Rapid Method for the Simultaneous Determination of Flavonol Aglycones in Food Using u-HPLC Coupled with Heating Block Acidic Hydrolysis

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.

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.


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.


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.


Author(s):  
Saniye Özcan ◽  
Serkan Levent ◽  
Nafiz Öncü Can

: The alkyl esters of p-hydroxybenzoic acid at the C-4 position, “the parabens,” including methyl, ethyl, propyl, and butyl, are widely used as antimicrobial preservatives in foods, cosmetics, and pharmaceuticals. Official regulations on the use of these compounds make their analysis essential for the estimation of their exposure. On this basis, the presented study was realized to develop a simple, selective and cheap high-performance liquid chromatographic method for the quantitative determination of methyl paraben (MP), ethyl paraben (EP), n-propyl paraben (NPP), isopropyl paraben (IPP), n-butyl paraben (NBP), isobutyl paraben (IBP) and benzyl paraben (BP) in pharmaceuticals and cosmetic products. The chromatographic separation of the analytes was achieved under flow rate gradient elution conditions using a C18-bonded core-shell silica particle column (2.6 μm particle size, 150 × 3.0 mm from Phenomenex Co.). The samples were injected into the system as aliquots of 1.0 μL, and the compounds were detected by using a photodiode array detector set at 254 nm wavelength. With this technique, seven paraben derivatives can be determined in the concentration range of 250-2000 ng/mL. The recovery of the method is in the range of 99.95-13.84%, and the RSD is at a maximum value of 3.95%. The proposed method was fully validated and successfully applied to different pharmaceutical and cosmetic samples (n=16), including syrups, suspensions, oral sprays, gels, etc. At least one paraben derivative was detected in six of the samples, and was determined quantitatively. The maximum amount of a paraben derivative found in the analyzed samples is 321.7 ng/mL, which was MP. To the best of our knowledge, this is the first LC method, which is applicable both on pharmaceutical and cosmetic samples.


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.


2010 ◽  
Vol 93 (3) ◽  
pp. 855-861 ◽  
Author(s):  
Qi Yang ◽  
Feng Zhang ◽  
Shou-Hong Gao ◽  
Lian-Na Sun ◽  
Wan-Sheng Chen

Abstract An HPLC method combined with a photodiode array detector was developed for quantitative determination of five bioactive compounds that belong to two subclasses, including limonin, phellodendrine, jatrorrhizine, palmatine, and berberine in Cortex Phellodendri. The analysis was performed on an Agilent Diamonsil C18 column (4.6 250 mm, 5 m) using a gradient of acetonitrile and 0.3 aqueous diethylamine phosphate (v/v), a flow rate of 0.8 mL/min, and a detection wavelength of 220 nm. The calibration curve was linear over the range of 2.5100.0 g/mL for both phellodendrine and jatrorrhizine, 5.0200.0 g/mL for palmatine, and 7.5300.0 g/mL for both berberine and limonin. The average recoveries ranged from 97.56 to 102.53 with RSD 1.00. Samples from different geographical locations were analyzed to evaluate the applicability of the established method, and the results indicated that the method was efficient, sensitive, and reliable for determining limonin and four alkaloids in Cortex Phellodendri.


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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