• Title/Summary/Keyword: HPLC detector

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Development of an analytical method for the quantification of oleanonic acid from mastic gum using HPLC/PDA

  • Hak-Dong Lee;Chang-Dae Lee;So Yeon Choi;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.67-72
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    • 2023
  • A simple and accurate method was developed for the quantitative analysis of oleanonic acid (OA) from mastic gum. The analysis was carried out using reverse-phase high-performance liquid chromatography combined with a photodiode array detector (HPLC/PDA). Our optimized method was validated by measuring various parameters, using an INNO C18 column fitted with a gradient elution system. The results revealed limits of detection and quantification of 0.34 and 1.042 ㎍/mL, respectively. The OA calibration curve exhibited excellent linearity over the concentration range of 0.0625 to 2.0 mg/mL, with r2 =0.9996. Accuracy tests revealed a high recovery rate of 99.44-103.66%, with precision values below 0.15%. These results suggest that the present analytical method can identify and quantify OA in mastic gum with high precision. The HPLC approach developed in this study might be applied to routine analyses and large-scale extraction procedures for OA content quantification.

Study on Decomposition of Several Pesticides by Gamma-Irradiation (감마선 조사에 의한 농약 성분의 분해 연구)

  • Lee, Joo-Sang;Jung, Su-Yeon;Oh, Seung-Yeol;Jang, Beom-Su;Park, Sang Hyun
    • Journal of Radiation Industry
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    • v.6 no.3
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    • pp.205-209
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    • 2012
  • The decomposition of 50 pesticides present in an aqueous solution using ${\gamma}-irradiation$ from a $^{60}Co$ gamma-ray source was investigated using laboratory-scale experiment. The rates of decomposition were determined using a gas chromatography-electron capture detector (GC-ECD), high-performance liquid chromatography-photo diode array detector (HPLC-PDA), and HPLC-fluorescence detector (FLD). When the initial concentration of pesticides was 10 ppm, and the radiation dose was 2, 5, 10, 20, and 30 kGy, respectively, 14 pesticide samples showed high removal rates (>50%) at absorbed doses of more than 10 kGy. With the exception of procymidone, they were all completely removed at a 30 kGy irradiation dose. These results provide fundamental data on the reactivity between gamma-irradiation and pesticides in an aqueous solution. Further, an evaluation of the toxicity of radiolytic intermediate products is required.

Simplified HPLC Method for the Determination of Pseudoephedrine Hydrochloride from Allegra D Tablet

  • Park, Moon-Hee;Shin, In-Chul
    • Biomolecules & Therapeutics
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    • v.15 no.2
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    • pp.123-126
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    • 2007
  • A sensitive, simple and highly selective liquid chromatography method of determination for extraction of pseudoephedrine hydrochloride from Allegra D tablet was developed. The chief benefit of the present method is the minimal sample preparation, as the procedure is only filtering through pore syringe filter. Two drugs (pseudoephedrine hydrochloride, fexofenadine) were separated on a C$_{18}$ column and analyzed by high performance liquid chromatography (HPLC). The method had a chromatographic run time of 8.0 min. 1 ml of pseudoephedrine hydrochloride solution (1 mg/ml) was filtered through 0.22 um pore syringe filter. 50 ul of filtering solution was injected to HPLC pump and we knew the retention time (1.85 min) of separating of pseudoephedrine hydrochloride using UV detector at 280 nm. We used C$_{18}$ column (4.6 mm${\times}$250 mm), mobile phase solution (<0.05 mol/L NaH$_2$PO$_4$, 2 ml/L H$_3$PO$_4$>/CH$_3$CN / sodium dodesyl sulfate = 60 ml / 40 ml / 1 g). We separated psedoephedrine hydrochloride at run time of 1.85 min from Allegra D tablet solution (1 mg/ml) filtered through 0.22 um pore syringe filter using UV detector at 280 nm. Flow rate was set at 1.0 ml/min and the column temperature was set at 40$^{\circ}C$. Psedoephedrine hydrochloride solution (1 mg/ml) separated from Allegra D tablet was filtered through 0.22 um pore syringe filter and injected 50 ul. We confirmed the peak of psedoephedrine hydrochloride at same retention time and the separating solution was freeze-dried. In conclusion, A simple isocratic reverse-phase HPLC method has been developed that provides excellent separation of pseudoephedrine from Allegra D tablet.

Fingerprint of Marker Substances in Gami-Honghwa-Tang(KH-19) by HPLC-DAD (High Performance Liquid Chromatography-Diode Array Detector(HPLC-DAD)에 의한 가미홍화탕 (KH-19)의 지문 분석)

  • Yu Young-Beob;Yoon Yoo-Sik;Cho Gi-Ho
    • The Journal of Korean Medicine
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    • v.25 no.3
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    • pp.45-54
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    • 2004
  • Objectives : This study was aimed to evaluate marker substances in Gami-Honghwa-Tang (KH-19) by high performance liquid chromatography-photodiode array detector (HPLC-DAD). Gami-Honghwa-Tang is composed of nine crude herbs, Rehmanniae Radix Preparata, Angelicae Gigantis Radix, Cnidii Rhizoma, Paeoniae Radix, Corni Fructus, Moutan Cortex Radicis, Lycii Fructus, Carthami Flos and Glycyrrhizae Radix. Methods : The separation was performed on an Aquasil C18 (4.6×250mm) column by gradient elution with 0.05% TFA in H2O - 0.05% TFA in acetonitrile (0 min 100:0, 20 min 90:10, 40 min 70:30, 60 min 50:50, 80 min 0:100, 90 min 100:0) as the mobile phase at a flow-rate of 1.0 ml/min with detection at 190-800nm. Also we examined the contents for bacteria, pesticide residue and harmful heavy metals. Results : HPLC-DAD was employed to determine the quantities and the qualities of several marker substances such as 5­hydroxymethyl-2-furaldehyde (5-HMF), paeonol, loganin, paeoniflorin, glycyrrhizin, and decursin in the KH-19. There were no bacterial contents, pesticide residues, or harmful heavy metals. Conclusions : We suggest these results could be a useful evidence for quality control of KH-19. This method permits fingerprints of selected individual marker substances from herbal prescriptions without derivatization, multiple purification steps, or lengthy separation times.

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Stability Test and Quantitative and Qualitative Analyses of the Amino Acids in Pharmacopuncture Extracted from Scolopendra subspinipes mutilans

  • Cho, GyeYoon;Han, KyuChul;Yoon, JinYoung
    • Journal of Pharmacopuncture
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    • v.18 no.1
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    • pp.44-55
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    • 2015
  • Objectives: Scolopendra subspinipes mutilans (S. subspinipes mutilans) is known as a traditional medicine and includes various amino acids, peptides and proteins. The amino acids in the pharmacopuncture extracted from S. subspinipes mutilans by using derivatization methods were analyzed quantitatively and qualitatively by using high performance liquid chromatography (HPLC) over a 12 month period to confirm its stability. Methods: Amino acids of pharmacopuncture extracted from S. subspinipes mutilans were derived by using O-phthaldialdehyde (OPA) & 9-fluorenyl methoxy carbonyl chloride (FMOC) reagent and were analyzed using HPLC. The amino acids were detected by using a diode array detector (DAD) and a fluorescence detector (FLD) to compare a mixed amino acid standard (STD) to the pharmacopuncture from centipedes. The stability tests on the pharmacopuncture from centipedes were done using HPLC for three conditions: a room temperature test chamber, an acceleration test chamber, and a cold test chamber. Results: The pharmacopuncture from centipedes was prepared by using the method of the Korean Pharmacopuncture Institute (KPI) and through quantitative analyses was shown to contain 9 amino acids of the 16 amino acids in the mixed amino acid STD. The amounts of the amino acids in the pharmacopuncture from centipedes were 34.37 ppm of aspartate, 123.72 ppm of arginine, 170.63 ppm of alanine, 59.55 ppm of leucine and 57 ppm of lysine. The relative standard deviation (RSD %) results for the pharmacopuncture from centipedes had a maximum value of 14.95% and minimum value of 1.795% on the room temperature test chamber, the acceleration test chamber and the cold test chamber stability tests. Conclusion: Stability tests on and quantitative and qualitative analyses of the amino acids in the pharmacopuncture extracted from centipedes by using derivatization methods were performed by using HPLC. Through research, we hope to determine the relationship between time and the concentrations of the amino acids in the pharmacopuncture extracted from centipedes.

HPLC Method for the Determination of Nicorandil in Human Plasma

  • Park, Sun-Hee;Shin, In-Chul
    • Biomolecules & Therapeutics
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    • v.16 no.2
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    • pp.168-172
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    • 2008
  • The present study is to determine of sensitive nicorandil analysis method using HPLC and measure the pharmacokinetics parameters (bioavailability, $C_{max}$, $T_{max}$, Ke, $T_{1/2}$) of nicorandil (5 mg, Tab; Choongwae Pharma Corporation). Plasma (500 ul) was mixed with furosemide (internal standard, 500 ug/ml). Detection wavelength was 256 nm. The mixture of 0.01 M ammonium acetate and acetonitrile 80:20 (v/v) was used mobile phase. The HPLC separation was accomplished on ODC reverse HPLC column. The nicorandil was analyzed by a HPLC system, which consists of CAPCELL PAK C18 column (5 ${\mu}$m, 4.6 × 150 mm) and a chromatography data analysis S/W, using a isocratic mobile phase (mixture of 0.01 M ammonium acetate and acetonitrile 80:20 ) at 1.0 ml/min. Its sensitivity, selectivity, accuracy and precision must be adequate for the bioavailabilty study of nicorandil, and the linearity ($r^2$ ≥ 0.9994) of nicorandil was also proved in the range of 0.05 ug/ml . 3 ug/ml. The pharmacokinetic parameters of nicorandil (5 mg) tablets were measured as the follow. AUC: 0.19 ug/ml·hr, $C_{max}$: 0.14 ug/ml, $t_{max}$: 0.58 hr, Ke: 0.11 hr., $t_{1/2\beta}$: 6.76 hrs. This method is simple and sensitive HPLC method using UV detector for determination of nicorandil in human plasma.

DERIVATIZATION OF FATTY ACIDS WITH 2-BROMOACETYLTRIPHENYLENE FOR HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

  • Ryu, Jae-Ha;Park, Man-Ki
    • Analytical Science and Technology
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    • v.6 no.4
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    • pp.411-415
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    • 1993
  • A method for UV labeling of fatty acids with 2-bromoacetyltriphenylene using 18-crown-6-ether as a catalyst is described. The procedure is rapid, simple, quantitative and applicable to the HPLC analysis of fatty acids with UV detector. They have high molar absorptivity and their detection limit was about 1ng level. Nine derivatives of saturated fatty acid($C_{12}-C_{22}$) were separated on reverse-phase column(${\mu}$-Bondapak C-18) using acetonitrile-water gradient.

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Durable Press Finishing of Silk/Cotton Fabrics with BTCA(2) - The Evaluation of Physical Properties of Silk/Cotton Fabrics Treated with BTCA by HPLC Analysis - (BTCA에 의한 실크/면 교직물의 DP 가공(2) - HPLC에 의한 BTCA 처리 실크/면 교직물의 물리적 특성 평가 -)

  • 조석현;이문철
    • Textile Coloration and Finishing
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    • v.14 no.3
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    • pp.19-25
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    • 2002
  • Silk/cotton fabrics were treated with butanetetracarboxylic acid(BTCA) under various treating conditions such as concentration, treated time and curing temperatures. Bending property, tensile strength, wrinkle recovery angle, and shrinkage were measured. The BTCA concentration in the saponfication mixture was measured by an isocratic HPLC equipped with the strong cationic exchange column Aminex HPX-87-H and a UV detector. The detected concentration of BTCA was shown in silk side much more than that of cotton side. The bending and shrinkage properties were improved at minimum curing condition and the lower concentration of BTCA. Tensile strength decreased with increasing concentration of BTCA, curing temperature and treated time, while wrinkle recovery angle increased.