• YAKHAK HOEJI
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• v.57 no.4
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• pp.272-281
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• 2013

In this study, we developed and validated the HPLC method using the isolated components from Erycibae caulis. Their structures were elucidated by spectroscopic methods including UV, $^1H$-NMR, $^{13}C$-NMR, FAB-Mass and ESI-Mass as Compound 1 (crypto-chlorogenic acid), Compound 2 (scopolin), Compound 3 (neochlorogenic acid) and Compound 4 (3,4-di-O-caffeoylquinic acid). Major three compounds and scopoletin were decided as representative components of Erycibae caulis. We established HPLC analytical method by using the representative components and 20 commercial samples which were collected considering to various cultivated area. The HPLC fingerprinting was successfully achieved with an AKZO NOBEL Kromasil 100-5C18 column. The mobile phase consisted of 0.5% acetic acid in water (A) and methanol (B) using gradient method of 85(A) to 50(A) for 35min. The fingerprints of chromatograms were recorded at an optimized wavelength of 330 nm. This developed analytical method was validated with specificity, selectivity, accuracy and precision. And it is suggested that scopolin, scopoletin, neochlorogenic acid, 3,4-di-O-caffeoylquinic acid were more than 0.162%, 0.133%, 0.057%, 0.044%, respectively. In addition, principal component analysis (PCA) was performed on the analytical data of 20 different Erycibae caulis samples in order to classify samples collected from different regions. We hope that this assay can be readily utilized as quality control method for Erycibae caulis.

• Analytical Science and Technology
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• v.22 no.4
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• pp.326-335
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• 2009

A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

• Analytical Science and Technology
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• v.32 no.4
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• pp.147-154
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• 2019

Ampicillin and Sulbactam (2:1, w/w) are combined in formulation to provide broader antibacterial action in treatment of many infections. The development of analytical method for simultaneouly determine these two compounds was difficult because of the differences in their chemical structures and ratio in the formulation. Current published methods still have some limitations. In this study, we developed an alternative high-performance liquid chromatography (HPLC) assay method for simultaneously determination of ampicillin sodium and sulbactam sodium in powder for injection. Method validation of HPLC method was conducted to determine linearity, precision, accuracy, system suitability, robustness. The linearity of the calibration curves in the desired concentration range was good ($r^2$> 0.9994). RSDs of intra-day and inter-day precision obtained were less than 2.00 %. Accuracy was obtained with the recoveries in range of 98.42 % and 101.36 %. As a result of system suitability, RSD of both retention time and the peak area obtained were not more than 1.0 %. The values of plate number were more than 7000 and symmetric factors obtained were 0.8. As intermediate-precision and robustness of the developed assay, it could be expected to become valuable tools for revising the Korean Pharmacopoeia (KP XI).

• Analytical Science and Technology
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• v.36 no.1
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• pp.32-43
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• 2023

This study reports for the first time about a stability indicating RP-HPLC method for qualitative and quantitative determination of acalabrutinib in bulk and dosage form and in presence its impurities 1, 2 and 3. The chromatographic separation was carried on Zorbax XDB-C18 (250×4.6 mm; 5 µ id) as stationary phase, Phosphate buffer pH 6.4 and methanol 80:20 (v/v) as mobile phase at a flow rate of 1.0 mL/min, UV detection was carried at wavelength of 238 nm and the analysis was completed with a run time of 15 min. In these conditions the retention time of acalabrutinib and its impurities 1, 2 and 3 was observed to be 3.50, 4.83, 8.40 and 9.93 min respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50 %, 100 % and 150 % was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for acalabrutinib and both impurities studied and the % RSD in each spiked level was found to be less than 2. Stability tests were done through exposure of the analyte solution to five different stress conditions i.e expose to 1N hydrochloric acid, 1 N sodium hydroxide, 3 % peroxide, 80 ℃ temperature and UV radiation at 254 nm. In all the degradation condition, standard drug acalabrutinib was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis there is no other chromatographic detection of other impurities and formulation excipients. Hence the developed method was found to be suitable for the quantification of acalabrutinib and can separate and analyse impurities 1 and 2.

• Analytical Science and Technology
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• v.18 no.5
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• pp.444-451
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• 2005

The accurate and simple extraction method for sterols and fatty acids in sesame oil was developed. The new method improved the extraction efficiency of sesamin in sesame oil and the ratio of sesamin over campesterol. It will be applied to judgement of adulteration of plant edible oils. The minor components of sterols were also confirmed. The simultaneous determination of sterols and fatty acids with derivatization were processed, but it was not enough to confirm adulteration, thus need more experiments.

• Analytical Science and Technology
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• v.14 no.4
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• pp.324-330
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• 2001

For the analysis of S, P and Zn in lubricating oil, microwave digestion method was studied by using inductively coupled plasma-atomic emission spectrometry(ICP-AES). Lubricating oil was completely decomposed with nitric acid or a mixture of nitric acid and hydrogen peroxide using and closed microwave digestion system. Digestions are completed within 50 min, a factor of at least 3~4 times faster than for the conventional digestion. A gradual heating program operated by the pulsed mode was found suitable for decomposing the lubricating oil matrix safely. The proposed method of digestion gave relative standard deviations(RSD) less than 3% for the elements determined.

• Analytical Science and Technology
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• v.32 no.6
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• pp.217-224
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• 2019

In this study, to evaluate the effectiveness and safety of oral therapy using Gastrodiae Rhizoma, a new HPLC-PDA analysis method was developed for the simultaneous quantitation of the three major components: (1) gastrodin, (2) gastrodigenin, and (3) p-hydroxybenzaldehyde, in steam processed and unprocessed tubers of Gastrodia elata Blume. The clear separation of the three components was achieved on a C18 column (250 × 4.6 mm, 5 ㎛) by gradient elution using water (including 0.1 % formic acid) and acetonitrile as the mobile phase. The flow rate was 1.0 mL/min, and the UV detector wavelength was set at 270 nm. The results demonstrate satisfactory linearity, recovery, precision, accuracy, stability, and robustness. The established HPLC-PDA method was applied to quantify three major compounds in 59 samples of G. elata Blume tubers. Finally, the steam processed and unprocessed tubers of G. elata Blume were successfully distinguished by pattern recognition analysis.

• Analytical Science and Technology
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• v.12 no.6
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• pp.571-576
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• 1999

Screening method for NSAIDs (Hon-Steroidal Anti-Inflammatory Drugs) in urine was developed using GC/NCI-MS. Derivatized six fenamates with pentafluoropropionic anhydride showed high sensitivity in NCI-MS. The conditions of the derivatization reaction and chromatographic conditions were established for screening with a trace analysis. Limit of detection was in the range of 4-25 pg/mL. This method may be used to the equine doping analysis for NSAIDs and forensic analysis.

• Korean Journal of Pharmacognosy
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• v.49 no.1
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• pp.70-75
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• 2018

Acer tegmentosum Maxim (ATM) has been used to treat hepatic disorders in traditional oriental medicine. However, there is little information about phytochemical constituents for quality control of ATM. In this study, we developed and established a simultaneous analytical method of the 10 marker compounds (three coumarins, 3 flavonoids, 1 lignan, 3 phenolics) in ATM using ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS). Chromatographic separation of ten target analytes was achieved with a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$), using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. Identifications and quantitation of all analytes were performed using a Q-Exactive UPLC-MS/MS system. Correlation coefficients of the calibration curve for all analytes were ${\geq}0.9986$. The values of limits of detection and quantification of all analytes were 0.5-10.0 and 5.0-50.0 ng/mL, respectively. The established UPLC-MS/MS method successfully identified all target analytes in ATM, and the phytochemicals were 0.01-67.98 mg/g in its lyophilized water extract.

• Journal of the Korea Concrete Institute
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• v.12 no.5
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• pp.101-110
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• 2000

A practical approach of calculating the ultimate strength of composite beams with unreinforced web opning is proposed through shear behavioral tests. In this method, the slab shear contribution at the opening is calculated as the smaller value of the pullout capacity of shear connector at the high moment end and the one way shear capacity of slab. A simple interaction equation is used to predict the ultimate strength under simultaneous bending moment and shear force. Strength prediction by the proposed method is compared with previous test results and the predictions by other analytical methods. The comparison shows that the proposed method predicts the ultimate capacity with resonable accuracy.