including tablet, granule, suspension, and tablet for suspension in Korea. This study presents how a universal and reliable method to quantify RXT in bulk drug and formulations was developed. Effects of factors including column type, buffer concentration, type and concentration of organic solvent, buffer pH, and type and concentration of mobile phase additive, were examined, and some categorical or crucial factors including the types of column, organic solvent, mobile phase additive and the buffer pH were optimized by one-factor-at-a-time approach. Subsequently, concentrations of the buffer and additive and column temperature were optimized by response surface methodology using Box-Behnken design aiming to acquire the RXT peak of good shape. The optimized method employed a Phenomenex Gemini $5{\mu}$ C18 110A ($150{\times}4.60mm$, $5{\mu}m$) maintained at $30^{\circ}C$ with the mobile phase consisting of 25 mM phosphate buffer (pH 6.0) with 0.3 % tetrabutylammonium hydroxide and methanol at a ratio of 37:63 (v/v). Method validation results showed that the developed method was linear, precise, and accurate. Compared to the compendial methods in KP 10 that exhibited a significant tailing of the RXT peak despite using unfavorably high buffer concentrations and were not harmonized among bulk drug and formulations, this method could be universally applied to RXT bulk drug and marketed products in various dosage forms and thus was adopted in KP 11.

Optimization and validation of HPLC/DAD method for the determination of adenosine and cordycepin in cordyceps products

  • Sasikarn Panpraneecharoen;Tisorn Chatrakoon;Sompong Sansenya;Saowapa Chumanee
    • 분석과학
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    • 제36권4호
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    • pp.152-160
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    • 2023
  • Adenosine and cordycepin are bioactive compounds with health benefits. Therefore, both substances are often used to assess the quality of Cordyceps products. Optimization and validation of the HPLC/DAD method for determining two nucleosides were studied. The samples were prepared using an ultrasound-assisted extraction (ultrasonic bath). The result was optimal conditions for aqueous extraction, an extraction time of 35 min, and an extraction temperature of 40 ℃. The Chromatographic separation was achieved using a reverse phase column (InfinityLab Poroshell 120 EC-C18, 4.6 × 250 mm, 2.7 ㎛) at 30 ℃ with a mobile phase gradient elution of water and methanol at a flow rate of 0.7 mL/min. The eluents were monitored via a diode array detector at 260 nm. Two nucleosides were separated by less than 12 min after injection. The developed method was found to be excellent linear (r2 > 0.9999), accurate (% recovery 95.34-98.51), and precise (% relative standard deviation < 2.0). The limit of detection (LOD) and quantification (LOQ) were 0.45 and 1.38 mg/mL for adenosine and 0.47 and 1.43 mg/mL for cordycepin, respectively. This method was satisfactory for simultaneously quantitating two nucleoside contents, which were used to evaluate Cordyceps products.

CDMA 셀룰러 RF 시스템에서 교차변조 잡음 레벨 분석 및 최적화 (Analysis and Optimization of Cross-Modulation Noise in CDMA Cellular RF System)

  • 곽준호;김학선
    • 한국통신학회논문지
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    • 제28권6A호
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    • pp.397-404
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    • 2003
  • 본 논문에서는 CDMA 단말기에서 요구하는 교차변조 잡음의 레벨을 분석하고 최적설계를 위한 기준을 제시하였다. 표준안의 분석으로부터 교차변조 잡음의 레벨은 시스템 잡음지수와 VCO 위상잡음에 의해서 결정되며, 서로 트레이드-오프 관계에 있음을 확인하였다. 또한 시스템 설계 시 앞의 레벨을 만족시키기 위한 LNA의 IIP3와 듀플렉서의 격리도 값을 결정하였다. 따라서 본 논문은 cdma2000 단말기 설계 시 부품선정을 위한 기준이 될 것이다.

새로운 형태의 휴대폰용 브러쉬리스 센서리스 진동모터의 설계 (Novel Design of Brushless and Sensorless Vibration Motor Used for Cell-Phones)

  • 이홍주;김광석;이창민;황건용;황상문
    • 한국소음진동공학회:학술대회논문집
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    • 한국소음진동공학회 2008년도 춘계학술대회논문집
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    • pp.224-229
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    • 2008
  • With the wide use of mobile phones, a paging signal by a sound transducer acts as an environmental noise on many occasions, thus necessitating an alternative paging signal by a vibration motor. Conventional vibration motors employ three-phase windings with mechanical brushes for commutation. In this paper, a new one-phase brushless and sensorless vibration motor is introduced utilizing digital signal processor chips in cell-phones. For electromagnetic field analysis, two-dimensional modeling can be implemented to determine the back electromotive force using axisymmetric boundary conditions. Geometric design parameters, such as coil pitch and magnet pitch. are considered for performance optimization. Through the experiments, it is shown that the proposed design has the equivalent performance with reduced number of parts, thus enhancing manufacturing productivity and reducing manufacturing cost.

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Optimization of HPLC-tandem mass spectrometry for chlortetracycline using response surface analysis

  • Bae, Hyokwan;Jung, Hee-Suk;Jung, Jin-Young
    • Environmental Engineering Research
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    • 제23권3호
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    • pp.309-315
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    • 2018
  • Chlortetracycline (CTC) is one of the most important compounds in antibiotic production, and its distribution has been widely investigated due to health and ecological concerns. This study presents systematic approach to optimize the high-performance liquid chromatography-tandem mass spectrometry for analyzing CTC in a multiple reaction monitoring mode ($479{\rightarrow}462m/z$). One-factor-at-a-time (OFAT) test with response surface analysis (RSA) was used as optimization strategy. In OFAT tests, the fragmentor voltage, collision energy, and ratio of acetonitrile in the mobile phase were selected as major factors for RSA. The experimental conditions were determined using a composite in cube design (CCD) to maximize the peak area. As a result, the partial cubic model precisely predicted the peak area response with high statistical significance. In the model, the (solvent composition) and (collision $energy^2$) terms were statistically significant at the 0.1 ${\alpha}$-level, while the two-way interactions of the independent variables were negligible. By analyzing the model equation, the optimum conditions were derived as 114.9 V, 15.7 eV, and 70.9% for the fragmentor voltage, collision energy, and solvent composition, respectively. The RSA, coupled with the CCD, offered a comprehensive understanding of the peak area that responds to changes in experimental conditions.

A Range-Based Monte Carlo Box Algorithm for Mobile Nodes Localization in WSNs

  • Li, Dan;Wen, Xianbin
    • KSII Transactions on Internet and Information Systems (TIIS)
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    • 제11권8호
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    • pp.3889-3903
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    • 2017
  • Fast and accurate localization of randomly deployed nodes is required by many applications in wireless sensor networks (WSNs). However, mobile nodes localization in WSNs is more difficult than static nodes localization since the nodes mobility brings more data. In this paper, we propose a Range-based Monte Carlo Box (RMCB) algorithm, which builds upon the Monte Carlo Localization Boxed (MCB) algorithm to improve the localization accuracy. This algorithm utilizes Received Signal Strength Indication (RSSI) ranging technique to build a sample box and adds a preset error coefficient in sampling and filtering phase to increase the success rate of sampling and accuracy of valid samples. Moreover, simplified Particle Swarm Optimization (sPSO) algorithm is introduced to generate new samples and avoid constantly repeated sampling and filtering process. Simulation results denote that our proposed RMCB algorithm can reduce the location error by 24%, 14% and 14% on average compared to MCB, Range-based Monte Carlo Localization (RMCL) and RSSI Motion Prediction MCB (RMMCB) algorithm respectively and are suitable for high precision required positioning scenes.

용출곡선법과 Frontal Analysis를 이용한 Langmuir 흡착평형식의 측정 (Measurement of Langmuir Adsorption Equilibrium by Elution-curve Method and Frontal Analysis)

  • 최용석;이종호;노경호
    • 공업화학
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    • 제10권5호
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    • pp.672-676
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    • 1999
  • 흡착을 이용한 분리공정에서 가장 기본적인 것은 흡착평형식이다. 본 연구에서는 용출곡선법과 frontal analysis(FA)을 사용하여 용출곡선에서 직접 흡착평형식을 구하였다. 역상 액체 크로마토그래피(RP-HPLC)에서 시료는 5'-GMP이고 buffer로서 sodium phosphate를 물에 첨가하여 이동상으로 사용하였다. 이 실험조건에서는 시료의 양이 증가함에 따라서 체류시간이 감소하고 피크의 앞부분이 매우 경사가 심한 Langmuir 흡착평형식이 되었다. 용출곡선을 이용한 방법을 이용하여 Langmuir 흡착평형식의 매개변수를 최적화하여 구하였고 FA 방법을 이용하여 고정상의 농도를 용출곡선으로부터 측정하고 회귀분석에 의하여 흡착평형식을 측정하였다. FA 방법에 비해서 용출곡선법은 시료의 양이 적게 소모되고 실험 횟수도 1-2번 정도로 간편하였다. 이동상에 포함된 sodium phosphate의 농도에 따라서 Langmuir 흡착평형식의 매개변수에 미치는 영향을 고찰하였다.

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Optimal Resource Planning with Interference Coordination for Relay-Based Cellular Networks

  • Kim, Taejoon;An, Kwanghoon;Yu, Heejung
    • KSII Transactions on Internet and Information Systems (TIIS)
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    • 제11권11호
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    • pp.5264-5281
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    • 2017
  • Multihop relay-based cellular networks are attracting much interest because of their throughput enhancement, coverage extension, and low infrastructure cost. In these networks, relay stations (RSs) between a base station (BS) and mobile stations (MSs) drastically increase the overall spectral efficiency, with improved channel quality for MSs located at the cell edge or in shadow areas, and enhanced throughput of MSs in hot spots. These relay-based networks require an advanced radio resource management scheme because the optimal amount of radio resource for a BS-to-RS link should be allocated according to the MS channel quality and distribution, considering the interference among RSs and neighbor BSs. In this paper, we propose optimal resource planning algorithms that maximize the overall utility of relay-based networks under a proportional fair scheduling policy. In the first phase, we determine an optimal scheduling policy for distributing BS-to-RS link resources to RSs. In the second phase, we determine the optimal amount of the BS-to-RS link resources using the results of the first phase. The proposed algorithms efficiently calculate the optimal amount of resource without exhaustive searches, and their accuracy is verified by comparison with simulation results, in which the algorithms show a perfect match with simulations.

Characterization of degradation products of the Balsalazide by Mass spectrometry: Optimization of stability-indicating HPLC method for separation and quantification of process related impurities of Balsalazide

  • Chilakabattina Naga Narasimha Babu;Ch. Srinivasa Reddy;Bhagya Kumar Tatavarti;M. Radha Madhavi;Venkateswara Rao Anna
    • 분석과학
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    • 제37권1호
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    • pp.25-38
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    • 2024
  • The study aimed to investigate a novel approach by utilizing liquid chromatography (LC) and liquid chromatography-mass spectrometry (LC-MS) to separate, identify and characterize very nominal quantities of degradation products (DPs) of balsalazide along with its process related impurities without isolation from their reaction mixtures. The impurities along with balsalazide were resolved on spherisorb ODS2 (250×4.6 mm, 5.0 ㎛) column at room temperature using 0.2 M sodium acetate solution at pH 4.5 and methanol in the ratio of 55:45 (v/v) as mobile phase pumped isocratically at 1.0 mL/min as mobile phase and UV detection at 255 nm. The method shows sensitive detection limit of 0.003 ㎍/mL, 0.015 ㎍/mL and 0.009 ㎍/mL respectively for impurity 1, 2 and 3 with calibration curve liner in the range of 50-300 ㎍/mL for balsalazide and 0.05-0.30 for its impurities. The balsalazide pure compound was subjected to stress studies and a total of four degradation products (DPs) were formed during the stress study and all the DPs were characterized with the help of their fragmentation pattern and the masses obtained upon LC-MS/MS. The DPs were identified as 3-({4-[(E)-(4-hydroxyphenyl) diazenyl]benzoyl}amino)propanoic acid (DP 1), 4-[(E)-(4-hydroxyphenyl)diazenyl] benzamide (DP 2), 5-[(E)-(4-carbamoylphenyl)diazenyl]-2-hydroxybenzoic acid (DP 3) and 3-({4-[(E)-phenyldiazenyl]benzoyl}amino)propanoic acid (DP 4). Based on findings, it was concluded that, the proposed method was successfully applicable for routine analysis of balsalazide and its process related impurities in pure drug and formulations and also applicable for identification of known and unknown impurities of balsalazide.

최적 분석조건에 의한 강황으로부터 Curcuminoids의 고체상추출(SPE) (Solid Phase Extraction(SPE) of Curcuminoids from Turmeric by Optimization Analytical Condition)

  • 이광진;마진열;김영준;김영식
    • 한국산학기술학회논문지
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    • 제13권10호
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    • pp.4927-4935
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    • 2012
  • 강황은 다양한 약리활성을 가진 약초이다. 강황에 포함된 curcumin, demethoxycurcumin(DMC)과 bisdemethoxycurcumin(BDMC)을 침적과 초음파방법을 이용하여 추출하였다. 그리고 고체상추출(SPE)을 사용하여 추출효율을 확인 하였다. 추출액은 3가지 상업용 $C_{18}$ 역상 고성능 액체 크로마토그래피에 의해 이동상으로 물과 아세토나이트릴을 사용하여 일정용매법으로 동시분리 분석을 하였다. 유속은 1.0mL/min, 주입부피는 $10{\mu}L$, 컬럼오븐 온도 $40^{\circ}C$, 파장 425nm에서 수행되었다. 실험결과, RS tech column을 사용하고 물과 아세토나이트릴의 조성비가 (50 : 50vol%)일 때 최적 조건을 얻을 수 있었다. 용매조성(물과 메탄올)에 따른 추출 수율에의 영향을 살펴본 결과 100% 메탄올에서 curcuminoids(추출시간 4h)가 가장 많이 추출되었고, 수용성 메탄올 조성보다 함량이 높았다. 100% 물에 의해, 고체상추출은 curcuminoids의 추출함량(mAU${\times}$mim)이 침적과 초음파방법보다 24.5와 14.3배 높았다. 이상의 결과는 제약 및 기능성 소재로서의 응용 가능성을 나타내었다.