scholarly journals Development and Validation of a HPLC–PDA Method for the Simultaneous Determination of Berberine, Palmatine, Geniposide, and Paeoniflorin in Haedoksamul-tang

2020 ◽  
Vol 10 (16) ◽  
pp. 5482
Author(s):  
Beom-Geun Jo ◽  
Kyung-Hwa Kang ◽  
Min Hye Yang

Haedoksamul-tang (HST) is a traditional medical prescription comprising eight medicinal herbs: Angelica gigas, Cnidium officinale, Coptis japonica, Gardenia jasminoides, Paeonia lactiflora, Phellodendron amurense, Rehmannia glutinosa, and Scutellaria baicalensis. HST is used to treat blood circulation disorders and has anti-inflammatory, hemostatic, and anticonvulsant effects. In this study, a high-performance liquid chromatography/photodiode array detector (HPLC–PDA) method was developed and validated for the simultaneous determination of four marker compounds in HST, namely, berberine, palmatine, geniposide, and paeoniflorin. Four standard solutions and HST sample solutions were analyzed using a reverse-phase SunFire®C18 column (4.6 × 250 mm, 5 μm) using a 0.05% aqueous formic acid/methanol gradient. The column temperature, flow rate, injection volume, and wavelengths used were 28 ± 2 ℃, 1.0 mL/min, 10.0 μL, and 230 nm and 240 nm, respectively. Calibration curves of the four marker compounds showed good linearity (r2 ≥ 0.9994), and limits of detection (LODs) and quantification (LOQs) were in the ranges 0.131–0.296 μg/mL and 0.398–0.898 μg/mL, respectively. Ranges of intra- and inter-day precisions and accuracies values were 96.74–102.53% and 97.95–100.83%, respectively, and relative standard deviation (RSD) values were all <4%. Recoveries averaged 92.33–116.72% with RSD values <5%. Quantitative analysis for the four marker compounds showed geniposide (10.77 mg/g) was most abundant in HST.

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.


2013 ◽  
Vol 96 (5) ◽  
pp. 1059-1064 ◽  
Author(s):  
You-Shin Shim ◽  
Seunghee Kim ◽  
Dongwon Seo ◽  
Masahito Ito ◽  
Hiroaki Nakagawa ◽  
...  

Abstract A rapid method for the simultaneous determination of flavonol aglycones in food using ultra-high-performance LC (u-HPLC) coupled with a heating-block acidic hydrolysis method was validated in terms of precision, accuracy, and linearity. The u-HPLC separation was performed on an RP C18 column (particle size 2 μm id, 2 mm, length 100 mm) with a photodiode array detector. The LOD and LOQ of the u-HPLC analyses were 0.15 and 0.47 mg/kg for myricetin, 0.09 and 0.28 mg/kg for quercetin, 0.16 and 0.49 mg/kg for kaempferol, and 0.08 and 0.25 mg/kg for isorhamnetin. The intraday and interday precisions of the individual flavonol aglycones were less than 9.31%. All calibration curves exhibited good linearity (r2 = 0.99) within the tested ranges. Total run time of u-HPLC was 13 min. The rapid u-HPLC method presented herein significantly improved the speed, sensitivity, and resolution of the analyses of myricetin, quercetin, kaempferol, and isorhamnetin in food.


2015 ◽  
Vol 98 (2) ◽  
pp. 390-396 ◽  
Author(s):  
Yang Chen ◽  
Ravinder M Reddy ◽  
Wenjing Li ◽  
Ramesh R Yettlla ◽  
Salvador Lopez ◽  
...  

Abstract An HPLC method for simultaneous determination of vitamins A and D3 in fluid milk was developed and validated. Saponification and extraction conditions were studied for optimum recovery and simplicity. An RP HPLC system equipped with a C18 column and diode array detector was used for quantitation. The method was subjected to a single-laboratory validation using skim, 2% fat, and whole milksamples at concentrations of 50, 100, and 200% of the recommended fortification levels for vitamins A and D3 for Grade “A” fluid milk. The method quantitation limits for vitamins A and D3 were 0.0072 and 0.0026 μg/mL,respectively. Average recoveries between 94 and 110%and SD values ranging from 2.7 to 6.9% were obtainedfor both vitamins A and D3. The accuracy of the method was evaluated using a National Institute of Standards and Technology standard reference material (1849a) and proficiency test samples.


2019 ◽  
Vol 10 (2) ◽  
pp. 1007-1012
Author(s):  
Sumith K Mathew ◽  
Blessed Winston A ◽  
Aswathy Mathew ◽  
Jeana Jacob ◽  
Ratna Prabha ◽  
...  

A robust and economical assay for routine determination of indocyanine green pharmacokinetics was developed and validated using high-performance liquid chromatography with a photodiode array detector. Plasma specimens from critically ill patients and those with hepatitis on various co-medications were used as blanks for validation of this assay. Extraction of indocyanine green was performed by simple protein precipitation with acetonitrile, and the supernatant was separated using an octadecyl column with detection at 784 nm. Blanks were found to have no interference for 40 blanks of patients who were on 56 different medications. The precision for LLOQ (0.5 µg/ml) as determined by the percentage coefficient of variation was 1.19. Stability of plasma calibration standards and stock were determined over a period of 61 days, and ICG was found to be stable for 20 days. Stability of whole blood specimens containing ICG was determined at 4°C for a period of 4 hours.


2019 ◽  
Vol 57 (9) ◽  
pp. 790-798 ◽  
Author(s):  
Mahmoud A Tantawy ◽  
Soheir Alweshahy ◽  
Dalia A Elshabasy ◽  
Nadia F Youssef

Abstract A selective reversed phase high performance liquid chromatography/photodiode array detector (RP-HPLC/PAD) method has been developed for simultaneous determination of the three co-administrated deflazacort, aprepitant and granisetron drugs used with chemotherapy. The three cited drugs have been chromatographed on C18 column using a mobile phase consisting of acetonitrile–0.2% v/v triethylamine (80:20 v/v, pH of 6.6 ± 0.05) with isocratic elution and monitored by photodiode array at 220 nm. International conference on harmonization (ICH) guidelines were followed to validate the developed method. Successful application of the developed method was assessed by the simultaneous determination of the studied drugs in pure forms, dosage forms and plasma samples in the ranges of 0.2–20, 0.4–40 and 0.2–20 μg/mL for deflazacort, aprepitant and granisetron, respectively.


2013 ◽  
Vol 49 (1) ◽  
pp. 117-126 ◽  
Author(s):  
Ana Cristina de Mattos ◽  
Najeh Maissar Khalil ◽  
Rubiana Mara Mainardes

The objective of this work was to develop and validate a rapid high performance liquid chromatography (HPLC) method for the quantitative analysis of fluorouracil (5-FU) in polymeric nanoparticles. Chromatographic analyses were performed on an RP C18 column with a mobile phase consisting of acetonitrile and water (10:90, v/v) at a flow rate of 1 mL/min. The 5-FU was detected and quantitated using a photodiode array detector at a wavelength of 265 nm. The method was shown to be specific and linear in the range of 0.1-10 µg/mL (r = 0.9997). The precision (intra- and inter-day) was demonstrated because the maximum relative standard deviation was 3.51%. The method is robust relative to changes in flow rate, column and temperature. The limits of detection and quantitation were 10.86 and 32.78 ng/mL, respectively. The method fulfilled the requirements for reliability and feasibility for application to the quantitative analysis of 5-FU in polymeric nanoparticles.


2011 ◽  
Vol 94 (4) ◽  
pp. 1076-1081 ◽  
Author(s):  
Fernando Rodríguez-Ramos ◽  
Víctor H Sánchez-Estrada ◽  
Alejandro Alfaro-Romero ◽  
Gabriela Rubí Tapia-Álvarez ◽  
Andrés Navarrete

Abstract An HPLC method was developed for the simultaneous determination of gnaphaliin A and B, active compounds of Gnaphalium liebmannii Sch. Bp ex Klatt. The HPLC separation was performed on an Inertsil ODS-3 (150 × 4.6 mm id, 5 μm) RP C18 column operated at 40°C; the isocratic mobile phase was 0.02% aqueous orthophosphoric acid– methanol–acetonitrile (50 + 30 + 20, v/v/v), with a run time of 20 min and flow rate of 1.5 mL/min. Detection with a photodiode array detector (PDAD) was at 270 nm. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ for gnaphaliin A and B were found to be in the range of 0.4–0.5 and 1.0–1.4 μg/mL, respectively. This is the frst report of an analytical method developed for the quantitative analysis of flavones from Gnaphalium species by HPLC-PDAD with applications for raw material and commercial products.


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