Novel oxygen-generation from electrospun nanofibrous scaffolds with anticancer properties: synthesis of PMMA-conjugate PVP–H2O2 nanofibers,characterization, and in vitro bio-evaluation tests

Released oxygen plays a critical role in reducing destructive tumor behavior. This study aims to utilize decomposed hydrogen peroxide as an oxygen source by conjugating it with polyvinylpyrrolidone (PVP). PVP–hydrogen peroxide complex (PHP) composed of different ratios of (PVP : H₂O₂) (0.5 : 1, 1 : 1, 1 : 1.5, 1 : 5, and 1 : 10) were successfully synthesized. PHP complex with a ratio of 1 : 1.5 was chosen as the optimized ratio, and it was incorporated into the polymethyl methacrylate (PMMA) nanofibrous scaffold via the electrospinning technique. Results have revealed that the PMMA–10% PHP complex provided a significant morphological structure of nanofibrous scaffolds. The mechanical properties of PMMA–10% PHP nanofibers showed the most suitable mechanical features such as Young''s modulus, elongation-at-break (%), and maximum strength, in addition to the highest degree of swelling. All PHP complex scaffolds released oxygen in a sustained manner. However, the PMMA–10% PHP complex gave the highest concentration of released-oxygen with (∼8.9 mg L⁻¹, after 2.5 h). PMMA–10% PHP nanofibers provided an ideal model for released-oxygen scaffold with anti-cancer effect and high selectivity for cancer cells, especially for breast cancer cells. Nanofibrous scaffolds with different composition revealed high cell viability for normal cells. Such outcomes support the suitability of using synthesized nanofibrous scaffolds as released-oxygen biomaterials to enhance cancer cells'' sensitivity and maximize the treatment effect.

Released oxygen plays a critical role in reducing destructive tumor behavior.     

Development of a fluorescent immunochromatographic assay based on quantum dots for the detection of fleroxacin

Fleroxacin (FLE) is a broad-spectrum fluoroquinolone antibiotic widely used in animal husbandry, veterinary medicine and aquaculture. Eating animal-derived foods with FLE residues can cause allergies, poisoning or drug resistance. The water-soluble QDs (CdSe/ZnS) and anti-FLE monoclonal antibody (mAb) were used to prepare a fluorescent probe by the method of N-(3-dimethylaminopropyl)-N′-ethylcarbodimide hydrochloride (EDC) activation. The fluorescent probe was characterized by dynamic light scattering (DLS). The better bioactivity and stability of the fluorescent probe was obtained under the pH value of 8.0, the molecule molar ratio of EDC (1 : 2000) and anti-FLE monoclonal antibodies (1 : 10). The control line (C line) and test line (T line) of a nitrocellulose (NC) filter membrane were sprayed with SPA (0.05 mg mL⁻¹) and FLE-OVA (1.4 mg mL⁻¹) solutions with optimal concentration, respectively. A novel method of fluorescent immunochromatographic assay based on quantum dots (QDs-ICA) in this work exhibited good accuracy, reproductivity and excellent specificity under the optimal experimental conditions. Compared with the traditional method for the visual detection of FLE, the developed QDs-ICA can successfully determine FLE residues in pork meat with a better cut-off value of 2.5 ng mL⁻¹. The QDs-ICA could be adapted for the rapid preliminary detection of FLE residues in pork meat for the first time.

(1) Water-soluble CdSe/ZnS QDs and an anti-FLE monoclonal antibody were used to prepare a fluorescent probe. (2) Primary rapid detection of FLE residues with visual fluorescent detection method.     

Remote loading of curcumin-in-modified β-cyclodextrins into liposomes using a transmembrane pH gradient

Curcumin (CRM) is a natural polyphenol with antioxidative, anti-inflammatory, and anticancer therapeutic properties. However, CRM therapeutic potential is limited by low water solubility and bioavailability. Intraliposomal remote loading describes the retention of drugs in liposome cores in response to transmembrane pH gradient. The current study describes for the first time the remote loading of CRM into liposomes using secondary (E-βCD) and tertiary (D-βCD) amino-modified β-cyclodextrins (βCDs) as carriers and solubilizers. βCDs were chemically modified to prepare the ionizable weak base functional group followed by forming a guest-host complex of CRM in the modified βCDs hydrophobic cavities via a solvent evaporation encapsulation technique. These complexes were then actively loaded into preformed liposomes, composed of DPPC/cholesterol (65/35 molar ratio) via pH gradient. The formation of CRM-βCDs inclusion complexes was characterized using UV-Vis spectroscopy, thermal analysis, and NMR spectroscopy. The complex stoichiometric ratio was determined to be 1 : 1 of CRM-βCDs based on Job''s plot which was also confirmed by the modified Benesi–Hildebrand equation with increasing probability of forming the 1 : 2 ratio of CRM-βCDs. The apparent formation constants (K_f) of 51.6, 100.9 and 55.4 mM⁻² were determined for CRM-βCD, CRM-E-βCD, and CRM-D-βCD complexes, respectively. Liposome size, charge and polydispersity index indicate the presence of a homogeneous population before and after active loading. The encapsulation efficiencies of CRM-βCD complexes into pH gradient preformed liposomes were 16.5, 51.1, and 41.7 for CRM-βCD, CRM-E-βCD, and CRM-D-βCD, respectively, showing more than 5 fold increase compared to normal liposomes. The current study provides a novel remote loading approach utilizing chemically modified cyclodextrins to incorporate hydrophobic drugs into liposomes.

The current study provides a novel remote loading approach utilizing chemically modified cyclodextrins to incorporate hydrophobic drugs into liposomes.     

Development of a colorless Centella asiatica (L.) Urb. extract using a natural deep eutectic solvent (NADES) and microwave-assisted extraction (MAE) optimized by response surface methodology

This study outlines a green process for Centella asiatica (L.) Urb. (CA) extraction. Natural deep eutectic solvents (NADESs) and microwave-assisted extraction (MAE) were combined to provide a high bioactive compound yield and high antioxidant activity. Among the NADESs evaluated, the combination of acetylcholine chloride : malic acid : water (1 : 2 : 2): water (40 : 60) was the best for extraction. These conditions provide high madecassoside (MS) (21.7 mg g⁻¹ dry weight) and asiaticoside (AS) (12.7 mg g⁻¹ dry weight) yields, with greater than 80% (v/v) EtOH (13.3 mg g⁻¹ MS and 7.80 mg g⁻¹ AS). In addition, the extracts from this process showed higher antioxidant activity (IC₅₀ = 0.26 mg mL⁻¹) than the CA aqueous EtOH and water extracts. Moreover, the color of the extract products was less green than that of the extracts prepared using EtOH and aqueous EtOH as solvents, which are suitable for cosmeceutical products. Response surface methodology (RSM) was used for MAE optimization. The ANOVA data from the central composition design (CCD) of RSM were fitted with quadratic models yielding acceptable R² (>0.93), adjusted R² (>0.87), predicted R² (>0.81), and nonsignificant lack of fit (p  > 0.05) values. The quadratic model was validated using optimal conditions (30 s, power 300 W, and a liquid to solid ratio 20 mL g⁻¹), and the model validation showed more than 80% accuracy in both MS and AS yields. This research presented an effective green process for CA extraction, which resulted in an environmentally friendly CA extract requiring little energy consumption and no organic solvents.

This study outlines a green process for Centella asiatica (L.) Urb. (CA) extraction.     

Magnetic graphene oxide-nano zero valent iron (GO–nZVI) nanohybrids synthesized using biocompatible cross-linkers for methylene blue removal

GO and nZVI have been used for removing different contaminants from aqueous solution; however, difficulty in the separation of GO, and the aggregation propensity of nZVI particles prevent them from having efficient practical applications. In this study, a green synthesis method was performed to prepare nanohybrids of GO and nZVI to provide an adsorbent with high adsorption efficiency that can be removed from aqueous solution easily by magnetic separation. GO–nZVI nanohybrids were synthesized by using biocompatible cross linkers named 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide (EDC) and N-hydroxysuccinimide (NHS). The effect of the nZVI ratio in the synthesized nanohybrids was studied at three different ratios of GO : nZVI, 1 : 1, 1 : 5 and 1 : 10. SEM/EDS, HRTEM, STEM/EDS, XRD, Raman, FTIR, and TGA analyses were conducted to provide physical and chemical properties of the adsorbents. The performance of nZVI and GO–nZVI nanohybrids as an adsorbent have been studied for methylene blue (MB) removal from an aqueous solution with an initial concentration of 12 mg L⁻¹ at adsorbent dosages of 0.1, 0.3, 0.5, and 1 mg mL⁻¹. Results indicated that GO–nZVI (1 : 5) provided the highest MB removal (99.1%) by using 10 mL of the 1 mg mL⁻¹ adsorbent. After regeneration of the GO–nZVI (1 : 5) nanohybrids with ethanol, 84.3%, 67.2%, and 63.0% of MB removal were achieved in the first to third regeneration cycle. Results also showed that the GO–nZVI nanohybrids were not affected by aggregation compared to nZVI.

A green synthesis method was used to prepare GO–nZVI nanohybrids to provide an adsorbent with high adsorption efficiency that can be removed from aqueous solutions easily by magnetic separation.     

A microporous Ce-based MOF with the octahedron cage for highly selective adsorption towards xenon over krypton

The collection of high-purity noble gases with recyclable nuclides provides substantial economic benefits and minimizes the risk of environmental pollution, which is a future development tendency for nuclear industries. Here, Ce-SINAP-1, with its radiation-resistance (up to 20 kGy of γ-ray irradiation) and suitable pore channels for the separation of noble gases (Ar, Kr and Xe), was synthesized. Ce-SINAP-1 exhibited the selective adsorption of Xe (2.02 mmol g⁻¹) over Kr (0.67 mmol g⁻¹) and Ar (0.27 mmol g⁻¹) at 293 K (1 bar) with a Henry''s selectivity of 8.24 (Xe/Kr), and an ideal adsorbed solution theory selectivity of 14.9 (Xe : Kr 20 : 80). The result of the dynamic breakthrough experiment also indicates a good separation for Xe/Kr with Ar.

A high selectivity of Xe over Kr at 293 K was achieved by a 3D Ce-based organic framework due to the geometric features. Favorable thermal stability and ionizing radio-resistance render it a promising candidate for radioactive inert gases treatment.     

Betaine host–guest complexation with a calixarene receptor: enhanced in vitro anticancer effect

p-Sulfonatocalix[n]arenes have shown excellent potential for accommodating chemotherapeutic drugs through host–guest complexation and enhancing their anticancer activity. Betaine has been reported to exert an anticancer effect at high concentrations. In order to increase its concentration in cancer cells, we have complexed it with p-SC4, which releases its content in an acidic environment typical of cancer tissue. In this work, a host–guest complex of the chemically stable, natural, and safe active methyl donor (betaine) and p-sulfonatocalix[4]arenes (p-SC4) was designed and characterized using ¹H NMR, UV, Job''s plot analysis, DFT calculations, and molecular modeling for use in cancer therapeutics. The peak amplitude of the prepared host–guest complexes was linearly proportional to the concentration of betaine in the range of 1.0 × 10⁻⁵ M⁻¹ to 2.5 × 10⁻⁴ M⁻¹. The reaction stoichiometry between p-SC4 and betaine in the formed complex was 1 : 1. The stability constant for the complex is 8.9 × 10⁴ M⁻¹ which corresponds to a complexation free energy of −6.74 kcal mol⁻¹. Complexation between betaine and p-SC4 was found to involve the insertion of the trimethylammonium group of betaine into the p-SC4 cavity, as supported by the experimental data. The complex displayed enhanced cytotoxic activities against breast adenocarcinoma cells (MCF-7) and cervical cancer cells (HeLa) compared to free betaine. In conclusion, the host–guest complexation of betaine with p-SC4 increases its concentration in cancer cells, which warrants further investigation for cancer therapy.

The complexation between p-SC4 and betaine was thoroughly investigated experimentally and computationally. A remarkable enhancement of the cytotoxic activities of betaine/p-SC4 complex was observed as compared to free betaine.     

Rapid electrochemical sensor for uranium(vi) assessment in aqueous media

The significance of reliable monitoring of uranium levels in water recourses calls for the development of time-saving, robust, and accurate methods for its estimation. In this view, the current study describes the design and analytical parameters of a potentiometric membrane sensor for uranium(vi) ions. The sensor is based on a new Schiff base derivative, as an ionophore, that was synthesized and structurally characterized by elemental, FTIR, and ¹HNMR analyses. The impact of the membrane constituents was studied and the membrane composition of PVC (32.50) : o-NPOE (65.00) : ionophore (2.00) :  KTpClPB (0.50) (%, w/w) achieved the optimal performance. A Nernestian response was observed for uranium(vi) ions within the concentration range 1.00 × 10⁻⁶ to 1.00 × 10⁻¹ mol L⁻¹. The sensor revealed a low detection limit of 3.90 × 10⁻⁷ mol L⁻¹ with satisfactory reproducibility. Stable and reproducible potentials were obtained within a short time (9 s) over the pH range 2.10–4.21. The impact of possible competing ions was investigated and the selectivity coefficients revealed appropriate selectivity for uranium(vi) ions over various cations without significant interference. The sensor''s performance was examined by determining the amount of uranium(vi) in water samples and the results showed no significant differences from those obtained by the ICP-OES method.

A new Schiff base was synthesized and applied as ionophore to construct potentiometric sensor for uranium(vi) determination.     

Development and validation of a sensitive LC-MS/MS method for pioglitazone: application towards pharmacokinetic and tissue distribution study in rats

In the present study, a sensitive LC-MS/MS method was developed and validated to measure pioglitazone (PGZ) concentrations in rat plasma and tissues. The chromatographic separation was achieved by using a YMC Pro C₁₈ column (100 mm × 4.6 mm, 3μ) with a mobile phase consisting of formic acid (0.1% v/v) and acetonitrile (5 : 95) at a flow rate of 0.7 mL min⁻¹ and injection volume of 10 μL (IS: rosiglitazone). Mass spectrometric detection was done using triple quadrupole mass spectrometry using the ESI interface operating in a positive ionization mode. The developed method was validated over a linearity range of 1–500 ng mL⁻¹ with detection and a lower quantification limit of 0.5 ng mL⁻¹ and 1 ng mL⁻¹. The method accuracy ranged from 95.89–98.78% (inter-day) & 93.39–97.68% (intra-day) with a precision range of 6.09–8.12% for inter-day & 7.55–9.87% for intra-day, respectively. The PGZ shows the highest C_max of 495.03 ng mL⁻¹ in plasma and the lowest C_max, 24.50 ± 2.71 ng mL⁻¹ in bone. The maximum T_max of 5.00 ± 0.49 h was observed in bone and a minimum of 1.01 ± 0.05 h in plasma. The AUC_{(0–24 h and 0–∞)} values are highest in plasma (1056.58 ± 65.78 & 1069.38 ± 77.50 ng h⁻¹ mL⁻¹) and lowest in brain (166.93 ± 15.70 &167.12 ± 16.77 ng h⁻¹ mL⁻¹), and the T_1/2 was highest in plasma (5.62 ± 0.74 h) and lowest in kidney (2.78 ± 0.19). The developed method was successfully used to measure the PGZ pharmacokinetic and tissue distribution. Further, the developed method could be utilized for validating target organ (adipose tissue) specific delivery of PGZ (nano-formulations) in addition to conventional dosage forms.

The developed method was investigated for target and off-target distribution of pioglitazone and could be applied to validate the site-specific delivery systems.     

A novel ultrasensitive surface plasmon resonance-based nanosensor for nitrite detection

Nitrite is a common food additive, however, its reduction product, nitrosamine, is a strong carcinogen, and hence the ultra-sensitive detection of nitrite is an effective means to prevent related cancers. In this study, different sized gold nanoparticles (AuNPs) were modified with P-aminothiophenol (ATP) and naphthylethylenediamine (NED). In the presence of nitrite, satellite-like AuNPs aggregates formed via the diazotization coupling reaction and the color of the system was changed by the functionalized AuNPs aggregates. The carcinogenic nitrite content could be detected by colorimetry according to the change in the system color. The linear concentration range of sodium nitrite was 0–1.0 μg mL⁻¹ and the detection limit was determined to be 3.0 ng mL⁻¹. Compared with the traditional method, this method has the advantages of high sensitivity, low detection limit, good selectivity and can significantly lower the naked-eye detection limit to 3.0 ng mL⁻¹. In addition, this method is suitable for the determination of nitrite in various foods. We think this novel designed highly sensitive nitrate nanosensor holds great market potential.

A satellite-like AuNP aggregate-based nitrite detection nanosensor was designed via diazotization coupling reaction and can significantly lower the naked-eye detection limit to 3.0 ng mL⁻¹. This nanosensor has important applications in food detection and cancer prevention.     

One pot synthesis of two cobalt(iii) Schiff base complexes with chelating pyridyltetrazolate and exploration of their bio-relevant catalytic activities

Two new cobalt(iii) tetrazolato complexes [Co(L¹)(PTZ)(N₃)] (1) and [Co(L²)(PTZ)(N₃)] (2) {where H₂L¹ = 2((3-(methylamino)propylimino)methyl)-6-methoxyphenol, H₂L² = 2((3-(dimethylamino)propylimino)methyl)-6-ethoxyphenol and HPTZ = 5-(2-pyridyl)tetrazole}, have been synthesized via in situ 1,3-dipolar cycloaddition reaction of 2-cyanopyridine and sodium azide in the presence of cobalt(ii) nitrate hexahydrate and respective Schiff bases in the open atmosphere. The structures of both complexes have been confirmed by single crystal X-ray diffraction studies. Features of noncovalent interactions in the solid state of both complexes have been studied by means of DFT and MEP calculations and characterized using Bader''s theory of “atoms in molecules” (AIM). These complexes act as biomimetic catalysts promoting the aerobic oxidation of 3,5-di-tert-butylcatechol (3,5-DTBC) to the corresponding o-benzoquinone at room temperature. The reaction follows Michaelis–Menten enzymatic reaction kinetics with turnover numbers of ∼0.030 s⁻¹ in an acetonitrile–methanol (2 : 1) mixture. Both complexes are also reactive towards aerobic oxidation of o-aminophenol in acetonitrile–methanol (2 : 1) with turnover numbers ∼0.095 s⁻¹.

Two cobalt(iii) tetrazolato complexes have been synthesized and characterized. Noncovalent interactions have been analysed by DFT and MEP calculations and characterized using Bader''s theory of AIM. Both complexes catalyze the aerial oxidation of 3,5-DTBC and OAPH.     

Development of a HPLC-FL method to determine benzaldehyde after derivatization with N-acetylhydrazine acridone and its application for determination of semicarbazide-sensitive amine oxidase activity in human serum

A novel fluorescence labeling reagent N-acetylhydrazine acridone (AHAD) was designed and synthesized. A highly sensitive high performance liquid chromatography (HPLC) method coupled with fluorescence detection to determine benzaldehyde after derivatization with AHAD was developed. Optimum derivatization was obtained at 40 °C for 30 min with trichloroacetic acid as catalyst. Benzaldehyde derivative was separated on a reversed-phase SB-C18 column in conjunction with a gradient elution and detected by fluorescence detection at excitation and emission wavelengths of 371 nm and 421 nm. The established method exhibited excellent linearity over the injected amount of benzaldehyde of 0.003 to 5 nmol mL⁻¹. The method was successfully applied to the determination of serum semicarbazide-sensitive amine oxidase (SSAO) activity in humans. SSAO is a significant biomarker because serum SSAO activity is elevated in patients with Alzheimer''s disease, vascular disorders, heart disease and diabetes mellitus. It was demonstrated that the SSAO activity of the hyperglycemic group (60 ± 4 nmol mL⁻¹ h⁻¹) was significantly higher than that of normal blood sugar group (44 ± 4 nmol mL⁻¹ h⁻¹) with P < 0.05.

A highly sensitive HPLC-FL method to determine semicarbazide-sensitive amine oxidase activity was developed utilizing AHAD as the novel fluorescence labeling reagent.     

Development of a selective and sensitive colour reagent for gold and silver ions and its application to desktop scanner analysis

Desktop scanners can be favorable alternatives to sophisticated spectrophotometers for the assessment of analytes in complex real samples. Distinctively, our method has been thoroughly investigated, optimized, validated and successfully applied to the assessment of silver and gold in complex real samples, applying syringal rhodanine (SR) as a novel specifically tailored chromogenic reagent and using a desktop scanner as a versatile sensor. Maximum colour absorbance was obtained in the presence of cetylpyridinium chloride (CPC) and cetyltrimethylammonium chloride (CTAC) for silver and gold chelates, respectively. For each metal ion, two ternary complexes were formed depending on the SR concentration with stoichiometries of 1 : 1 : 1 and 1 : 2 : 3 (Ag–SR–CPC) and 1 : 2 : 3 and 1 : 3 : 4 (Au–SR–CTAC), respectively. The methods adhered to Beer''s law for 0.15–2.5 and 0.15–2.25 μg mL⁻¹ with detection limits of 0.0089 and 0.0163 μg mL⁻¹ for silver and gold, respectively. The molar absorptivities were 3.63 × 10⁴ and 6.15 × 10⁴ L mol⁻¹ cm⁻¹ at 550 nm and 554 nm, with Sandell''s sensitivity indexes of 0.0029 and 0.0032 μg cm⁻², respectively. The method was successfully applied to the assessment of silver and gold in a wide range of complex environmental samples.

Desktop scanners can be favorable alternatives to sophisticated spectrophotometers for the assessment of analytes in complex real samples.     

Spermidine enhanced resistance of Chlorella to high levels of CO2 and light intensity for improving photosynthetic growth rate

In order to promote the photosynthetic growth rate of Chlorella in the presence of flue gas CO₂ from coal-fired power plants, spermidine was first used to enhance cellular resistance to a high CO₂ concentration (15%) and high light intensity (30 000 lux). It was found that low concentrations (100–300 μM) of spermidine significantly enhanced the photosynthetic growth rate of Chlorella. The accelerated cell division decreased the cell diameter from 3.64 μm to 2.71 μm and the fractal dimension from 1.60 to 1.49, and the activity of total superoxide dismutase (T-SOD) increased from 0.48 U mL⁻¹ to 5.33 U mL⁻¹. Expression levels of key enzymes of photosystems I and II, ATP synthase and transportase markedly increased, thereby enhancing the electron transport and energy supply that reduced oxidative damage. Finally, an enhanced cellular resistance to the high CO₂ concentration and high light intensity increased the biomass yield from 0.11 g L⁻¹ to 1.71 g L⁻¹ (300 μM).

Spermidine enhanced resistance of Chlorella to high levels of CO₂ and light intensity.     

Al(iii)-responsive “off–on” chemosensor based on rhodamine derivative and its application in cell imaging

In this work, a new rhodamine chemosensor (P) with excellent photochromic properties upon vis irradiation was designed and synthesized. The fabricated chemosensor P could detect Al³⁺via the opening of the spirolactam ring of the rhodamine unit with high selectivity and sensitivity. The spirolactam ring opening was confirmed by NMR and infrared spectroscopy. Upon binding with Al³⁺, the generated 1 : 1 P-Al³⁺ complex, confirmed by Job''s plot titrations and mass spectrometry analysis, could exhibit a remarkable fluorescence enhancement with a limit of detection (LOD) of 0.16 μM. Furthermore, the sensing of P to Al³⁺in vivo was also studied quantitatively and qualitatively in detail, and the results showed that the coordination between P with Al³⁺ was reversible in living cells.

In this work, a new rhodamine chemosensor (P) with excellent photochromic properties upon vis irradiation was designed and synthesized.     

A new class of fluorogenic thiazolo[2,3-b]quinazolinone receptor: selective detection towards mercury and hydrogen bisulfate ions in aqueous medium

A series of fluorophoric and structurally diverse thiazoloquinazoline derivatives were synthesized in a one-pot multicomponent cascade reaction using a microwave irradiation technique. The unique structural arrangement of the synthesized compounds encouraged us to design a new type of bioactive molecular receptor. This receptor interacts with HSO₄⁻ in 1 : 1 and Hg²⁺ in 1 : 2 binding stoichiometric ratios resulting in a change in fluorescence as well as absorption spectra in aqueous medium. The ion bonded receptor complex possibly enhances the fluorescence signal of the receptor via H-bonded complex formation with HSO₄⁻ ions and co-ordinate complex formation with Hg²⁺ ions.

Fluorophoric thiazoloquinazoline derivatives were synthesized under microwave assisted one-pot three-component cascade reaction. Owing to their unique structural arrangement, a new bioactive molecular receptor was developed for HSO⁴⁻ and Hg²⁺ ions.     

Quality by design approach for green HPLC method development for simultaneous analysis of two thalassemia drugs in biological fluid with pharmacokinetic study

This work implements a combined experimental approach of analytical quality-by-design (AQbD) and green analytical chemistry (GAC) to develop an HPLC method for simultaneous determination of the two thalassemia drugs, deferasirox (DFX) and deferiprone (DFP), in biological fluid for the first time. This integration was designed to maximize efficiency and minimize environmental impacts, as well as energy and solvent consumption. To accomplish this goal, an analytical quality-by-design approach was performed, beginning with quality risk assessment and scouting analysis, followed by Placket–Burman design screening for five chromatographic parameters. Critical method parameters were thoroughly recognized and then optimized by using a two levels-three factors custom experimental design to evaluate the optimum conditions that achieved the highest resolution with acceptable peak symmetry within the shortest run time. The desirability function was used to define the optimal chromatographic conditions, and the optimal separation was achieved using an XBridge® HPLC RP-C18 (4.6 × 250 mm, 5 μm) column with ethanol : acidic water at pH 3.0 adjusted by phosphoric acid in the ratio of (70 : 30, v/v) as the mobile phase at a flow rate of 1 mL min⁻¹ with UV detection at 225 nm at a temperature of 25 °C. Linearity was obtained over the concentration range of 0.30–20.00 μg mL⁻¹ and 0.20–20.00 μg mL⁻¹ for DFX and DFP, respectively, using 20.00 μg mL⁻¹ ibuprofen (IBF) as an internal standard. The established method''s greenness profile was evaluated and measured using various assessment tools, and the developed method was green. For the validation of the developed method, FDA recommendations were followed, and all the results obtained met the acceptance criteria. The suggested method was successfully used to study the pharmacokinetic parameters of DFX and DFP in rat plasma. Due to the substantial increase in bioavailability of the two iron chelating drugs, the results from this study strongly recommend their co-administration.

This work implements a combined experimental approach of analytical quality-by-design and green analytical chemistry to develop an HPLC method for simultaneous determination of the two thalassemia drugs, deferasirox and deferiprone in biological fluid for the first time.     

Purification,structure and anti-oxidation of polysaccharides from the fruit of Nitraria tangutorum Bobr.

In this paper, polysaccharides were extracted from the fruits of Nitraria tangutorum Bobr. (NTWP) using a hot water extraction method and extraction conditions were optimized by RSM. The optimal conditions were determined as follows: extraction time 7 h, extraction temperature 60 °C, ratio of water to raw material 15 : 1, and with these conditions, the yield was 14.01 ± 0.11%. After purification using DEAE-cellulose column and Sephadex G-200 column, NTWP-II was successfully obtained. The results of GC-MS and SEC-LLS analysis suggested that monosaccharide composition of NTWP-II was composed of Rha, Ara, Man, Glc and Gal with the molar ratio of 1.14 : 2.5 : 3.00 : 2.69 : 5.28 and M_w, M_w/M_n and R_z 2.29 × 10⁵, 1.32, 15.22. The detailed structure of NTWP-II was characterized by FT-IR, NMR. Based on these analyses, the structure of the repeating unit of NTWP-II was established.

Antioxidant activity of NTWP-II, evaluated in vitro, indicates that NTWP-II has good potential as a natural antioxidant used in the food industry.     

Ultrasensitive fluorescent aptasensor for MUC1 detection based on deoxyribonuclease I-aided target recycling signal amplification

A novel sensing strategy for sensitive detection of mucin 1 protein (MUC1) based on deoxyribonuclease I-aided target recycling signal amplification was proposed. In this paper, in the absence of MUC1, the MUC1 aptamer is absorbed on the surface of graphene oxide (GO) via π-stacking interactions. This results in quenching of the fluorescent label and no fluorescence signal is observed. Upon adding MUC1, the probe sequences could be specifically recognized by MUC1, leading to an increase in the fluorescence intensity. The detection limit is as low as 10 pg mL⁻¹, and a linear range from 50 pg mL⁻¹ to 100 ng mL⁻¹. The assay is specific and sensitive, and successfully applied to the determination of MUC1 in spiked human serum, urine and saliva. Importantly, the proposed aptasensing strategy has great potential in detecting various protein and even cancer cells.

A novel sensing strategy for sensitive detection of mucin 1 protein (MUC1) based on deoxyribonuclease I-aided target recycling signal amplification was proposed.     

Green innovative fluorescence approach for the feasible and reliable assay of thiol-containing drugs; captopril as a model

In the present study, a novel spectrofluorimetric approach was designed for the analysis of captopril as a thiol-containing compound. The approach is based on the formation of a ternary fluorescent compound between the target thiol compound, ortho-phthaldehyde, and a suitable primary amine-containing compound. The produced 1-thio-alkyl-isoindole derivative exhibited very high emission activity in a faintly alkaline aqueous solution that could be monitored at 448 nm (excitation at 334 nm). 2-Amino-6-methyl-6-hydroxy-heptane was selected as the primary amine candidate that gave the high fluorescence intensity with the stability of the formed product. At the optimal experimental condition, the intensity of fluorescence of the formed product was linearly related to the concentration of captopril in 20–450 ng mL⁻¹ range. Commercial pharmaceutical tablets were analyzed, and the obtained results agreed with those of the published method regarding precision and accuracy. The mechanism of the reaction was discussed. In addition, the greenness of the approach was rated following eco-scale criteria.

The excitation and emission spectra of the reagent blank and the reaction product of captopril (200 ng mL⁻¹) with o-phthaldehyde/heptaminol.