• The Korea Journal of Herbology
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• v.28 no.5
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• pp.95-101
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• 2013

Objectives : A quantitative method using high performance liquid chromatography with a photodiode array detector(HPLC-PDA) was established for the quantitative analysis of the four main compound and pattern analysis to classification Piiellia ternate, P. pedatisecta and Typhonium flagelliforme. Methods : The analytical procedure for the determination of P. ternata, together with the known main compounds uracil, uridine, guanosine and adenosine was established. Optimum HPLC-PDA separation of these P. ternata was possible on Luna C18(2) column material, using water and acetonitrile as mobile phase. The method was validated according to regulatory guidelines. In addition, this assay method were analyzed for the content of four main compound in P. ternata, P. pedatisecta and T. flagelliforme and by data obtained from the HPLC-PDA analysis was performed principal component analysis(PCA). Results : Validation results indicated that the HPLC method is well suited for the determination of the roots of P. ternata with a good linearity ($r^2$ > 0.999), precision and recovery rates. Analysis of HPLC-PDA, the average content of uracil, uridine, guanosine and adenosine was significantly higher in P. ternate>P. pedatisecta> T. flagelliforme order. The application of PCA to main compound data by HPLC-PDA permitted the effective discrimination among the three species. Conclusions : Analysis of both HPLC-PDA and PCA confirmed the fact that four main compound and pattern profiles of P. ternata, P. pedatisecta and T. flagelliforme were different from each other.

• Bulletin of the Korean Chemical Society
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• v.31 no.11
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• pp.3371-3381
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• 2010

In this study, quantitative and pattern recognition analysis for the quality evaluation of Magnoliae Flos using HPLC/UV was developed. For quantitative analysis, eleven major bioactive lignan compounds were determined. The separation conditions employed for HPLC/UV were optimized using ODS $C_{18}$ column ($250{\times}4.6\;mm$, $5\;{\mu}m$) with isocratic elution of acetonitrile and water with 1% acetic acid as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 278 nm. These methods were fully validated with respect to the linearity, accuracy, precision, recovery, and robustness. The HPLC/UV method was applied successfully to the quantification of eleven major compounds in the extract of Magnoliae Flos. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of twenty one reference samples corresponding to seven different species of Magnoliae Flos and nine samples purchased from market. The results indicate that the established HPLC/UV method is suitable for the quantitative analysis and quality control of multi-components in Magnoliae Flos.

• Bulletin of the Korean Chemical Society
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• v.32 no.1
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• pp.239-246
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• 2011

In this study, quantitative and pattern recognition analysis for the quality evaluation of Cimicifugae Rhizoma using HPLC/UV was developed. For quantitative analysis, three major bioactive phenolic compounds were determined. The separation conditions employed for HPLC/UV were optimized using ODS $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}M$) with isocratic elution of acetonitrile and water with 0.1% phosphoric acid as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 323 nm. These methods were fully validated with respect to the linearity, accuracy, precision, recovery, and robustness. The HPLC/UV method was applied successfully to the quantification of three major compounds in the extract of Cimicifugae Rhizoma. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of twelve reference samples corresponding to five different species of Cimicifugae Rhizoma and seventeen samples purchased from markets. The results indicate that the established HPLC/UV method is suitable for the quantitative analysis and quality control of multi-components in Cimicifugae Rhizoma.

• Journal of Food Hygiene and Safety
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• v.12 no.1
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• pp.71-77
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• 1997

Sulfonamides, a therapeutically important group of antimicrobial drugs, are widely used to treat and prevent the acute systemic and skin infections in dairy cattle. They also pose an economic hazard through inhibition of growth of dairy starter cultures. This study was carried out to compare four screening methods for detection of sulfamethazine in milk and determine the positive milk sample by HPLC method. Sulfamethazine was used to spike at five levels of sulfamethazine. The Lac-Tek test and CharmII test were also consistent better than TTCII test and Delvo SP test in sulfamethazine detection. Analysis probabilities of obtaining a positive response with TTCII test and Delvo SP test assay at 50 ppb sulfamethazine level in milk samples were only 14%, 42% each. Whereas using the Lac-Tek test and CharmII test would have resulted in 100% identification of the five levels. Determination of sufamethazine using the HPLC method in the spiked milk were 10.64, 19.30, 30.76,38.83 and 50.23 ppb, respectively.

• Archives of Pharmacal Research
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• v.16 no.2
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• pp.99-103
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• 1993

We describe here the conditions of thin layer chromatography (TLC) and high pressures liquid chromatography (HPLC) to improve the analytical method of phosphotyrosine (p-Tyr) in biological sample. TLC was performed on silica plate with the mixture of propanol and water (2.1 : 1 v/v) as a mobile phase and $R_1$ values were 0.42, 0.39 and 0.33 for phosphotyrosine, phosphothreonine and phosphoserine, respectively. HPLC was performed on $NH_2$ column with a mobile phase of potassium biphosphate solution by UV deterction at 192 nm. The optimum condition of HPLC was obtained at 0.01 M, pH 4.5 with a clear separation within 12 min. These procedures have been applied to the analysis of phosphotyrosine obtained from tyrosine-phosphorylated enolase. Both TLC and HPLC methods were suitable to analyze tyrosine-phosphorylated protein without being affected by contaminants from hydrolysates.

• Natural Product Sciences
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• v.17 no.4
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• pp.321-327
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• 2011

In this study, quantitative analysis was developed using HPLC/UVD for the quality evaluation of Scutellariae Radix. For quantitative analysis, six major bioactive compounds were assessed. The separation conditions employed for HPLC/UVD were optimized using Phenomenex $C_{18}$ column ($250{\times}4.6$ mm, 5 ${\mu}m$) with a gradient of solvent A (1% acetic acid of $H_2O$) and solvent B (acetonitrile : methanol : acetic acid = 70 : 30 : 1) as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 275 nm. These methods were fully validated with respect to linearity, accuracy, precision and recovery. The HPLC/UVD method was applied successfully to the quantification of six major compounds in the extract of Scutellariae Radix. The results indicate that the established HPLC/UVD method is suitable for the quantitative analysis and quality control of multicomponents in Scutellariae Radix.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.39 no.6
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• pp.542-547
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• 1994

To find out the most reasonable analysis conditions of paeoniflorin, different paeoniflorin extraction methods and various UV detector wavelengths were conducted with paeonia radix of 4-year old Euisung local variety. The most reasonable paeoniflorin extraction time by reflux apparatus was 1hr. and by ultrasonic apparatus was 3hrs. and those methods were completed only once. Concentration of paeoniflorin by reflux apparatuses at 1hr. and 2hrs. of extracting time were higher than those of ultrasonic apparatus, and the differences were highly significant. However, the differences of paeoniflorin concentration at 3hrs. and 4hrs. in two methods were not significant. In comparing paeoniflorin concentration of many lines, ultrasonic extracting apparatus was more simple and effective than the reflux apparatus. Paeoniflorin was more reasonable sensitivity at 240nm, and albiflorin was 254nm by HPLC. When paeoniflorin and albiflorin were analyzed simultaneously, 254nm was more stable than any other wavelength.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.48
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• pp.72-78
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• 2003

Carotenoids are the major pigment of pepper (Capsicum annuum) and tomato (Lycopersicon esulentum) which are very important foods in Korea. However the analysis of carotenoids is quite complicated because of their diversity and the presence of cis-trans isomeric forms of these compounds. The objective of this review is to collect the achievements on the field of the chromatographic separation of carotenoids in food and some vegetables, to describe and critically evaluate the techniques, And to compare the benefits and shortcomings of the various chromatographic methods such as adsorption and reversed-phase HPLC and thin-layer chromatography. HPLC equipped with ultra-violet or photodiode array detection is most often employed in routine use for the analysis of carotenoids. Here, the method to analyze carotenoids by HPLC separation after solvent extration and purification from pepper powder samples done in our laboratory is also mentioned.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.25 no.3
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• pp.312-321
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• 2015

Objectives: The purpose of this study was to determine the best method to analyze PAHs at extremely low concentrations. To this end, 16 PAHswere analyzed simultaneously by GC/MS, HPLC/FLD and HPLC/UVD, and the analytical characteristics of HPLC and GC/MS were compared. Methods: This study was conducted by GC/MS and HPLC/FLD/UVD, and evaluated linearity, precision and detection limit. Standard solutions were prepared for 21 samples in the range of $0.00001{\sim}1.0{\mu}g/mL$ and the samples were divided into four groups. All samples were made in three sets and analysis was replicated seven times. Results: Sixteen PAHs could be simultaneously separated by HPLC and GC/MS, and the adequate equipment was HPLC/FLD. The retention times by HPLC were shorter than GC/MS, and HPLC had better separation for most PAHs than GC/MS. The peaks of naphthalene and naphthalene-D8 partially overlapped for GC/MS. HPLC/FLD had a 20-2000 times lower limit of detection than GC/MS and UVD. However FLD was not adequate for analyzing acenaphthylene because it has too low a fluorescence quantum yield to be detected. The precision of HPLC/FLD/UVD and GC/MS showed less than 20% at $0.001{\mu}g/mL$ PAHs and when the concentration was higher, the coefficient of variation was decreased. HPLC/FLD was better for the overall detection of limits. Conclusions: The results indicate that the HPLC/FLD method has good linear range, precision and a detection of limits from $0.00001{\sim}0.0001{\mu}g/mL$ for all 16 PAHs. This study contributes to providing useful data for analysis technology and can be applied to occupational exposure measurement for PAHs in workplaces.

• Mass Spectrometry Letters
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• v.13 no.3
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• pp.58-83
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• 2022

We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL^-1; linearity (r²) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL^-1, linearity (r²) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.