• Analytical Science and Technology
• /
• v.12 no.3
• /
• pp.203-208
• /
• 1999

The ion-pair high performance liquid chromatographic elution behavior of salicylic acid and its derivatives was studied with measuring capacity factor, k', changing the concentration of ion-pairing reagent (tetrabutylammonium chloride, TBACl) in mobile phase. As a result, it was found that k' of the samples increase at pH 7.2 as the TBACl concentration increases. The derivatives of salicylic acid were separated each other at an optimum mobile phase condition which was found from the observation of the retention behavior. The optimum mobile phase condition was methanol solution($MeOH:H_2O_2$ 30:70) containing 20 mM TBACl for the determination of salicylic acid and methanol solution($MeOH:H_2O_2$ 20:80) containing 40 mM TBACl for p-aminosalicylic acid at pH 7.2. The method has been applied for the analysis of the contents of salicylic acid derivatives in an aspirin tablet and a tuberculosis curing agent.

• Analytical Science and Technology
• /
• v.30 no.1
• /
• pp.39-48
• /
• 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.

• Journal of the Korean Chemical Society
• /
• v.53 no.2
• /
• pp.137-143
• /
• 2009

Liquid chromatographic enantiomer separation of N-tert-butoxycarbonyl (BOC) $\alpha$-amino acids and their ethyl esters was performed on covalently immobilized chiral column (Chiralpak IC) derived from polysaccharide derivative. The solvent versatility of the covalently immobilized Chiralpak IC in enantiomer separation of N-BOC $\alpha$-amino acid ethyl ester derivatives was shown and the chromatographic parameters of their enantioselectivities and resolution factors were greatly influenced by the nature of the mobile phase. Also the effect on the dissolving solvent for these analytes on the enantiomer separation using the same mobile phase and the examples of preparative enantiomer separation on analytical column were shown.

• KSBB Journal
• /
• v.18 no.4
• /
• pp.261-265
• /
• 2003

Ibuprofen was analyzed by chiral high performance liquid chromatography. Retention behaviours of the standard mixtures of ibuprofen were investigated to obtain their acceptable resolution. A chromatographic column (3.9 ${\times}$ 300 mm) was packed by Kromasil CHI-TBB packings (10 $\mu\textrm{m}$) and n-hexane was used as a mobile phase with 0.1％ acetic acid and tert-butyl methyl ether. Isocratic elution of ibuprofen at 1.0 $m\ell$/min was performed by changing the mobile phase compositions. The experimental variables affecting the resolution were the compositions of mobile phase and chemical buffer (n-hexane and tert-butyl methyl ether). The resolution between the enantiomers were correlated into the several types of empirical equations including linear form, and their agreements between experimental data and calculated values were examined by the regression coefficient.

• FOCUS: LIFE SCIENCE
• /
• no.1
• /
• pp.1.1-1.4
• /
• 2024

This article provides comprehensive guidance on the maintenance, cleaning, regeneration, and storage of silica-based HPLC (High-Performance Liquid Chromatography) columns. The general considerations emphasize the importance of using in-line filters and guard cartridges to protect columns from blockage and irreversible sample adsorption. While these measures help, contamination by strongly adsorbed sample components can still occur over time, leading to an increase in back pressure, loss of efficiency, and other issues. To maximize column lifetime, especially with UHPLC (Ultra-High Performance Liquid Chromatography) columns, it is advisable to use ultra-pure solvents, freshly prepared aqueous mobile phases, and to filter all samples, standards, and mobile phases. Additionally, an in-line filter system and sample clean-up on dirty samples are recommended. However, in cases of irreversible compound adsorption or column voiding, regeneration may not be possible. The document also provides specific recommendations for column cleaning procedures, including the flushing procedures for various types of columns such as reversed phase, unbonded silica, bonded normal phase, anion exchange, cation exchange, and size exclusion columns for proteins. The flushing procedures involve using specific solvents in a series to clean and regenerate the columns. It is emphasized that the flow rate during flushing should not exceed the specified limit for the particular column, and the last solvent used should be compatible with the mobile phase. Furthermore, the article outlines the storage conditions for silica based HPLC columns, highlighting the impact of storage conditions on the column's lifetime. It is recommended to flush all buffers, salts, and ion-pairing reagents from the column before storage. The storage solvent should ideally match the one used in the initial column test chromatogram provided by the manufacturer, and column end plugs should be fitted to prevent solvent evaporation and drying out of the packing bed.

• Journal of the Korean Institute of Telematics and Electronics A
• /
• v.31A no.9
• /
• pp.26-33
• /
• 1994

In this paper, the performance of the trellis coded CPFSK with the coherent detection over mobile communication channels is calculated. The characteristics of channels, including phase jitter effects and fading effects, are examined and modeled. The phase jitter channel is modeled to have a nonzero mean and a gaussian distribution. The fading channel has a Rayleigh distribution in the multipath. For the optimal decoding method(MLSE), the Viterbi algorithm is used for the trellis structure of trellis coded CPFSK. The results indicate that the trellis coded CPFSK with a small moulation indes gets more sensitive, as the index gets smaller, to the phase noise under the phase jitter channel. Using the interleaving method. It gives considerable improvements in the error rate under the fading channel.

• ETRI Journal
• /
• v.28 no.2
• /
• pp.227-230
• /
• 2006

There has been a growing need for increased capacity in cellular systems. This has resulted in the adoption of the code division multiple access (CDMA) system as a multiple channel access method. Thus, it is important to obtain the phase offsets of binary codes in the CDMA system because distinct phase offsets of the same code are used to distinguish signals received at the mobile station from different base stations. This letter proposes an efficient algorithm to compute the phase offset of a binary code in the CDMA system through the use of the basic facts of number theory and a new notion of the subcodes of a given code. We also formulate the algorithm in a compact form.

• Journal of the Korean Institute of Telematics and Electronics A
• /
• v.33A no.3
• /
• pp.152-162
• /
• 1996

Diffraction gratings were designed to generate multiple beams for the real-time optical interconnection in free-space using a liquid crsytal television. Multi-level phase gratings consisted of stepped phase value, 0 to 2$\pi$, and generate a 5$\times$5 spot array, and V-shaped spot patterns which have a maximum diffraction efficiency of 78.84%. Simulated annealing technique was used to determine phase states of each pixel having uniform intensity and high diffraction efficiency. Through the optical interconnection experiments, we compared the diffraction characteristics of beam paterns obtained by binary-level, four-level, and eight-level phase gratings.

• JSTS:Journal of Semiconductor Technology and Science
• /
• v.2 no.1
• /
• pp.41-48
• /
• 2002

This paper presents a 18-mW, 2.5-㎓ fractional-N frequency synthesizer with l-bit $4^{th}$-order interpolative delta-sigma ($\Delta{\;}$\sum$)modulator to suppress fractional spurious tones while reducing in-band phase noise. A fractional-N frequency synthesizer with a quadruple prescaler has been designed and implemented in a $0.5-\mu\textrm{m}$ 15-GHz $f_t$ BiCMOS. Synthesizing 2.1 GHzwith less than 200 Hz resolution, it exhibits an in-band phase noise of less than -85 dBc/Hz at 1 KHz offset frequency with a reference spur of -85 dBc and no fractional spurs. The synthesizer also shows phase noise of -139 dBc/Hz at an offset frequency of 1.2 MHz from a 2.1GHz center frequency.

• Analytical Science and Technology
• /
• v.5 no.4
• /
• pp.389-399
• /
• 1992

Liquid Chromatographic behavior of Pd(II) in Isonitrosoethylacetoacetate lmine, $Pd(IEAA-NR)_2$ (R=H, $CH_3$, $C_2H_5$, $n-C_3H_7$, $C_6H_5-CH_2$, $n-C_4H_9$) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of $Pd(IEAA-NR)_2$ chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It wass found that metal chelates were properly eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the logarithm of capacity factor(k') on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extration distribution ratio($D_c$) in methanol-water/n-alkane extration system was investigated. Both kinds of dependence are linear, which susggests that the retention of the electroneutral metal chelate is largely due to the solvophobic effect. Standard adsorption enthalpy changes (${\Delta}H^{\circ}$) and standard adsorption entropy changes (${\Delta}S^{\circ}$) of Pd(II) Isonitrosoethylacetoacetate imine chelates on Micropak MCH-5 column were calculated by measuring capacity factor with changing temperature of the column.