• Archives of Pharmacal Research
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• v.11 no.1
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• pp.45-51
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• 1988

The feature of resolution enhancement by derivative operation is linked to one of the multivariate analysis, which is multiple linear regression with two options, all possible and stepwise regression. Examined samples were synthetic mixtures of 5 vitamins, thiamine mononitrate, riboflavin phosphate, nicotinamide, pyridoxine hydrochloride and ascorbic acid. All components in mixture were quantified with reasonably good accuracy and precision. Whole data processing procedure was accomplished on-line by the development of three computer programs written in APPLESOFT BASIC language.

• Natural Product Sciences
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• v.27 no.4
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• pp.264-273
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• 2021

Simultaneous quantification of multiple marker compounds in herbal medicine by high performance liquid chromatography (HPLC) analysis is still a challenge due to the complexity in various parameters to be considered and co-existing multi-components. As a case study, a reliable HPLC method for simultaneous quantification of paeoniflorin from Paeoniae Radix and decursin from Angelicae Gigantis Radix in various commercial herbal medicine was developed based on analytical quality by design (AQbD) strategy. As a first step, risk assessment was performed to select the critical method parameters (CMPs) which were decided as organic mobile phase ratio and column oven temperature. In order to evaluate the effect of the CMPs on critical method attributes (CMAs) of peak resolution and tailing, central composite design (CCD) was employed. The final chromatographic conditions were optimized as follows: column- C₁₈, 4.6 × 250 mm, 5 ㎛ particle size; mobile phase- A: acetonitrile, B: 0.1% acetic acid water; detection wavelength- 235 nm for paeoniflorin, 325 nm for decursin; column oven temperature- 25℃; flow rate- 1.0 mL/min; gradient mobile phase system as Time (min) : % A, 0:14, 25:14, 30:50, 60:50, 61:100, 65:100, 66:14, 75:14. The method was successfully validated according to the International Conference on Harmonization (ICH) guidelines and piloted for ten commercial herbal medicines.

• Archives of Pharmacal Research
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• v.11 no.2
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• pp.99-113
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• 1988

Quantitation of ethenzamide, isopropylantipyrine and caffeine takes about 41 hrs by conventional GC method. Quantitation of allylisoprorylacetylurea takes about 40 hrs by conventional UV method. But quantitation of them takes about 6 hrs by DRIFT developing method. Each standard and sample sieved, powdered and acquired DRIFT spectrum. Out of them peak of each component was selected and ratio of each peak to standard peak was acquired, and then linear stepwise multiple regression was performed with these data and concentration. Reflectance value, Kubelka-Munk equation and Inverse-Kubelka-Munk equation were modified by us. Inverse-Kubelka-Munk equation completed the deficit of Kubelka-Munk equation. Correlation coefficients acquired by conventioanl GC and UV against DRIFT were more than 0.95.

• YAKHAK HOEJI
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• v.30 no.4
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• pp.185-192
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• 1986

Authors developed the computer application program (language: APPLE SOFT BASIC) for derivative spectrophotometry. By means of this program, derivative of spectral absorbance with respect to wavelength is recorded versus wavelength. To try this program in connection with spectrophotometer system, the authors have done the simultaneous quantitation of pyridoxine center dot HCl and nicotinamide in the mixture, and the result was compared with that of absorbance method.

• Journal of Food Hygiene and Safety
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• v.8 no.1
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• pp.17-23
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• 1993

In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents n meat simultaneously, we studied a gas chromatogrphy-mass spectrometry (GC/MS) analysis. For a simultaneous analysis of macrolide antibiotics such as erythromycin and tylosin in meat, the homogenization with MeOH, defatting with n-hexane, extraction with CHCl3, elution with CHCl3 : MeOH=2:1 from Sep-Pak silica cartridge, acid gydrolysis, back extraction with CHCl3, and quantitation by selected ion monitoring(SIM) mode after trimethylsilyl derivatization were performed. The recoveries of erythromycin and tylosin (CV,%) at 10 ppm fortification level were 90.59(4.89) and 45.91(0.20) , and the detection limits of those were 0.02 and 2.0 $\mu\textrm{g}$/g beef, respectively. From these results, the developed analytical method using GC/MS-SIM mode allows excellent detection and quantitation of residual macrolide antibiotics in meats, using complementary method with bio-assay.

• Journal of Food Hygiene and Safety
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• v.5 no.3
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• pp.159-164
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• 1990

To detect and quantitation residual antibiotics and antibacterial agents in meats, we performed a biological assay employing the three microorganisms Bacillus subtilis ATCC 6633, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778 for the screening purpose and developed a Gas Chromatography-mass Spectrometry(GC/MS) analysis for the confirmation and quantiation. In the biological assay (paper disk method), three test solution are used depending on the character of the residual antibiotics and antibacterial agents, follow by a simple clean up procedure which includes homogenization with Mcilvaine buffer, defatting with includes homogenization with Mcilvaine buffer, defatting with hexane, extraction with chloroform, clean-up by Sep-Pak $C_{18}$ and Bakerbond SPE carboxylic acid column. The chloroform layer is used for the analysis of sulfa agents. macrolides antibiotics and antibacterial agents, Adsorbed materials in the Sep-Pak $C_{18}$ were also employed for th analysis of penicillins and tetracyclines. Effluents from the Sep-Pak $C_{18}$ were cleaned-up one more by Bakerbond 10 SPE COOH column and employed for the analysis of aminoglycosides. In the instrumental analysis by using the GC/MSD, residual antibiotics and antibacterial agent were quantitated by selected ion monitoring (SIM) mode after derivatization. A simultaneous analysis of six residual antibiotic and antibacterial agent such as oxytetracycline, penicillin, ampicillin, choliraphenicol and thiamphenicol was developed with simple cleanup procedures revealing good recovery and reproducibility. Also, simultaneous detection of macrolides antibiotics such as erythromycin, spiramycin, and oleandomycin was developed after acid hydrolysis due to their large molecular structures. Because of the high reproducibility and selectivity of these two methods, it is very desirable that the combination of the two methods be used in the bioassay for the screening of residual antibiotics and antibacterial agent and that GC/MSD analysis be used for the confirmation and quantitation.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2000.05a
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• pp.3-8
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• 2000

A simple and rapid simultaneous analysis method of BTEX and TPH in soil was developed. 5g of soil sample were mixed with sodium sulfate and then extracted with 10 mL of mixture of acetone and dichloromethane (1:1). Extraction was performed for 10 min in sonicator and analysis was with GC-FID. The detection limits of BTEX and TPH was 0.8 and 10 mg/kg, respectively. The analytical recoveries were >90% for all BTEX and TPH. Low boiling point fuels and high boiling point fuels are consistently reproduced within RSD 7%. The analysis results show very simple and rapid quantitation of BTEX and TPH in soil sample with low RSD.

• Natural Product Sciences
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• v.18 no.3
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• pp.171-176
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• 2012

We previously isolated cordycepin, guanosine and tryptophan from Cordyceps militaris as antiadipogenic constituents. For the quality control of C. militaris for anti-adipogenic activity, simultaneous analytical method using high-performance liquid chromatography (HPLC)-diode array detection (DAD) was developed and validated. Quantitation of these compounds in various Cordyceps samples from different sources and various extraction methods were conducted using developed method. Our study shows that natural Cordyceps and host insect possess higher content than cultured ones and fruiting bodies, respectively. The content of cordycepin showed great difference in different C. militaris samples whereas trytophan content was similar in tested samples. Addition of water to extraction solvent greatly increased the yield of guanosine and tryptophan. High temperature and longer extraction time increased yield of guanosine, whereas the content of trytophan was decreased in high temperature during extraction with water. Extraction using ultrasonic apparatus slightly increased extraction efficiency. Cordycepin, however, has little variation in different extraction method tested. Strong anti-adipogenic activity was observed in the samples that contain all the three constituents. Taken together, quantitation of these compounds using developed analytical method might provide basic requirement for the anti-adipogenic activity of C. militaris.

• Journal of Pharmaceutical Investigation
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• v.21 no.3
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• pp.179-188
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• 1991

An HPLC assay method of a drug to be applied to the pharmacokinetic studies of the drug should be completely validated. The validation process for an HPLC assay method in a biological sample was discussed using the data obtained from the development of HPLC method for the simultaneous quantitation of verapamil and norverapamil in human serum. The validation criteria included were specificity, linearity, accuracy, precision, sensitivity, recovery, drug stability, and ruggedness of an assay method.

• Archives of Pharmacal Research
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• v.13 no.3
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• pp.215-220
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• 1990

Two different, derivative spectrophotometric and gas-liquid chromatographic, procedures for direct quantitation of caffeine and some commonly dispensed antihistaminics in bulk forms, in their laboratory prepared mmixtures and in dosage formulations, have been investigated. The limit, sensitivity reproducibility and accuracy of each method were studied for each individual drug substance and in some usual pharmaceutical formulations.