Phase pH Values Research Articles

Preventing emulsification during rare earths solvent extraction by the addition of Span 80 to enhance the interfacial stability of the P507 oil droplets

The demand for rare earth elements is increasing daily with rapid economic development, thereby increasing the requirements for its separation and purification technologies. The major method for purification and separation of rare earth elements in the industry is currently solvent extraction. In the actual production process, emulsification often occurs because of improper control of the organic phase, aqueous phase properties or operating conditions, and resulting in resource wastage and environmental pollution. This has become an issue that restricts the development of the rare earths industry. To prevent emulsification during rare earths solvent extraction, the organic structure of the P507-kerosene solution was regulated by the addition of Span 80 as a regulator. This study investigated the effects of Span 80 content, P507 concentration, saponification degree and the amount of pre-loading rare earth elements in the organic phase after adding Span 80 on the extraction efficiency of Er3+ and oil content in the raffinates. The results demonstrated that when the content of Span 80 was 6 %, the saponification degree of P507 in the organic phase was 10 %, the concentration of Er3+ in the aqueous phase was 0.5 g /L, the pH value in the aqueous phase was 3, the phase ratio (VO: VA) was 1:2, the extraction efficiency could still reach more than 99 %, and the oil content in the raffinates was 13.9 mg/L. The results demonstrated that the final extraction efficiency did not decrease; however, the extraction rate of rare earth elements did. Further, the oil content in the raffinates decreased greatly after the addition of Span 80. The mechanism was investigated using Fourier-transform infrared (FTIR) spectroscopy and atomic force microscopy (AFM). The interfacial stability of P507 oil droplets was enhanced by the addition of Span 80. Emulsification was, thus, effectively prevented and the dissolution loss of the organic phase was greatly reduced. The results provide a novel method for preventing emulsification during rare earths extraction at the source, and a novel idea for preventing resource loss and protecting the ecological environment.

Removal of Methylene Blue Dye from Aqueous Solutions Using Polymer Inclusion Membrane Containing Calix[4]pyrrole.

The effective purification of aqueous solutions of methylene blue dye was tested using polymer inclusion membranes (PIMs) that contained cellulose triacetate (CTA) as a polymer base, o-nitrophenyl octyl ether (o-NPOE) as a plasticizer, and meso-tetra methyl tetrakis-[methyl-2-(4-acetlphenoxy)] calix[4]pyrrole (KP) as a carrier. Scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy were used to define the microstructure and surface of PIMs. Experimental results showed that, with an increased concentration of methylene blue in an aqueous solution, the removal percentage also increased. Further observation showed that the flux increased with the rise in the source phase pH values from 3 to 10. The carrier and plasticizer content in the membrane significantly influenced the membrane's transport properties. The optimal composition of the membrane in percent by weight for KP was 74% plasticizer; 18% support, and 8% carrier. The maximum MB removal (93.10%) was achieved at 0.10 M HCl solution as the receiving phase. It was shown that the membrane with optimal composition showed good reusability and enabled the easy and spontaneous separation of methylene blue from aqueous solutions.

Developement and Stability Evaluation of Natural Topical Formulations Containing Pinus sibirica Essential Oil

Abstract Pinus sibirica (P. sibirica) is used in folk medicine for centuries in treatment of various diseases due to its anti-inflammatory, antioxidant, and antimicrobial activity. The present study was focused on formulating semi-solid topical cream and gel preparations with P. sibirica essential oil (EOPS) and on evaluation of their stability during three months of storage. After preparation of semi-solid formulations (cream and gel), we followed parameters such as organoleptic characteristics, pH values, electrical conductivity, phase separation, washability, swelling index and microbiological contamination. Tests for physical and microbiological stability were performed considering different storage conditions at temperature (4±2° C, 25±2°C and 40±2°C) for 12 weeks. All test were performed at sampling time points of 7th, 30th, 60th, 90th day after storage. Cream with EOPS was white colour, it is homogenous with pleasant odor characteristic to used EOPS while gel with EOPS was transparent, it is homogenous with specific odor. After application to skin, EOPS cream was leaving non-greasy film while gel with EOPS was leaving sticky film and cooling effect. In all tested samples, we observed no phase separation and pH values were optimal for skin application. During three months of storage at different conditions, all tested formulations were stable and addition of EOPS did not cause any changes in followed parameters. Both cream and gel formulation remained stable since we did not notice any significant changes in all followed parameters during storage at different temperatures. Addition of 0.5% of EOPS did not change visual, sensory and microbial properties of formulations.

Properties and reaction mechanism of magnesium phosphate cement modified by calcium lactate

The properties of magnesium phosphate cement (MPC) are studied by measurements of setting time, flowability, compressive strength and by multiple technique analyses of pH values, calorimetry, XRD, TG, MIP and SEM taking calcium lactate (CL) content as variables. Results show that CL can significantly prolong the setting time and promote the synergetic development of compressive strength of MPC, but the addition of CL leads to a decrease in flowability of MPC. Comprehensive consideration on these properties, the optimal dosage of CL is 5%. In this case, the setting time, flowability and 1 day & 28 days compressive strength of MPC are 84 minutes, 185 mm, 40.8 MPa & 54.2 MPa, respectively. Multiple technique analyses show that the addition of CL can decrease the liquid phase pH value and hydration rate of MPC, resulting in the extension of setting time. A low content of CL (3%) can improve the reaction degree and optimize the matrix pore structure of MPC, and thus promoting the strength development (50.90 MPa increased to 65.93 MPa). However, an excessive addition of CL (7%) will lead to the decrease in reaction products and the increase in matrix porosity of MPC, resulting in a decrease in compressive strength (43.30 MPa reduced to 37.36 MPa).

Solubility of di-(2-ethylhexyl)phosphoric acid (D2EHPA) in aqueous electrolyte solutions: Studies relevant to liquid-liquid extraction

Di-(2-ethylhexyl)phosphoric acid (D2EHPA) is an acidic extractant frequently used in solvent extraction for metal refining. Only limited information is available on the amount and type of impurities present in commercially available D2EHPA and their effect on liquid-liquid extraction. In this paper, these impurities were identified and the importance of pre-conditioning the extractant before carrying out extractions is demonstrated. Furthermore, the solubility of D2EHPA in aqueous solutions was investigated as a function of pH, concentration of extractant and anion present in the aqueous phase (chloride, bromide, iodide, sulfate, methanesulfonate, thiocyanate, and nitrate). The density of the organic phases and the sodium and water uptake in the organic phase were determined as a function of the different anions present in the aqueous phase. The type of anion was found not to have a large influence on the solubility of D2EHPA in the aqueous phases. Low concentrations of salt in the aqueous phase or high pH values resulted in significant losses of D2EHPA to the aqueous phase. A very sharp increase in water content in the organic phase was observed around pH 5 (pH 6 for the nitrate system), accompanied by a significant increase in extraction of sodium ions, which explains the observed increase in density of the organic phase, and the tendency to third-phase formation. The results from this fundamental study help to better understand the behavior of liquid-liquid extraction systems in which D2EHPA is used as extractant and can help to prevent third-phase formation and losses of extractant to the aqueous phase. Moreover, the impurities present in commercially available D2EHPA and their impact on liquid-liquid extraction processes are determined.

Comparative study of performances of UHPLC-MS/MS and HPLC/UV methods for analysis of ziprasidone and its main impurities

AbstractZiprasidone is the second generation antipsychotic drug with unique multipotent G-protein-coupled (GPCR) receptor binding profile. Since ziprasidone is a highly lipophilic and unstable compound, development of efficient method for a concurrent assay of ziprasidone and its main impurities was a very challenging task.The UHPLC-MS/MS method that we developed for simultaneous determination of ziprasidone and its main impurities (BITP, Chloroethyl-chloroindolinone, Zip-oxide, Zip-dimer, and Zip-BIT) was compared with some other related HPLC-UV methods of our own and other authorship. An increase of the mobile phase pH value from 2.5 to 4.7 units in the examined analytical methods influenced elution order of the investigated compounds. It was found out that the UHPLC-MS/MS method is more selective and sensitive than the earlier developed HPLC-UV method. Similar to our earlier HPLC-UV method, the UHPLC-MS/MS method is linear with a correlation coefficient (r) above 0.99 for all the analysed compounds, but with a negligibly lower precision and accuracy. Finally, with shorter analysis time, smaller column size and reduction of solvent consumption, UHPLC-MS/MS is assumed as a greener method than HPLC-UV for the ziprasidone purity assay.After transfer of the UHPLC-MS/MS method to the UHPLC-DAD system, suitability of the UHPLC-DAD method for routine control of ziprasidone and its main impurities is examined and confirmed based on the retained good selectivity, resolution and short analysis time.

Impact of mobile phase composition on reverse-phase separation of polar basic compounds

Method development for determination of polar basic compounds on ion-suppression reverse-phase liquid chromatography, requires appropriate selection of stationary phase and composition and pH value of the mobile phase. The addition of the organic solvent in aqueous buffers with defined pH value, results in shift of the pH value of the mobile phase, resulting in significant change in chromatographic retention and selectivity. The aim of this study was to evaluate the impact of the variation of pH value of the mobile phase and percentage of the organic solvent, on the chromatographic separation of basic compound (octenidine dihydrochloride). The design of experiment was used for the optimization of the chromatographic conditions and selection of the most suitable mobile phase composition. The optimal composition of the mobile phase, providing satisfactory chromatographic performance based on ion-suppression reverse-phase chromatography, included 0.1M citric acid/0.2M sodium dihydrogen phosphate, pH =2.5, combined with 70% v/v organic solvent-acetonitrile. The suitability of the method was confirmed by satisfactory results for the system suitability parameters, specificity, linearity and precision. Key Words: polar basic compounds, ion-suppression, pH value, composition of mobile phase

QSRR modeling of the chromatographic retention behavior of some quinolone and sulfonamide antibacterial agents using firefly algorithm coupled to support vector machine

Quinolone and sulfonamide are two classes of antibacterial agents with an opulent history of medicinal chemistry features that contribute to their bacterial spectrum, efficacy, pharmacokinetics, and adverse effect profiles. The urgent need for their use, combined with the escalating rate of their resistance, necessitates the development of suitable analytical methods that accelerate and facilitate their analysis. In this study, the advanced firefly algorithm (FFA) coupled with support vector regression (SVR) was used to select the most significant descriptors and to construct two quantitative structure-retention relationship (QSRR) models using a series of 11 selected quinolone and 13 sulfonamide drugs, respectively, to predict their retention behavior in HPLC. Precisely, the effect of the pH value and acetonitrile composition in the mobile phase on the retention behavior of quinolones and sulfonamides, respectively, were studied. The obtained QSRR models performed well in both internal and external validations, demonstrating their robustness and predictive ability. Y-randomization validation demonstrated that the obtained models did not result by statistical chance. Moreover, the obtained results shed the light on the molecular features that influence the retention behavior of these two classes under the current chromatographic conditions.

A novel Fe/HNT visible light-driven heterogeneous photocatalyst: Development as a semiconductor and photocatalytic application

Fe/HNT (Iron/Halloysite-nanotube) heterogeneous semiconductor catalysts operating effectively under visible light were developed by using FeCl3, FeSO4 and Fe(OH)3 sludge precipitated after electro-Fenton process and named as Fe/HNT-I, Fe/HNT-II and Fe/HNT-III, respectively. Chemical configuration and particle morphology of the catalysts were characterized with XRD, SEM-EDS and UV–vis DRS. Effect of the developed Fe/HNT photocatalysts was investigated for the degradation of Reactive Orange 16 (RO16) textile dye under visible light. The photocatalytic decolorization of RO16 was 95.6%, 99.3% and 96.6%, respectively. It was found that the photocatalytic performance of Fe/HNT-III catalyst under visible light was effective compared to Fe/HNT-I and Fe/HNT-II. The iron ratio in the catalyst's structure (Fe:HNT ratio 0.25, 0.5 and 0.75 (w/w)) and pH value (4, 7 and 9) in production phase were also changed to investigate the photocatalytic effect of Fe/HNT-III. An Fe:HNT ratio of 0.25 and a pH of 4 were determined as the optimum conditions for catalyst production. Optimum H2O2 dosage value was also investigated for photocatalytic oxidation process and determined to be 10 ​mM. Finally, the optimum conditions were further used for the degradation of Terbinafine hydrochloride (TerHCl) active drug and the treatment of wastewater from the textile and pharmaceutical industries.

Цементные материалы на основе фосфатов магния и кальция с гиалуронатом натрия

In the recent years, a magnesium-calcium phosphate materials are considered as an alternative to materials based on the calcium phosphates in the reconstructive surgery. The injectable bone cements have been particular interest for the minimally invasive surgical approaches. The aim of this work is considered to the creating and studying of the structural-phase state of cement materials based on the Newberite phase (MgHPO4·3H2O). The addition of a polymer - sodium hyaluronate in the cement fluid, based on a sodium phosphate solution, leeds to the increasing of the viscosity of the system, thereby increasing the cohesion of cement materials. The effect of addition sodium hyaluronate in the various concentrations on the phase composition, setting time, pH value, microstructure, injectability and strength properties of cement materials has been studied.

Ion Flotation of Ytterbium Water-Salt Systems—An Innovative Aspect of the Modern Industry

Considering the ever-increasing role of rare-earth elements (REE) in the modern hi-tech field, their effective use has tremendous significance, although the production process is inevitably linked to the large volumes of industrial ammonia effluents and heavy metal wastes. In the process of metallurgical separation of metals, the emission of large volumes of noxious gases and radioactive substances is inevitable. Lean technogenic raw material processing is sensible under the condition of the development of non-waste technology. The lack of competent regulations governing the disposal of waste containing REE has an impact on adjacent territories, accumulating in water bodies and, as a result, in the human body. Such an impact cannot pass without a trace, however, the ambiguity of opinions in the scientific community regarding the toxic effects of REE on living organisms determines the relevance of a more detailed study of this issue. The study of ytterbium ions removal from aqueous standard test solutions by the adsorptive bubble method—ion flotation—was conducted. The experiments showed that by using the ion flotation method, the maximum removal of ytterbium (III) was achieved at pH = 8.30. It was shown that ytterbium (+3) distribution coefficients as a function of aqueous phase pH value in the process of ion flotation with sodium dodecyl sulphate were derived. The comparison of values of removal pH with those of hydrate formation pH allowed to conclude that ytterbium floate as basic dihydroxoytterbium dodecyl sulphate Yb(OH)2(C12H25OSO3).

PH-Responsive Pickering high internal phase emulsions stabilized by Waterborne polyurethane

HypothesisWaterborne polyurethane (WPU) is a common colloidal dispersion that can aggregate in the aqueous phase to form nanoparticles with hydrophobic polyurethane chains as the core and hydrophilic ionic groups as the shell. Considering their structure and pH-responsive functional groups, WPU nanoparticles could be ideal particulate emulsifiers for preparing pH-responsive Pickering high internal phase emulsions (HIPEs). ExperimentsA series of anionic WPU with different content of 2,2-bis(hydroxymethyl)propionic acid (DMPA) side chains were synthesized via a polyaddition reaction. The DMPA content, size, ζ-potential, and interfacial behaviors of WPU were then investigated. Furthermore, the effects of particle concentration, internal phase fraction (ϕ), oil type, and pH values on the Pickering HIPEs’ morphology, stability, and rheological behaviors were systematically studied. Finally, we demonstrated the emulsification–demulsification process of WPU-stabilized Pickering HIPEs and discussed its mechanism. FindingsOil-in-water (O/W) Pickering HIPEs with tailored morphology and excellent pH-responsiveness were prepared from anionic WPU nanoparticles. The WPU concentration, ϕ, and oil type had a large impact on the formation and mean droplet size of the WPU-stabilized emulsions. Rheology analysis demonstrated that the strictly limited movement of droplets endowed the WPU-stabilized HIPEs with high stability, shear sensitivity, and excellent thixotropic recovery. By simply changing the aqueous-phase pH value, the WPU-stabilized HIPEs could undergo more than ten emulsification-demulsification cycles, as the physical and interfacial properties of WPU nanoparticles were pH-dependent. The excellent performance of the WPU-stabilized pH-responsive Pickering HIPEs exhibited their potential practical applications, such as for oil transportation and recovery, emulsion polymerization, and heterogeneous catalysis.

The electrosorptive response of a carbon nanotube flow-through electrode in aqueous systems

The capture and recovery of valuable products from wastewater and/or bio-broths is one of today’s industrial challenges. Potential-controlled chromatography is a versatile solution to separate charged or polarized target species from aqueous systems. This capacitive flow-through technique combines the advantages of capacitive desalination and ion-exchange chromatography. The separation principle is controlled by system-dependent solid–liquid interaction mechanisms at the potential-controlled interface and characterized by the electrochemical double layer (EDL) formation. We conducted new experiments on the process- and environment-dependent surface effects in aqueous systems to better understand electrically driven processes inside a macroporous multi-walled carbon nanotube electrode. Here, the column and current response are investigated as a function of flow rate, as well as mobile phase pH-value, composition and concentration. Due to the strong water affinity of the material, water ions significantly co-define the EDL. The current response depends particularly on the ion properties and concentration. The use of electrolytes promotes capacitive and faradaic current and diminishes pH-deviation occurring at a negative potential. The effective range of the EDL decreases with increasing shear forces. Finally, a better performance for electrosorbing maleic acid is guaranteed at higher electrolyte concentration and low flow rate. This paper successfully addresses research gaps in potential-dependent effects that occur in multi-walled carbon nanotube electrodes.

Facile fabrication of silica@covalent organic polymers core-shell composites as the mixed-mode stationary phase for hydrophilic interaction/reversed-phase/ion-exchange chromatography

Covalent organic polymers (COPs) are a promising class of cross-linked polymeric networks that attracted extensive attention in separation and analysis fields. Exploring facile and convenient strategy to prepare COPs-based mixed-mode stationary phases for high performance liquid chromatography (HPLC) has seriously lagged and has never been reported. Herein, we describe a facile in-situ grow strategy for fabrication of silica@COPs core-shell composites (SiO2@TpBD-(OH)2) as a novel mixed-mode stationary phase for HPLC. Owing to the co-existing of abundant hydroxyl, carbonyl, imine, cyclohexyl groups, and benzene rings in the skeleton of COPs shell, the developed mixed-mode stationary phase exhibits hydrophilic interaction liquid chromatography (HILIC)/reversed-phase liquid chromatography (RPLC)/ion-exchange chromatography (IEX) retention mechanisms. The content of acetonitrile, pH value, and salt concentration in the mobile phase were investigated on SiO2@TpBD-(OH)2 packed column. In comparison to conventional single-mode columns, the SiO2@TpBD-(OH)2 column showed flexible selectivity, enhanced separation performance, and superior resolution for benzene homologues, polycyclic aromatic hydrocarbons, nucleosides and bases, and acidic organic compounds. The column efficiency of p-nitrobenzoic acid was up to 54440 plates per meter. The packed column also possessed outstanding chromatographic repeatability for six nucleosides and bases with the RSDs of 0.07–0.23%, 0.58–1.77%, and 0.31–1.23% for retention time, peak area, and peak height, respectively. Besides, the SiO2@TpBD-(OH)2 column offered baseline separation of multiple organic pollutants in lake water, which verified its great potential in real sample analysis. Overall, the silica@COPs core-shell composites not only provide a new candidate of mixed-mode stationary phases, but also extend the potential application of COPs in separation science.

Quantitative analysis of nine types of virus-like particles in human papilloma virus bulk by size-exclusion chromatography

据统计,5%以上的人类癌症由人乳头瘤病毒(HPV)导致。HPV疫苗的使用,尤其是多价HPV疫苗的使用,可有效预防HPV感染和肿瘤的发生。例如,9价HPV疫苗可有效预防90%以上HPV相关癌前病变。人乳头瘤病毒样颗粒(VLP)是HPV疫苗的唯一抗原。VLP由360份衣壳蛋白L1组成。VLP的含量测定对HPV原液和HPV疫苗的质量评价至关重要。该文发展了一种以体积排阻色谱(SEC)为基础的9种型别人乳头病毒样颗粒的定量方法。实验优化了包括色谱柱类型、色谱柱孔径、流动相离子强度和流动相pH值在内的色谱条件。经过考察,以SHIMSEN Ankylo SEC-300色谱柱(300 mm×7.8 mm, 3 μm)为固定相,以含有300 mmol/L NaCl和50 mmol/L磷酸盐(pH 7.0)的缓冲溶液为流动相时,VLP的色谱峰更窄,从而可获得更高的响应和更好的灵敏度,因此选择该色谱条件用于VLP与基质的分离。优化所得的方法具有较宽的线性范围,良好的重复性(峰面积的相对标准偏差不大于5.0%)和灵敏度(定量限为4.58~15.24 μg/mL)。将方法用于HPV原液中VLP的含量测定,监测VLP的稳定性。结果显示,HPV原液中VLP颗粒不稳定,于4 ℃放置一周后,VLP含量与生产后立即测得的含量相比存在一定程度的降解。此外,方法还可用于疫苗上清液中游离蛋白质的分析,监测铝佐剂对VLP的吸附情况。被测厂家的铝佐剂可较好的吸附VLP,无明显残余蛋白质检出。与传统的蛋白质定量方法相比,如Folin-酚法(Lowry法),该法具有操作简单、自动化程度高、分析通量高等优点,可实现VLP含量的批量化分析。

Characterization of a highly stable mixed-mode reversed-phase/weak anion-exchange stationary phase based on hybrid organic/inorganic particles.

We have characterized Atlantis ethylene‐bridged hybrid C18 anion‐exchange, a mixed‐mode reversed‐phase/weak anion‐exchange stationary phase designed to give greater retention for anions (e.g., ionized acids) compared to conventional reversed‐phase materials. The retention and selectivity of this stationary phase were compared to that of three benchmark materials, using a mixture of six polar compounds that includes an acid, two bases, and three neutrals. The compatibility of the ethylene‐bridged hybrid C18 anion‐exchange material with 100% aqueous mobile phases was also evaluated. We investigated the batch‐to‐batch reproducibility of the ethylene‐bridged hybrid C18 anion‐exchange stationary phase for 27 batches across three different particle sizes (1.7, 2.5, and 5 μm) and found it to be comparable to that of one of the most reproducible C18 stationary phases. We also characterized the acid and base stability of the ethylene‐bridged hybrid C18 anion‐exchange stationary phase and the results show it to be usable over a wide pH range, from 2 to 10. The extended upper pH limit relative to silica‐based reversed‐phase/weak anion‐exchange materials is enabled by the use of ethylene‐bridged hybrid organic/inorganic particles. The improved base stability allows Atlantis ethylene‐bridged hybrid C18 anion‐exchange to be used with a wider range of mobile phase pH values, opening up a greater range of selectivity options.

Ionic liquid functionalized β-cyclodextrin and C18 mixed-mode stationary phase with achiral and chiral separation functions

A novel reversed-phase/hydrophilic interaction/ion-exchange (RPLC/HILIC/IEC) and chiral recognition mixed-mode stationary phase material was synthesized using 3-n-octadecyl-1-vinylimidazolium bromide and 6-(1-allylimidazolium)-cyclodextrin tosylate as functional monomers. After identifications of intermediates and stationary phase materials using nuclear magnetic resonance analysis, Fourier transform infrared spectrometer, element analysis and thermogravimetric analysis, the synthesized Sil-VMBD material was packed into an empty column under high pressure. The mixed-mode retention performance was researched by hydrophobic, hydrophilic and ionic compounds. And the retention mechanism of the multi-mode stationary phase was studied via changing the mobile phase composition and pH value. Moreover, the enantiomers of 1-phenyl-1-propanol, warfarin and styrene oxide were separated rapidly under reverse-phase mode. Fast enantioseparation of ibuprofen and ketoprofen were obtained within 4 min under polar organic mode. The experimental results show that the as-prepared mixed-mode column possesses reversed-phase, hydrophilic and ion-exchange interactions with various analytes, and these interactions also enable the stationary phase with multi-mode and chiral separation abilities.

Preparation and application performance of lignin-polyurea composite microcapsule with controlled release of avermectin

Pickering emulsion stabilized by lignin/sodium dodecyl sulfate composite nanoparticles (LSNP) was used as template to prepare the avermectin @ lignin/polyurea composite microcapsules (AVM@LPMC) through ion cross-linking and interfacial polymerization. The inner wall of the microcapsules is a firm and compact polyurea layer, and the outer wall is a loose lignin layer. The effects of stirring speed, dosage of sodium dodecyl sulfate (SDS), and pH value in aqueous phase on the formation of microcapsules were systematically studied. The results showed that the optimal stirring speed was 200 rpm, and the optimal dosage ratio in water phase was HCl (mmol):SDS (mmol):lignin AL (g) = 0.375:1.25:1 in fixed oil-water ratio (1:9) and oil phase composition. In this way, the encapsulation efficiency of microcapsules could reach up to 85.4%, while it would slightly decrease with the increase of lignin content in the wall materials. The polyurea layer played a key role in supporting the spherical structure of the capsule wall and delaying the release of avermectin, while the loose lignin layer contributed less to the slow release performance of microcapsule. By changing the amount of lignin, the polyurea-layer thickness could be regulated to adjust the release rate of microcapsule. Remarkably, a small amount of lignin introduced in the wall material could significantly improve the anti-photolysis performance of avermectin in microcapsules.

Rapid Separation and Screening of Mycophenolate Mofetil and Mycophenolic Acid with a Novel (Vinyl Ester) Resin Molecular Imprinted Monolithic Column

We introduced a new molecular imprinted polymers (MIPs) monolithic column of Mycophenolate mofetil (MMF) for HPLC. The monolithic column was prepared using MMF as the template molecule, methcrylic acid (MAA) as the functional monomer, vinyl ester resin as the crosslinking agent and AIBN as the initiator. HPLC was used to study the binding and separation performance of MIPs for template MMF and its cleavage product Mycophenolic acid (MPA). For chromatographic analysis the effects on the separation, mobile phase composition, flowrate and pH value were discussed respectively. Under the selected chromatographic conditions, MMF and MPA could achieve base line separation within 4 min with a separation degree of 2.68. Moreover, the linearity of the calibration plot was evaluated of seven spiked samples (2.0–100.0 µg·mL−1) in plasma, and the limit of detection (LOD) for MMF in plasma and the stability of the monolithic column were also studied. Twelve-hour pharmacokinetic profile of both MMF and MPA for a renal transplant recipient receiving oral dosing of 1000 mg MMF was investigated. Results indicated that this method could be applied for separation and screening of MMF and MPA, It provided a simple and fast method for assaying this drug in plasma sample.

Preparation of a stilbene diamido-bridged bis(β-cyclodextrin)-bonded chiral stationary phase for enantioseparations of drugs and pesticides by high performance liquid chromatography

A stilbene diamido-bridged bis(β-cyclodextrin) was synthesized via the reaction between 4,4′-stilbene dicarboxylic acid and 6-deoxy-6-amino-β-cyclodextrin. Then it was bonded onto the surface of an ordered mesoporous SBA-15 to obtain a novel bridged bis(β-cyclodextrin)-bonded chiral stationary phase (SBCDP). The structures of the bridged bis(β-cyclodextrin) and SBCDP were characterized by the mass spectrometry, nuclear magnetic resonance, infrared spectroscopy, elemental analysis and thermogravimetric analysis. The chromatographic performance of SBCDP was systematically evaluated by separating 23 racemic drugs and pesticides, including trimeprazine, praziquantel, flavanones, β-blockers and triazole pesticides in the reversed-phase chromatography or the polar organic mode. The chromatographic conditions that affect the enantioselectivity or diasterioselectivity of SBCDP were investigated in detail, including the mobile phase composition, pH value and column temperature. As a result, all tested analytes were resolved on SBCDP with high resolutions (1.51∼5.15) within about 25 min, and the enantioseparation resolutions of flavanone and imazalil were up to 5.15 and 4.38, respectively. Compared with the native β-cyclodextrin stationary phase (CDCSP), the SBCDP had a better chromatographic performance in enantioselectivity and diasterioselectivity. For example, enantiomers of trimeprazine, praziquantel, flavanone and imazalil those could not be separated by CDCSP, were separated by SBCDP with high resolutions. Unlike the small cavity (0.65 nm) of native CD, the bridging linker of the bridged bis(β-CD) supplied a well-organized “pseudo-cavity”, and combined two native CDs as an organic whole, which could synergistically encapsulate and complex some bulky analytes, making the chiral discrimination of SBCDP more precise. Moreover, we also found that SBCDP possessed high enantioselectivity and diastereoselectivity over a wide range of temperature (30∼60 °C), which made the fast analysis possible. As a new chiral separation material, SBCDP may have wider applications in analysis of chiral compounds.