Simultaneous determination of 6-shogaol and 6-gingerol in various ginger (Zingiber officinale Roscoe) extracts and commercial formulations using a green RP-HPTLC-densitometry method

© 2020 by the authors. Licensee MDPI, Basel, Switzerland. Various analytical methodologies have been reported for the determination of 6-shogaol (6-SHO) and 6-gingerol (6-GIN) in ginger extracts and commercial formulations. However, green analytical methods for the determination of 6-SHO and 6-GIN, either alone or in combination, have not yet been reported in literature. Hence, the present study was aimed to develop a rapid, simple, and cheaper green reversed phase high-performance thin-layer chromatography (RP-HPTLC) densitometry method for the simultaneous determination of 6-SHO and 6-GIN in the traditional and ultrasonication-assisted extracts of ginger rhizome, commercial ginger powder, commercial capsules, and commercial ginger teas. The simultaneous analysis of 6-SHO and 6-GIN was carried out via RP-18 silica gel 60 F254S HPTLC plates. The mixture of green solvents, i.e., ethanol:water (6.5:3.5 v/v) was utilized as a mobile phase for the simultaneous analysis of 6-SHO and 6-GIN. The analysis of 6-SHO and 6-GIN was performed at λmax = 200 nm for 6-SHO and 6-GIN. The densitograms of 6-SHO and 6-GIN from traditional and ultrasonication-assisted extracts of ginger rhizome, commercial ginger powder, commercial capsules, and commercial ginger teas were verified by obtaining their single band at Rf = 0.36 ± 0.01 for 6-SHO and Rf = 0.53 ± 0.01 for 6-GIN, compared to standard 6-SHO and 6-GIN. The green RP-HPTLC method was found to be linear, in the range of 100–700 ng/band with R2 = 0.9988 for 6-SHO and 50–600 ng/band with R2 = 0.9995 for 6-GIN. In addition, the method was recorded as “accurate, precise, robust and sensitive” for the simultaneous quantification of 6-SHO and 6-GIN in traditional and ultrasonication-assisted extracts of ginger rhizome, commercial ginger powder, commercial capsules, and commercial ginger teas. The amount of 6-SHO in traditional extracts of ginger rhizome, commercial ginger powder, commercial capsules, and commercial ginger teas was obtained as 12.1, 17.9, 10.5, and 9.6 mg/g of extract, respectively. However, the amount of 6-SHO in ultrasonication-assisted extracts of ginger rhizome, commercial ginger powder, commercial capsules, and commercial ginger teas were obtained as 14.6, 19.7, 11.6, and 10.7 mg/g of extract, respectively. The amount of 6-GIN in traditional extracts of ginger rhizome, commercial ginger powder, commercial capsules, and commercial ginger teas were found as 10.2, 15.1, 7.3, and 6.9 mg/g of extract, respectively. However, the amount of 6-GIN in ultrasonication-assisted extracts of ginger rhizome, commercial ginger powder, commercial capsules, and commercial ginger teas were obtained as 12.7, 17.8, 8.8, and 7.9 mg/g of extract, respectively. Overall, the results of this study indicated that the proposed analytical technique could be effectively used for the simultaneous quantification of 6-SHO and 6-GIN in a wide range of plant extracts and commercial formulations

QUANTIFICATION OF GLYCYRRHIZIN BIOMARKER IN GLYCYRRHIZA GLABRA RHIZOME AND BABY HERBAL FORMULATIONS BY VALIDATED RP-HPTLC METHODS

Background: A simple and sensitive thin-layer chromatographic method has been established for quantification of glycyrrhizin in Glycyrrhiza glabra rhizome and baby herbal formulations by validated Reverse Phase HPTLC method. Materials and Methods: RP-HPTLC Method was carried out using glass coated with RP-18 silica gel 60 F254S HPTLC plates using methanol-water (7: 3 v/v) as mobile phase. Results: The developed plate was scanned and quantified densitometrically at 256 nm. Glycyrrhizin peaks from Glycyrrhiza glabra rhizome and baby herbal formulations were identified by comparing their single spot at Rf = 0.63 ± 0.01. Linear regression analysis revealed a good linear relationship between peak area and amount of glycyrrhizin in the range of 2000-7000 ng/band. Conclusion: The method was validated, in accordance with ICH guidelines for precision, accuracy, and robustness. The proposed method will be useful to enumerate the therapeutic dose of glycyrrhizin in herbal formulations as well as in bulk drug

Disposition kinetics and urinary excretion of ciprofloxacin in goats following single intravenous administration

We evaluated the pharmacokinetics of ciprofloxacin in serum (n = 6) and urine (n = 4) in goats following a single intravenous administration of 4 mg/kg body weight. The serum concentration-time curves of ciprofloxacin were best fitted by a two-compartment open model. The drug was detected in goat serum up to 12 h. The elimination rate constant (β) and elimination half-life (t1/2β) were 0.446 ± 0.04 h-1 and 1.630 ± 0.17 h, respectively. The apparent volume of distribution at steady state (Vdss) was 2.012 ± 0.37 l/kg and the total body clearance (ClB) was 16.27 ± 1.87 ml/min/kg. Urinary recovery of ciprofloxacin was 29.70% ± 10.34% of the administered dose within 36 h post administration. In vitro serum protein binding was 41% ± 13.10%. Thus, a single daily intravenous dose of 4 mg/kg is sufficient to maintain effective levels in serum and for 36 h in urine, allowing treatment of systemic, Gram-negative bacterial infections and urinary tract infections by most pathogens

A Green RP-HPTLC-Densitometry Method for the Determination of Diosmin in Pharmaceutical Formulations

Green analytical technologies for the determination of a bioactive compound diosmin (DIOM) in the real samples of pharmaceutical formulations and biological fluids are scarce in literature. Therefore, the present investigation was carried out to develop a novel, rapid, simple, and economical green “reversed phase high-performance thin-layer chromatography (RP-HPTLC)” method for the determination of DIOM in commercial tablets and in-house developed spray-dried microparticles (MPs). The quantification of DIOM was conducted via “RP-18 silica gel 60 F254S HPTLC plates”. The binary combination of green solvents, i.e., ethanol:water (5.5:4.5 v/v) was proposed as a green mobile phase. The analysis of DIOM was conducted in absorbance/reflectance mode of densitometry at λmax = 348 nm. The densitograms of DIOM from the commercial tablets and in-house developed spray-dried MPs were verified by recording their single band at Rf = 0.80 ± 0.02 compared to standard DIOM. Green RP-HPTLC method was observed as linear in the range of 100–700 ng/band with R2 = 0.9995. The proposed method was found as “accurate, precise, robust, and sensitive” for the determination of DIOM in the real samples of commercial tablets and in-house developed spray-dried MPs. The % content of DIOM in the real samples of commercial tablets and in-house developed spray-dried MPs was obtained as 99.06 and 101.30%, respectively. The recorded results of this research suggested that the green RP-HPTLC method can be effectively used for the routine analysis of DIOM in pharmaceutical products

Solubility Determination, Hansen Solubility Parameters and Thermodynamic Evaluation of Thymoquinone in (Isopropanol + Water) Compositions

This article studies the solubility, Hansen solubility parameters (HSPs), and thermodynamic behavior of a naturally-derived bioactive thymoquinone (TQ) in different binary combinations of isopropanol (IPA) and water (H2O). The mole fraction solubilities (x3) of TQ in various (IPA + H2O) compositions are measured at 298.2–318.2 K and 0.1 MPa. The HSPs of TQ, neat IPA, neat H2O, and binary (IPA + H2O) compositions free of TQ are also determined. The x3 data of TQ are regressed by van’t Hoff, Apelblat, Yalkowsky–Roseman, Buchowski–Ksiazczak λh, Jouyban–Acree, and Jouyban–Acree–van’t Hoff models. The maximum and minimum x3 values of TQ are recorded in neat IPA (7.63 × 10−2 at 318.2 K) and neat H2O (8.25 × 10−5 at 298.2 K), respectively. The solubility of TQ is recorded as increasing with the rise in temperature and IPA mass fraction in all (IPA + H2O) mixtures, including pure IPA and pure H2O. The HSP of TQ is similar to that of pure IPA, suggesting the great potential of IPA in TQ solubilization. The maximum molecular solute-solvent interactions are found in TQ-IPA compared to TQ-H2O. A thermodynamic study indicates an endothermic and entropy-driven dissolution of TQ in all (IPA + H2O) mixtures, including pure IPA and pure H2O

A High-Performance Thin-Layer Chromatographic Method for the Simultaneous Determination of Curcumin I, Curcumin II and Curcumin III in <i>Curcuma longa</i> and Herbal Formulation

Curcuma longa (turmeric) has traditionally been used in Ayurvedic, Unani and herbal drugs to cure numerous ailments. Due to the high demand, the quantitative standardization of herbal products is challenging to maintain their quality. We aim to develop a rapid, sensitive and validated high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination and quantification of curcumin I, curcumin II and curcumin III in C. longa and herbal formulation. The three standards were separated using centrifugal preparative thin-layer chromatography (CPTLC) silica gel and identified by different spectroscopic methods. The developed HPTLC method was validated by following ICH guidelines (linearity; limit of detection, LOD; limit of quantitation; accuracy; precision; and robustness). The calibration curves of both the compounds were linear (50–500 ng/spot), with a correlation coefficient (r2) of >999. The developed HPTLC method was effectively applied to the concurrent detection and quantification of curcumins I–III in fresh, dry rhizomes and the herbal formulation of C. longa extracts was obtained by hot and cold extraction methods

Ecofriendly Validated RP-HPTLCMethod for Simultaneous Determination of the Bioactive Sesquiterpene Coumarins Feselol and Samarcandin in Five Ferula Species Using Green Solvents

An environmentally friendly unreported rapid and simple reverse-phase high-performance thin-layer chromatography (RP-HPTLC) has been designed for the simultaneous determination of bioactive sesquiterpene coumarins feselol and samarcandin in the methanol extract of five Ferula species. The method was developed using glass plates coated with RP-18 silica gel 60 F254S and a green solvent system of ethanol-water mixture (8:2 v/v) as mobile phase. After development, the plates were quantified densitometrically at 254 for feselol and samarcandin. Feselol and samarcandin peaks from methanol extract of five Ferula species were identified by comparing their single band at Rf = 0.43 +/- 0.02 and Rf = 0.60 +/- 0.01, respectively. Valid linear relationships between the peak areas and concentrations of feselol and samarcandin in the range of 1000-7000 ng/band respectively were obtained. The method was subjected to the validation criteria of the international conference on harmonization (ICH) for precision, accuracy, and robustness. The new method provides an analytical tool to enumerate the therapeutic doses of feselol and samarcandin in herbal formulations and/or crude drugs. The obtained results indicated that F. drudeana was the richest species in the more active samarcandin, with 0.573% w/w, while F. duranii had the largest quantity of the less active feselol, 0.813% w/w. F. drudeana was superior to the other species in the sum of the two active compounds, 1.4552% w/w, and was consequently expected to be the most active aphrodisiac among the five studied species.Deanship of Scientific Research at Prince Sattam Bin Abdulaziz UniversityThis work was supported by Deanship of Scientific Research at Prince Sattam Bin Abdulaziz University