Crystallinity: A Complex Critical Quality Attribute of Amorphous Solid Dispersions.

Does the performance of an amorphous solid dispersion rely on having 100% amorphous content? What specifications are appropriate for crystalline content within an amorphous solid dispersion (ASD) drug product? In this Perspective, the origin and significance of crystallinity within amorphous solid dispersions will be considered. Crystallinity can be found within an ASD from one of two pathways: (1) incomplete amorphization, or (2) crystal creation (nucleation and crystal growth). While nucleation and crystal growth is the more commonly considered pathway, where crystals originate as a physical stability failure upon accelerated or prolonged storage, manufacturing-based origins of crystallinity are possible as well. Detecting trace levels of crystallinity is a significant analytical challenge, and orthogonal methods should be employed to develop a holistic assessment of sample properties. Probing the impact of crystallinity on release performance which may translate to meaningful clinical significance is inherently challenging, requiring optimization of dissolution test variables to address the complexity of ASD formulations, in terms of drug physicochemical properties (e.g., crystallization tendency), level of crystallinity, crystal reference material selection, and formulation characteristics. The complexity of risk presented by crystallinity to product performance will be illuminated through several case studies, highlighting that a one-size-fits-all approach cannot be used to set specification limits, as the risk of crystallinity can vary widely based on a multitude of factors. Risk assessment considerations surrounding drug physicochemical properties, formulation fundamentals, physical stability, dissolution, and crystal micromeritic properties will be discussed.

Extraction and Encapsulation of Phytocompounds of Poniol Fruit via Co-Crystallization: Physicochemical Properties and Characterization.

Poniol (Flacourtia jangomas) has beneficial health effects due to its high polyphenolic and good antioxidant activity content. This study aimed to encapsulate the Poniol fruit ethanolic extract to the sucrose matrix using the co-crystallization process and analyze the physicochemical properties of the co-crystalized product. The physicochemical property characterization of the sucrose co-crystallized with the Poniol extract (CC-PE) and the recrystallized sucrose (RC) samples was carried out through analyzing the total phenolic content (TPC), antioxidant activity, loading capacity, entrapment yield, bulk and traped densities, hygroscopicity, solubilization time, flowability, DSC, XRD, FTIR, and SEM. The result revealed that the CC-PE product had a good entrapment yield (76.38%) and could retain the TPC (29.25 mg GAE/100 g) and antioxidant properties (65.10%) even after the co-crystallization process. Compared to the RC sample, the results also showed that the CC-PE had relatively higher flowability and bulk density, lower hygroscopicity, and solubilization time, which are desirable properties for a powder product. The SEM analysis showed that the CC-PE sample has cavities or pores in the sucrose cubic crystals, which proposed that the entrapment was better. The XRD, DSC, and FTIR analyses also showed no changes in the sucrose crystal structure, thermal properties, and functional group bonding structure, respectively. From the results, we can conclude that co-crystallization increased sucrose's functional properties, and the co-crystallized product can be used as a carrier for phytochemical compounds. The CC-PE product with improved properties can also be utilized to develop nutraceuticals, functional foods, and pharmaceuticals.

Morphological crystal adsorbing tetracyclines and its interaction with magnesium ion in the process of struvite crystallization by using synthetic wastewater.

Struvite (MgNH4PO4·6H2O) crystallization is a promising method of phosphorus recovery from wastewater. As for digestive livestock wastewater, the extensive residues of antibiotics could induce struvite recovery to spread antibiotic resistance and thereafter pose ecological risks to the environment. In this study, struvite crystals with different morphologies were produced from synthetic swine wastewater, and tetracyclines (TCs) adsorbing capacities were investigated. The important factors, including the existence of Mg2+ ions and initial TCs concentration, were examined. The predominant adsorption between TCs and struvite crystals was electrostatic interaction, with the maximum capacity at doxycycline (DXC) 876.5 µg/Kg, oxytetracycline (OTC) 1946.7 µg/Kg and tetracycline (TC) 2376.2 µg/Kg, respectively. Well-faceted struvite crystallites possessed high adsorption capacities than those of dendritic crystallite, due to higher Mg intensities on the crystallite surface. The increment of phosphorus concentration could trigger the transformation of struvite morphology from needle to dendritic shapes with X-shape as an intermediate stage, which would reduce Mg density in specific crystallite facets and therefore limit TCs adsorption onto struvite crystals. The existence of Mg2+ ion would inhibit TCs deprotonation and thereafter improve TCs adsorption onto struvite crystals. Further investigation revealed that continuously elevating initial TCs concentration would promote the formation of 1:2 transferring to 1:1 TCs-Mg chelates, which would result in a fluctuation following a drastic augment of TCs adsorption capacity.

Recovery of phosphate as hydroxyapatite by fluidized bed homogeneous crystallization technique.

Phosphorous recovery from aqueous solutions gained substantial attention and this not only secure the food demand but also curtail the pollution of freshwater courses. In the current study, authors employed novel fluidized bed homogeneous crystallization (FBHC) technique to granulate the phosphorous as hydroxyapatite (HAP). FBHC technique nurtures the formation of high pure HAP crystals without seed addition and potential technique to recover phosphorous compared to other techniques. The key operational parameters influencing the HAP crystallization were analyzed prior to FBHC by batch analysis. From the batch study results, the range of pH and calcium to phosphorous molar ratio fixed for FBHC studies. Maximum phosphate removal and granulation efficiencies obtained were 91.25% and 82.55%, respectively, at 500 mg/L phosphate concentration, pH 12, and calcium to phosphorous molar ratio 1.65. Box-Behnken design of response surface methodology was employed for evaluating interaction impact of process parameters on granulation efficiency. Granulation efficiency of 79.74% was attained at pH 11.83, calcium to phosphorous molar ratio 1.637, and reaction time 70.73 h.

Enrichment of Palmitoleic Acid by a Combination of Two-step Solvent Crystallization and Molecular Distillation.

Palmitoleic acid shows a variety of beneficial properties to human health. In this study, enrichment of palmitoleic acid from sea buckthorn pulp oil by two-step solvent crystallization and molecular distillation was investigated. Sea buckthorn pulp oil was first converted to its corresponding mixed fatty acids (SPOMFs) containing 27.17% palmitoleic acid. Subsequently, the effects of various factors on crystallization (i.e., crystallization temperature, type of solvent, ratio of SPOMFs to solvent (w/v), crystallization time) and molecular distillation (distillation temperature) were assessed on a 5-g scale. It was found that optimal primary crystallization conditions were a 1:15 ratio of SPOMFs to methanol (w/v), -20°C and 12 h. Secondary crystallization conditions were set to a 1:4 ratio of methanol to palmitoleic acid product obtained from the first step crystallization to methanol (w/v), -40°C and 6 h. For further purification of palmitoleic acid by molecular distillation, the optimal distillation temperature was determined to be 100°C. After purification by crystallization and molecular distillation under the optimal conditions, the final product consisted of 54.18% palmitoleic acid with an overall yield of 56.31%. This method has great potential for adoption by the food and medical industries for the preparation of palmitoleic acid concentrate for nutritional studies.

Repurposing Melt Degradation for the Evaluation of Mixed Amorphous-Crystalline Blends.

Medicine regulators require the melting points for crystalline drugs, as they are a test for chemical and physical quality. Many drugs, especially salt-forms, suffer concomitant degradation during melting; thus, it would be useful to know if the endotherm associated with melt degradation may be used for characterising the crystallinity of a powder blend. Therefore, the aim of this study was to investigate whether melt-degradation transitions can detect amorphous content in a blend of crystalline and amorphous salbutamol sulphate. Salbutamol sulphate was rendered amorphous by freeze and spray-drying and blended with crystalline drug, forming standards with a range of amorphous content. Crystalline salbutamol sulphate was observed to have a melt-degradation onset of 198.2±0.2°C, while anhydrous amorphous salbutamol sulphate prepared by either method showed similar glass transition temperatures of 119.4±0.7°C combined. Without the energy barrier provided by the ordered crystal lattice, the degradation endotherm for amorphous salbutamol sulphate occurred 50°C below the melting point, with an onset of 143.6±0.2°C. The enthalpies for this degradation transition showed no significant difference between freeze- and spray-dried samples (p>0.05). Distinct from convention, partial integration of the crystalline melt-degradation endotherm was applied to the region 193-221°C which had no contribution from the degradation of amorphous salbutamol sulphate. The linear correlation of these partial areas with amorphous content, R2=0.994, yielded limits of detection and quantification of 0.13% and 0.44% respectively, independent of drying technique. Melt-degradation transitions may be re-purposed for the measurement of amorphous content in powder blends, and they have potential for evaluating disorder more generally.

The mechanism of binding with the α-glucosidase in vitro and the evaluation on hypoglycemic effect in vivo: Cocrystals involving synergism of gallic acid and conformer.

Cocrystallization of Active Pharmaceutical Ingredients (API) with formers can induce positive or negative synergistic effects on activity; however, the underlying mechanism is unclear. In this study, we screened two cocrystals of gallic acid (GA): GA-p-aminobenzoic acid (cocrystal A) and GA-amino acetic acid (cocrystal B). Solubility, dissolution rate, and oral bioavailability and hypoglycemic effect of the two cocrystals were evaluated. Additionally, we examined the effect induced by cocrystallization of GA with each former on inhibition activity on α-glucosidase, a protein target involved in hypoglycemic effects. Cocrystals A and B were constructed in a 1:1 API/former molar ratio by CO⋯HN and OH⋯OC hydrogen bonds, respectively. As predicted, cocrystallization improved oral bioavailability; AUC0-∞s of cocrystal A and B were 2.24-fold and 1.70-fold higher than that of GA. Interestingly, the α-glucosidase inhibition rate increased with cocrystal A (i.e., positive synergism) and decreased with cocrystal B (i.e., negative synergism) compared to GA alone. For each cocrystal system, an obvious difference in the α-glucosidase inhibition rate between cocrystal and its physical mixture (PM) of API and former was observed. The 1H NMR analysis of two cocrystals and their respective PM indicated that hydrogen bond interactions between API and former molecules were just present in the solutions of cocrystal; but not in that of PMs. Molecular docking indicated that the hydrogen bonds between GA and CCF achieved binding with α-glucosidase in the form of supramolecular. Due to improvements in both oral bioavailability and α-glucosidase inhibition rate, the maximum hypoglycemic rate in diabetic mice treated with cocrystal A was 3.4-fold higher than that of GA alone. Conversely, although cocrystal B displayed improved bioavailability compared with GA alone, the maximum hypoglycemic rate remained almost unchanged due to the negative synergism on α-glucosidase inhibition activity of GA and amino acetic acid. Cocrystallization with each former induced variation not only on physiochemical properties and bioavailability but also on biological profiles involving inhibition rate on target proteins, which likely contributed to the observed positive and negative synergistic effects on API activity.

An insight into crystallization test: A neoteric approach for screening premalignant and malignant lesions.

INTRODUCTION: Crystallization test is based on the principle that, when a salt crystallizes out of an aqueous solution, the crystal growth is influenced by the presence of other substances in the solution, such as blood or plant extracts. If a mixture of copper chloride solution with a small amount of whole blood is allowed to crystallize under controlled experimental conditions, an aggregate of crystals forms. Crystallization method can be used as a diagnostic aid to provide information about the systemic conditions and general health of the patient. AIM: This study aims to study the patterns of crystallization and to further determine the efficacy of crystallization test as a screening modality in premalignant lesions and oral squamous cell carcinoma (OSCC). MATERIALS AND METHODS: Fifty patients of OSCC, 50 patients of premalignant lesions, and 50 healthy individuals were selected. One drop of blood was collected from the study groups to perform crystallization using cupric chloride. STATISTICAL ANALYSIS USED: Statistical analysis was performed using Chi-square test, Student's t-test (two-tailed), and analysis of variance. RESULTS: The different patterns of crystals formed were studied and statistically analyzed. CONCLUSION: Based on the study, it was concluded that Crystallization test can be used as an effective screening modality for detection of premalignant lesions and OSCC.

The tangential flow absorption model (TFAM) - A novel dissolution method for evaluating the performance of amorphous solid dispersions of poorly water-soluble actives.

There is a substantial demand for absorptive dissolution tests, as single vessel dissolution experiments were originally not designed for testing supersaturating systems. Current approaches suffer from inadequate mass transfer of the dissolved active from the dissolution site, discrepancies in the fluid volume compared to in vivo intestinal fluid volumes or the dilution of functional excipients. In this work a novel dissolution apparatus was developed that enables adjustable mass transfer of the active through a membrane, while retaining the functional polymeric excipients at the dissolution site. Using this setup the dissolution behavior of various spray dried amorphous solid dispersions containing carbamazepine, hydrochlorothiazide and ketoconazole as model actives at intermediate and high supersaturation levels was evaluated. Compared to non-absorptive dissolution experiments, differences in the concentration-time profiles were noted. The experiments with a high supersaturation of ketoconazole revealed a concentration decrease over time under absorptive conditions. Additionally, it was observed that the difference between "spring" as well as "spring and parachute" formulations was less pronounced with increasing drug efflux. Further, the apparatus was also tested with Fasted State Simulated Intestinal Fluid as dissolution medium and results were compared to phosphate buffer pH6.8. As major benefits of the new TFAM apparatus the easy experimental procedure and sample preparation for drug concentration measurements using spectroscopy in the permeate, without the necessity for additional filtration and/or centrifugation to remove precipitated drug molecules, could be highlighted. This TFAM approach seems to be a promising tool for identifying formulations for amorphous solid dispersions with optimal in vitro performance.

Discovery of Orally Bioavailable Chromone Derivatives as Potent and Selective BRD4 Inhibitors: Scaffold Hopping, Optimization, and Pharmacological Evaluation.

Bromodomain-containing protein 4 (BRD4) represents a promising drug target for anti-inflammatory therapeutics. Herein, we report the design, synthesis, and pharmacological evaluation of novel chromone derivatives via scaffold hopping to discover a new class of orally bioavailable BRD4-selective inhibitors. Two potent BRD4 bromodomain 1 (BD1)-selective inhibitors 44 (ZL0513) and 45 (ZL0516) have been discovered with high binding affinity (IC50 values of 67-84 nM) and good selectivity over other BRD family proteins and distant BD-containing proteins. Both compounds significantly inhibited the expression of Toll-like receptor-induced inflammatory genes in vitro and airway inflammation in murine models. The cocrystal structure of 45 in complex with human BRD4 BD1 at a high resolution of 2.0 Å has been solved, offering a solid structural basis for its binding validation and further structure-based optimization. These BRD4 BD1 inhibitors demonstrated impressive in vivo efficacy and overall promising pharmacokinetic properties, indicating their therapeutic potential for the treatment of inflammatory diseases.

Organic Structure-directing Agent-free Synthesis for *BEA-type Zeolite Membrane.

Membrane separation has drawn attention as a novel-energy saving separation process. Zeolite membranes have great potential for hydrocarbon separation in petroleum and petrochemical fields because of their high thermal, chemical, and mechanical strength. A *BEA-type zeolite is an interesting membrane material because of its large pore size and wide Si/Al range. This manuscript presents a protocol for *BEA membrane preparation by a secondary growth method that does not use an organic structure-directing agent (OSDA). The preparation protocol consists of four steps: pretreatment of support, seed preparation, dip-coating, and membrane crystallization. First, the *BEA seed crystal is prepared by conventional hydrothermal synthesis using OSDA. The synthesized seed crystal is loaded on the outer surface of a 3 cm long tubular α-Al2O3 support by a dip-coating method. The loaded seed layer is prepared with the secondary growth method using a hydrothermal treatment at 393 K for 7 days without using OSDA. A *BEA membrane having very few defects is successfully obtained. The seed preparation and dip-coating steps strongly affect the membrane quality.

Cocrystals of diacerein: Towards the development of improved biopharmaceutical parameters.

The effectiveness of Diacerein as an anti-osteoarthritis drug is limited due to its acutely poor aqueous solubility and bioavailability. The present study demonstrates cocrystallization as a successful technique to improve the biopharmaceutical parameters of diacerein. Three cocrystals of diacerein were prepared by an eco-friendly technique with three suitable coformers namely isonicotinamide, nicotinamide, and theophylline. The formation of a new solid phase was inferred from the DSC thermograms and powder diffraction pattern and was supported by FTIR. The crystal structures of the cocrystals determined from the PXRD pattern using Material Studio software. Detailed analysis showed the formation of supramolecular hetero-synthons of complementary functional groups of the coformers with the carbonyl and carboxyl groups of diacerein. The structural conformation of the cocrystalline state was also provided by the shifts in the ssNMR pattern of the cocrystals. The three new cocrystals were found to have a relatively high solubility and intrinsic dissolution rate which showed remarkable improvement in anti-arthritic activity as compared to diacerein. Thus, proving cocrystallization to be a potential solution to the solubility limited bioavailability problems of diacerein.

Characterization of Pearl Millet (Pennisetum glaucum) waste.

Environmental considerations in recent times have led to increasing interest in naturally occurring lignocellulosic materials as they are abundant and biodegradable. Pearl Millet (PM) stalks are currently discarded in North India and add to agrowaste generation. In this study, raw stalk of PM was characterized for physicochemical properties such as composition, moisture content, water absorbency and thermal behaviour. Morphology and crystallinity were studied using scanning electron microscope and X-ray diffraction respectively. Pure cellulose, extracted from the stalk using an optimised process, was characterised similarly. XRD patterns indicate the presence of cellulose type I structure with crystallinity index of 32% for raw stalk and 55% for the purified material. Water absorbency was 10 g/g for raw and 13 g/g for extracted cellulose. Material was thermally stable up to 200 °C. These findings indicate that PM stalks may be used as an indigenous source of cellulose for the absorbent layer in hygiene products.

Application of In Situ Product Crystallization and Related Techniques in Biocatalytic Processes.

This Minireview highlights the application of crystallization as a very powerful in situ product removal (ISPR) technique in biocatalytic process design. Special emphasis is placed on its use for in situ product crystallization (ISPC) to overcome unfavorable thermodynamic reaction equilibria, inhibition, and undesired reactions. The combination of these unit operations requires an interdisciplinary perspective to find a holistic solution for the underlying bioprocess intensification approach. Representative examples of successful integrated process options are selected, presented, and assessed regarding their overall productivity and applicability. In addition, parallels to the use of adsorption as a very similar technique are drawn and similarities discussed.

Selection of cost-effective magnesium sources for fluidized struvite crystallization.

Struvite crystallization has been considered a promising approach to recover phosphorus from wastewater. However, its practical application is limited, probably because of the high cost of magnesium (Mg). In this study, a comprehensive economic analysis was conducted using five Mg sources (MgCl2, MgSO4, MgO, Mg(OH)2, and bittern) during the operation of a pilot-scale fluidized bed reactor (FBR), using swine wastewater as the case matrix. First, the economic operating conditions were investigated, and subsequently, the performance and the costs of the five Mg sources were compared. The results indicated that the FBR could be operated most economically at pH of 8.5 and Mg to phosphorus (Mg/P) molar ratio of 1.5. Under these conditions, no significant differences in phosphorus removal and product quality could be found between the five Mg sources. Selecting the most economical Mg source was thus highly dependent on the prices of the reagents and Mg sources. Low-solubility Mg sources were preferable when NaOH was priced higher, while high-solubility Mg sources proved more economical when HNO3 was expensive. The bittern was the most economical choice only when the distances for total inorganic orthophosphate removal and struvite recovery were shorter than 40 and 270km, respectively. The current study provides an overview of the economic selection of an Mg source, which can help reduce the cost of struvite crystallization.

Application of Struvite-MAP Crystallization Reactor for Treating Cattle Manure Anaerobic Digested Slurry: Nitrogen and Phosphorus Recovery and Crystal Fertilizer Efficiency in Plant Trials.

Recycling and reusing the nutrient resources from anaerobic digested slurry is very promising for environmental pollution control and agriculture sustainable development. We focus here on nitrogen and phosphorus recycling in treating cattle manure anaerobic digested slurry by a magnesium ammonium phosphate (struvite-MAP) crystallization process and examine the impact of MAP precipitation on plant growth. The MAP crystallization process was studied by a combination of Design-Expert 8.0.6 software, mathematical modeling, and experiments. The influence of Mg/P, N/P and pH on nitrogen (N) and phosphorus (P) recovery was investigated. Then, the fertilizing efficiency of the MAP precipitate on the growth of three vegetables (water spinach (Swamp cabbage), amaranth and Brassica parachinensis) was also evaluated. The results showed that more than 89% of N and 99% of P could be recovered at pH = 10 with molar ratios of Mg/P = 1.6 and N/P = 1.2. Compared with the control pots and potassium chloridepots, the fresh weight, dry weight and average height of swamp cabbage in the MAP pots were obviously enhanced without burning effects. The results showed that MAP precipitation can promote the development of plants, which is promising for its use as a slow-release fertilizer for agricultural production.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses.

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely Mössbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. Mössbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

PicW2 from Picea wilsonii: preparation, purification, crystallization and X-ray diffraction analysis.

Low temperature is a major limiting factor for plant growth and development. Dehydrin proteins are generally induced in response to low-temperature stress. In previous research, a full-length dehydrin gene, PicW2, was isolated from Picea wilsonii and its expression was associated with hardiness to cold. In order to gain insight into the mechanism of low-temperature tolerance by studying its three-dimensional crystal structure, prokaryotically expressed PicW2 dehydrin protein was purified using chitosan-affinity chromatography and gel filtration, and crystallized using the vapour-diffusion method. The crystal grew in a condition consisting of 0.1 M HEPES pH 8.0, 25%(w/v) PEG 3350 using 4 mg ml-1 protein solution at 289 K. X-ray diffraction data were collected from a crystal at 100 K to 2.82 Šresolution. The crystal belonged to space group C121, with unit-cell parameters a = 121.55, b = 33.26, c = 73.39 Å, α = γ = 90.00, ß = 109.01°. The asymmetric unit contained one molecule of the protein, with a corresponding Matthews coefficient of 2.87 Å3 Da-1 and a solvent content of 57.20%. Owing to a lack of structures of homologous dehydrin proteins, molecular-replacement trials failed. Data collection for selenium derivatization of PicW2 and crystal structure determination is currently in progress.

Extraction Optimization and Structural and Thermal Characterization of the Antimicrobial Abietane 7α-Acetoxy-6ß-hydroxyroyleanone.

The abietane 7α-acetoxy-6ß-hydroxyroyleanone (AHR), obtained from plant extracts, is an attractive lead for drug development, given its known antimicrobial properties. Two basic requirements to establish any compound as a new drug are the development of a convenient extraction process and the characterization of its structural and thermal properties. In this work seven different methods were tested to optimize the extraction of AHR from Plectranthus grandidentatus. Supercritical fluid extraction (SFE) proved to be the method of choice, delivering an amount of AHR (57.351 µg·mg-1) approximately six times higher than the second best method (maceration in acetone; 9.77 µg·mg-1). Single crystal X-ray diffraction analysis of the ARH molecular and crystal structure carried out at 167 ± 2 K and 296 ± 2 K showed only a single phase, here dubbed form III (orthorhombic space group P21212), at those temperatures. The presence of two other polymorphs above room temperature was, however, evidenced by differential scanning calorimetry (DSC). The three forms are enantiotropically related, with the form III → form II and form II → form I transitions occurring at 333.5 ± 1.6 K and 352.0 ± 1.6 K, respectively. The fact that the transitions are reversible suggests that polymorphism is not likely to be an issue in the development pharmaceutical formulations based on ARH. DSC experiments also showed that the compound decomposes on melting at 500.8 ± 0.8 K. Melting should therefore be avoided if, for example, strategies to improve solubility based on the production of glassy materials or solid dispersions are considered.

Chiral Metal-Oxide Nanofilms by Cellulose Template Using Atomic Layer Deposition Process.

In this article, we describe an advance approach for the fabrication of chiral metal-oxide nanofilms. Our approach is based on the atomic layer deposition of titania and alumina nanofilms onto cellulose microfibers, used as chiral templates, leading to the formation of chiral nanofilms with a spatial fibrous structure. The chiral nanofilms were extensively characterized by X-ray photoelectron spectroscopy and high-resolution electron microscopy. The chiral property of the produced titania nanofilms was studied by enantioselective adsorption experiments using circular-dichroism spectroscopy and chiral high-performance liquid chromatography. We demonstrate the application of the titania chiral nanofilms for enantioselective crystallization. Overall, the basic principle for the preparation of chiral nanofilms by atomic layer deposition is demonstrated, as well as their uses for several enantioselective applications.