Reversed‐phase vortex‐assisted liquid–liquid microextraction: A new sample preparation method for the determination of amygdalin in oil and kernel samples

A novel, simple, and rapid reversed‐phase vortex‐assisted liquid–liquid microextraction coupled with high‐performance liquid chromatography has been introduced for the extraction, clean‐up, and preconcentration of amygdalin in oil and kernel samples. In this technique, deionized water was used as the extracting solvent. Unlike the reversed‐phase dispersive liquid–liquid microextraction, dispersive solvent was eliminated in the proposed method. Various parameters that affected the extraction efficiency, such as extracting solvent volume and its pH, vortex, and centrifuging times were evaluated and optimized. The calibration curve shows good linearity (r² = 0.9955) and precision (RSD < 5.2%) in the range of 0.07–20 μg/mL. The limit of detection and limit of quantitation were 0.02 and 0.07 μg/mL, respectively. The recoveries were in the range of 96.0–102.0% with relative standard deviation values ranging from 4.0 to 5.1%. Unlike the conventional extraction methods for plant extracts, no evaporative and re‐solubilizing operations were needed in the proposed technique.     

Abeliaside,a new phenolic glucoside from Abelia triflora

A new phenolic glucoside, abeliaside, along with four known compounds, 5,6,7,4′-tetrahydroxy flavones, caffeic acid, 4-O-caffeoylquinic acid and caffeic acid glucoside, was isolated from the leaves of Abelia triflora R. Br. (Caprifoliaceae). The structure of the new compound was elucidated by different spectroscopic techniques. Compounds 1–5 were assayed for their anticancer activities against two cancerous human cell lines, MCF-7 and PC-3 cells, and normal Vero cell line using the crystal violet staining method. From the results it could be seen that caffeic acid possessed the highest anticancer effect against MCF-7 (IC₅₀: 17 μg/mL) and PC-3 (IC₅₀: 20.1 μg/mL) compared to vinblastine sulphate as reference drug (IC₅₀: 4.6, 2.8 μg/mL). The other compounds showed weak anticancer activity on both cell lines.     

Synthesis of a graphene‐based nanocomposite for the dispersive solid‐phase extraction of vancomycin from biological samples

The approach of this work was to study the capability of graphene‐based materials in the field of biological sample preparation. A polypyrrole/graphene composite was synthesized and characterized. The potential of the nanocomposite was investigated as a sorbent in dispersive solid‐phase extraction followed by high‐performance liquid chromatography with UV detection for vancomycin as a model drug. The effect of different parameters influencing extraction efficiency such as sample pH and sample volume, ionic strength, extraction time, type, and volume of desorption solvent and desorption time were investigated. A comparison study was also conducted between polypyrrole/graphene and some different novel and classic sorbents. Under optimized conditions, the calibration curve for vancomycin showed linearity in the range of 0.05–10 μg/mL. In addition, limits of detection, and quantification were 0.003 and 0.01 μg/mL, respectively. The intraday and interday relative standard deviations at a concentration of 0.05 μg/mL (n = 3) were 1.6 and 2.1%, respectively. Furthermore, the proposed method was successfully applied for the determination of vancomycin in plasma and urine samples. The relative recoveries indicated the feasibility of graphene‐based sorbents in biological sample analysis.     

Suitability of dispersive liquid–liquid microextraction for the in situ silylation of chlorophenols in water samples before gas chromatography with mass spectrometry

Trace analysis of chlorophenols in water was performed by simultaneous silylation and dispersive liquid–liquid microextraction followed by gas chromatography with mass spectrometry. Dispersive liquid–liquid microextraction was carried out using an organic solvent lighter than water (n‐hexane). The effect of different silylating reagents on the method efficiency was investigated. The influence of derivatization reagent volume, presence of catalyst and derivatization/extraction time on the yield of the derivatization reaction was studied. Different parameters affecting extraction efficiency such as kind and volume of extraction and disperser solvents, pH of the sample and addition of salt were also investigated and optimized. Under the optimum conditions, the calibration graphs were linear in the range of 0.05–100 ng/mL and the limit of detection was 0.01 ng/mL. The enrichment factors were 242, 351, and 363 for 4‐chlorophenol, 2,4‐dichlorophenol, and 2,4,6‐trichlorophenol, respectively. The values of intra‐ and inter‐day relative standard deviations were in the range of 3.0–6.4 and 6.1–9.9%, respectively. The applicability of the method was investigated by analyzing water and wastewater samples.     

Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples

In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra‐trace amounts of rhodium after adsorption of its 2‐(5‐bromo‐2‐pyridylazo)‐5‐diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015–0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values.     

Enabling arbitrary wavelength frequency combs on chip

A necessary condition for generation of bright soliton Kerr frequency combs in microresonators is to achieve anomalous group velocity dispersion (GVD) for the resonator modes. This condition is hard to implement in the visible as well as ultraviolet since the majority of optical materials are characterized with large normal GVD in these wavelength regions. We overcome this challenge by borrowing ideas from strongly dispersive coupled systems in solid state physics and optics. We show that photonic compound ring resonators can possess large anomalous GVD at any desirable wavelength, even if each individual resonator is characterized with normal GVD. Based on this concept, we design a mode‐locked frequency comb with thin‐film silicon nitride compound ring resonators in the vicinity of the rubidium D₁ line (794.6 nm) and propose to use this optical comb as a flywheel for chip‐scale optical clocks.

     

Ultra-trace determination of arsenic species in environmental waters,food and biological samples using a modified aluminum oxide nanoparticle sorbent and AAS detection after multivariate optimization

We describe a simple and efficient method for solid phase extraction and speciation of trace quantities of arsenic. It is based on the use of functionalized aluminum oxide nanoparticles and does not require any oxidation or reduction steps. The experimental parameters affecting extraction and quantitation were optimized using fractional factorial design methods. Adsorbed arsenic was eluted from the sorbent with 1 M hydrochloric acid and determined by graphite furnace atomic absorption spectrometry. Preconcentration factors up to 750 were achieved depending on the sample volume. Studies on potential interferences by various anions and cations showed the method to be highly selective. Under optimum conditions, the calibration plots are linear in the 5.0 to 280 ng L⁻¹ and 8.0 to 260 ng L⁻¹ concentration ranges for As(III) and total arsenic, respectively. The detection limits (calculated for S/N ratios of 3) are 1.81 and 1.97 ng L⁻¹ for As(III) and total arsenic, respectively. The method was successfully applied to the determination and speciation of arsenic in (spiked) environmental, food and biological samples and gave good recoveries. The method was validated using a certified geological reference material.

Novel functionalized Al₂O₃ nanoparticles were synthesized and used for speciation and determination of arsenic in different samples. The experimental variables were optimized using fractional factorial design that can save time and operational costs.

     

Modified carbon nanotubes as a sorbent for solid-phase extraction of gold,and its determination by graphite furnace atomic absorption spectrometry

A simple, sensitive and accurate method was developed for solid-phase extraction and preconcentration of trace levels of gold in various samples. It is based on the adsorption of gold on modified oxidized multi-walled carbon nanotubes prior to its determination by graphite furnace atomic absorption spectrometry. The type and volume of eluent solution, sample pH value, flow rates of sample and eluent, sorption capacity and breakthrough volume were optimized. Under these conditions, the method showed linearity in the range of 0.2–6.0 ng L⁻¹ with coefficients of determination of >0.99 in the sample. The relative standard deviation for seven replicate determinations of gold (at a level of 0.6 ng L⁻¹) is ±3.8 %, the detection limit is 31 pg L⁻¹ (in the initial solution and at an S/N ratio of 3; for n = 8), and the enrichment factor is 200. The sorption capacity of the modified MWCNTs for gold(III) is 4.15 mg g⁻¹. The procedure was successfully applied to the determination of gold in (spiked) water samples, human hair, human urine and standard reference material with recoveries ranging from 97.0 to 104.2 %.

A sorbent based on modified carbon nanotubes was prepared and used to extract gold ion from various samples prior to its determination by graphite furnace atomic absorption spectrometry

     

Fisetin Inhibits UVB‐induced Cutaneous Inflammation and Activation of PI3K/AKT/NFκB Signaling Pathways in SKH‐1 Hairless Mice

Solar ultraviolet B (UVB) radiation has been shown to induce inflammation, DNA damage, p53 mutations and alterations in signaling pathways eventually leading to skin cancer. In this study, we investigated whether fisetin reduces inflammatory responses and modulates PI3K/AKT/NFκB cell survival signaling pathways in UVB‐exposed SKH‐1 hairless mouse skin. Mice were exposed to 180 mJ cm^?2 of UVB radiation on alternate days for a total of seven exposures, and fisetin (250 and 500 nmol) was applied topically after 15 min of each UVB exposure. Fisetin treatment to UVB‐exposed mice resulted in decreased hyperplasia and reduced infiltration of inflammatory cells. Fisetin treatment also reduced inflammatory mediators such as COX‐2, PGE₂ as well as its receptors (EP1–EP4) and MPO activity. Furthermore, fisetin reduced the level of inflammatory cytokines TNFα, IL‐1β and IL‐6 in UVB‐exposed skin. Fisetin treatment also reduced cell proliferation markers as well as DNA damage as evidenced by increased expression of p53 and p21 proteins. Further studies revealed that fisetin inhibited UVB‐induced expression of PI3K, phosphorylation of AKT and activation of the NFκB signaling pathway in mouse skin. Overall, these data suggest that fisetin may be useful against UVB‐induced cutaneous inflammation and DNA damage.