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Assessment of seasonal variation of the bioactive oleuropein in Olea europaea L. leaves cultivated in Saudi Arabia

Alqarni Mohammed Hamed, Salkini Mohamad Ayman, Alam Prawez, Alanazi Mazen Talal, Abdel-Kader Maged Saad, El Sohafy Samah M.

Acta Chromatographica

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2022

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Vol. 34, no. 3

297--303

EN

Plants secondary metabolites undergoes qualitative and quantitative variation due to environment al and growth factors. It is a crucial factor to select the proper time for collection of medicinal plants to assure maximum content of active components reflected as maximum efficacy. Olive leaves (Oleaeuropaea L.) are known traditionally for their antidiabetic effect. The secoiridoid glycoside oleur-opein is the main active component of Olive leaves responsible for the biological activity. The current study was conducted to monitor the seasonal variation of oleuropein in Olives leaves collected from the same location. To achieve this goal a validated HPLC method following the ICH guidelines was established. Separation was conducted using RP18 column and a mobile chase consisted of ultrapure water containing 20% acetonitrile and 1% acetic acid. Detection was performed at 254 nm with 1 mL/min flow rate. The method was simple, linear, accurate, precise, specific and robust. The analyses revealed considerable variations in the level of oleuropein throughout the year. This variation cannot be explained by temperature variation during the year. Two points of high levels of oleuropein were detected prior to flowering stage and ripening of the fruits. The levels of growth regulators most likely is responsible for the increased production of oleuropein. It is recommended that leaves intended for medicinal use to be collected during the fruiting stage prior to fruit ripening.

2

High-Performance Thin-Layer Chromatographic Analysis of Eugenol in Developed Nanoemulsion Gel and Nanoparticles: Validation of a Stability-Indicating Method

Pramod K., Ilyas U. K., Singh M., Kamal Y. T., Ahmad S., Ansari S. H., Ali J.

Acta Chromatographica

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2015

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Vol. 27, no. 3

571--582

EN

High-performance thin-layer chromatography (HPTLC) method for the quantification of eugenol from nanostructured drug delivery systems was successfully developed and validated. The mobile phase consisted of n-hexane:acetone (7:3, v/v), and the densitometric scanning was performed in the absorbance mode at 280 nm. The method was valid with respect to linearity and range, accuracy, precision, specificity, detection limit (DL), and quantitation limit (QL). The linearity of the method was established by a correlation coefficient value of 0.9930 ± 0.0013. The precision was tested by checking intra-day (repeatability) and inter-day (intermediate precision) variations. The method was established to be precise by low relative standard deviation (RSD) values for different concentration of eugenol. The results of the recovery studies of eugenol from preanalyzed samples demonstrated the accuracy of the method. The specificity of the developed method for the analysis of eugenol in the nanoemulsion gel and nanoparticles samples was confirmed by comparing the spectra obtained in standard and sample analysis. The DL and QL were determined to be 31.41 and 95.17 ng band−1, respectively, for the HPTLC method. The forced degradation studies revealed on eugenol established the effectiveness of the developed and validated method. The developed and validated HPTLC method was found to be a stability-indicating one, as indicated by the results of forced degradation studies, for its use during the accelerated stability studies of the nanoemulsion gels and nanoparticles of eugenol.

3

Walidacja metod analitycznych wykorzystujących technikę HPLC w przemyśle farmaceutycznym

Padkowska K.

Laboratorium - Przegląd Ogólnopolski

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2014

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nr 5-6

54--56

PL

Walidacja metod analitycznych z wykorzystaniem techniki HPLC to działanie, które ma na celu potwierdzenie i udokumentowanie, że opracowana metoda analityczna spełnia założone kryteria akceptacji dobrane odpowiednio do jej zastosowania. Uszczegółowienie podejścia do walidacji metod wykorzystujących HPLC dla przemysłu farmaceutycznego odnajdujemy w wytycznych ICH.

EN

Validation of analytical methods using HPLC is an action that aims to support and substantiate that the developed analytical method meets the established acceptance criteria matched to its application. Refinement approach to the validation of methods using HPLC for the pharmaceutical industry can be found in the ICH guidelines.

4

Development and validation of HPTLC-densitometric method for estimation of trigonelline in leaves of Abrus precatorius L. and its formulation

Kumbhalkar B. B, Rajopadhye A. A, Upadhye A. S

Acta Chromatographica

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2012

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Vol. 24, no. 3

511--518

EN

A new, simple and reproducible HPTLC-densitometric method has been established and validated for estimation of trigonelline in leaves of Abrus precatorius L. and its herbal formulation Chatak® using ICH guidelines. Accelerated solvent extraction (ASE) as an alternative to convention techniques was also explored for the rapid extraction. The methanol extracts of leaves, its formulation, and standard solution of trigonelline were applied on silica gel F254 HPTLC plates and developed in twin chamber using mobile phase toluene-ethyl acetate-formic acid-methanol (2:3:1.8:3.8, v/v/v/v). The plates were scanned at 268 nm (λmax of trigonelline) using Camag TLC scanner 3 with CATS 4 software. A linear relationship was obtained between response (peak area) and amount of trigonelline in the range 40–200 ng spot−1; the correlation coefficient was 0.9957. ASE method has higher extraction efficiency in less time as compared to Soxhlet extraction. The HPTLC-densitometric method showed good linearity, recovery and high precision of compound. It is useful to analyze trigonelline in A. precatorius leaves and routine quality control of its marketed formulation.

5

Development and validation of an HPTLC-densitometric method for the estimation of trigonelline in the leaves of Abrus precatorius L. and its formulation

Kumbhalkar B. B, Rajopadhye A. A, Upadhye A. S

Acta Chromatographica

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2012

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Vol. 24, no. 2

263--273

EN

A new, simple, and reproducible HPTLC-densitometric method has been established and validated for estimation of trigonelline in the leaves of Abrus precatorius L. and its herbal formulation Chatak® using ICH guidelines. Accelerated solvent extraction (ASE) as an alternative to conventional techniques was also explored for rapid extraction. The methanol extracts of leaves, its formulation, and standard solution of trigonelline were applied on silica gel F254 HPTLC plates and developed in a twin chamber using the mobile phase toluene-ethyl acetate-formic acid-methanol (2:3:1.8:3.8, υ/υ/υ/υ). The plates were scanned at 268 nm (λmax of trigonelline) using a Camag TLC scanner 3 with the CATS 4 software. A linear relationship was obtained between the response (peak area) and the amount of trigonelline in the range 40–200 ng per spot; the correlation coefficient was 0.9957. The ASE method gives higher extraction efficiency in less time compared to Soxhlet extraction. The HPTLC-densitometric method showed good linearity, recovery, and high precision. It is useful to analyze trigonelline in A. precatorius leaves and routine quality control of its marketed formulation.

6

Development and validation of a simple, stability-indicating high-performance liquid chromatographic method for analysis of tolterodine tartrate in the bulk drug and in its tablet formulation

Sinha V. R, Jindal V, Kumar R. V, Bhinge J. R, Goel H

Acta Chromatographica

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2011

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Vol. 23, no. 1

133--143

EN

A stability-indicating HPLC method has been developed for analysis of tolterodine tartrate in the bulk drug and in formulations. Acceptable separation of the drug and its degradation products was achieved at 40°C on a 4.6 mm i.d. × 250 mm, 5-μm particle, C18 column with 40:60 (υ/υ) buffer solution-methanol containing 0.5% (υ/υ) triethylamine as mobile phase. The pH of the mobile phase was adjusted to 7.0 ± 0.1 with orthophosphoric acid. The flow rate was 1.2 mL min -1and the detection wavelength 220 nm. The method was validated for linearity, precision, accuracy, specificity, and robustness. Response was a linear function of concentration over the range 1–100 μg mL-1. The slope of the calibration plot was 17.82 mV s -1ppm-1, the correlation coefficient 0.999, and the relative standard deviation (RSD) 0.23%. Assessment of precision revealed method RSD was low — from 1.59 to 1.88% for intra-day precision and from 0.59 to 1.90% for inter-day precision. Stress degradation studies showed tolterodine tartrate was stable to acidic and neutral hydrolysis, oxidative stress, photolytic stress, and thermal stress but labile to alkaline hydrolysis.

7

Densitometric HPTLC analysis of cordifolioside A in Tinospora cordifolia and commercial formulations

Alam P., Ali M., Singh R., Shakeel F.

Acta Chromatographica

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2009

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Vol. 21, no. 4

683--692

EN

A densitometric HPTLC method for analysis of cordifolioside A both in 60% methanolic extract of Tinospora cordifolia and in a commercial formulation has been established and validated. Cordifolioside A was separated on aluminum-backed silica gel 60 F254 plates with chloroform-methanol 85:15 (%, v/v ) as mobile phase. A compact band was obtained for cordifolioside A at R F 0.52 ± 0.03. The limits of detection (LOD) and quantification (LOQ) were 20.12 and 60.36 ng per band, respectively. The highly precise and accurate method was used for analysis of cordifolioside A.