Influence Of Drug Loading, Efficiency And Dissolution
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INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION Name of the Student Name of the University Author Note
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INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION Executive Summary Mesopore nano molecules are increasingly used in the field of drug production because of its high bioavailability, biocompatibility and biodegradability. The drug loading efficiency also needs a revise because of the higher dosage of drug can harm the body. So, newer innovative techniques are being developed to improve the stability, dissociation rate of the drug so that little amount of drug can do the needful without causing any harm to the body. There are also a few characterizing techniques that confirm the efficacy of these particles and it’s stability.
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION Table of Contents INTRODUCTION......................................................................................................................4 AIM AND OBJECTIVES..........................................................................................................6 RESEARCH QUESTIONS........................................................................................................6 LITERATURE REVIEW...........................................................................................................6 CONCLUSION........................................................................................................................13 REFERENCES.........................................................................................................................15
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION INTRODUCTION Mesoporous particles can be used as a successful drug delivery system. As the solubility of drugs remains to be very low, patients need to take medication of higher doses to meet the therapeutic benefits of a drug. A study was conducted to ensure the extent of the capabilityofmesoporoussilicananoparticles(MSNPs)asadrugdeliverysystem. Mesoporous silica nanoparticles are preferred because of their desirable chemical properties and thermal stability along with their compatibility with biological tissue. The distinctive structure of the MSNP allows it to deliver drugs effectively by controlling its slow release into the body’s target site. The physical and chemical properties of the mesoporous silica such as the pore size, drug loading capacity and porous nature along with surface properties can be changed by using additives during the development of MSNP. The altered properties of the surface of MSNP can make it adhesive to the drugs. The application of MSNP includes diagnosis, drug delivery into the specific target, uptaking cellular substances and monitoring body fluids (Bhartiet al.2015). Drugs that are administered orally should have the property to solubilise and be absorbed by the intestine to show its therapeutic action but about 40% of drugs that are sold into the market have low solubility and 70-80% of the newly developed drugs are not sold into the market because they suffer from low solubility (Leet al.2019). Solid dispersion systems can address the solubilization of mesoporous material such as silica which performs effectively in achieving the delivery of drug molecules within their nanopore structure. There are various techniques to load the drug into the mesoporous silica including solevent-free and solvent-dependent techniques. Solvent-based methods are easy to use for amorphisation of the drug into the mesoporous silica where the drug is dissolved in either ethanol or impregnated with mesoporous silica followed by removal of the solvent by drying. Spray
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INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION drying,asolvent-basedtechniqueprovidesgreaterefficiencyindrugloadinginto mesoporous silica compared to solvent-free methods (Choudhariet al.2014). MSNP confer low toxicity inside various cell lines and to evaluate its safety two parameters are considered which include surface chemistry and particle size. These two parameters influence the factors associated with cytotoxicity and biological behaviour that include particle agglutination, adsorption of protein onto the particle, cellular toxicityparticle trafficking and nano-bio interface interactions. The MSNP toxicity depends on the size of the particle and research reveals that native MSNPs possesses more cytotoxicity than the functional MSNPs. It was reviewed that PEGylation of MSNP decreased its attachment to serum proteins thereby reducing hemolysis of human blood cells and enhancing blood compatibility when drugs are injected intravenously (Jafariet al.2015). To visualise the physical properties after drug loading through mesoporous silica, the following techniques can be used which include differential scanning calorimetry (DSC) for thermal analysis of drug encapsulation into the silica matrix, scanning electron microscope (SEM) to visualise the size of particles and morphology of the surface of mesoporous silica and perform dissolution of drug with aqueous solution the drug to check the aqueous equilibrium solubility of the drug. The drug dissolution will compare the highest saturation degree and time of drug-loaded silica carriers (Kiwilszaet al.2015). Confocal microscopy demonstrated the distribution and location of the nanoparticle containing drug inside the cells (Costanzoet al.2016). In this paper, various studies that have already been conducted on this topic will be discussed elaborately.
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION AIM AND OBJECTIVES The aim of this study is to derive the main differences between the different drug loading methods, impact of drug loading methods on the loading efficiency and dissolution performance of mesoporous polymeric carriers. Objectives: To deduce the differences between different drug loading methods. To find out the loading efficiency of various drug loading methods. To find out the dissolution performance of mesoporous polymeric carriers. RESEARCH QUESTIONS Q1. What are the differences between the drug loading methods available? Q2. State the loading efficiency of the available drug loading method into mesoporous polymeric carriers. Q3. State the drug solid-state stability and dissolution performance of mesoporous polymeric carriers. LITERATURE REVIEW Since the last decade, there has been extensive research conducted on mesoporous polymeric carriers or mesoporous silica nanoparticles (MSN) as it can be used as an alternative in a drug delivery system. A conducted review sheds light on the advancements that have been done regarding these particles. The first advancement of MSN is its immediate and sustained drug delivery system where the drug reaction timing can be set from before, which might be immediate or sustained. The other advancement of MSN is its controlled and targeted drug delivery system where the drug reaction can be set to act on a particular target
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION or act in a controlled manner. The researchers also discussed its biotherapeutic agent delivery efficiency, its bioimaging applications and its capability of tissue regeneration as bioactive substance. All the results showed the high ability of mesoporous particles (Wanget al.2015). A study was conducted to observe if any increase in drug loading and decrease in drug delivery is possible by changing the surface of mesoporous particle SBA-15. AT first, thestructureofSBA-15nanoparticleswasalteredbytheadditionof3-aminopropyl triethoxysilane. Then it was used as a transporter of an anti-inflammatory and non-steroidal drug after the loading was optimised. The modified version of SBA-15 was characterised by SEM, XRD and Thermal Analysis. Then by changing the drug loading factors which include time, stirring rate and temperature loading optimisation was done. It resulted in a significant increase in drug loading and decrease in the rate of drug delivery (Ahmadiet al.2014). MagneticResonanceImaging(MRI) isone ofthemostwidelyused imaging procedure (Morris and Slesnick 2018). To get enlarged and clear images of the organs in MRI, contrast agents are used. Gadolinium is used as the contrast agent, but it has a high risk of nephrogenic systemic fibrosis. To avoid the usage of this element, researchers conducted an experiment on mesoporous manganese silicate-coated silica nanoparticle as the contrast agent in MRI. The results showed it can be used as the contrast agent. However, more research is required to use as a permanent alternative of gadolinium because the researchers are sceptical of its efficacy (Liet al.2016). Anti-cancer drugs are often not properly delivered at the tumour site and it has quite a lot of toxic side-effects. To avoid this, researchers conducted an experiment to produce a non- toxic and target-specific drug delivery system. They took a polyethylene glycol (PEG) shieldingandatumourmicroenvironmentactivatingcascadepH-responsivehollow mesoporous silica nanoparticles (HMSN) drug delivery system and the surface was modified
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INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION by the addition of 3-(3, 4-dihydroxyphenyl) propionic acid (DHPA) with the help of boronic acid catechol ester bonds. Different characterising techniques proved the fact of the proper attachment of DHPA on the surface of HMSN. It was then tested on both in vitro and in vivo conditions. In vitro test showed that as the compound enters the tumour with increased permeability and retention effect, PEG was cleaved from Ada in the slightly acidic state of the tumour microenvironment. On the other hand, the PEG facilitates cellular uptake of HMSN molecules and leads to apoptosis of tumour cells. The in vivo test showed that the drug loaded HMSN molecules inhibited the growth of the tumour cells, and it did not even have any toxic effect (Liuet al.2016). Nano-Engineering techniques can make the use of MSNPs in many ways. In this study, the researchers proved this again by synthesising three MSNP molecules of different sizes: 48nm, 72nm and 100nm with PEG incorporated in its surface. Then by the help of cleavable disulphide bonds, amino-β-cyclodextrin was added to block the rugs inside the mesopore. Then active folate ligand was incorporated into the MSNPs, creating PEG- MSNPs48-CD-PEG-FA leading to improvement and selective uptake of these nanoparticles inside the tumour. It was seen that these MSNP nanoparticles were able to inhibit the growth of breast cancer tumours in mice much more effectively(Zhanget al.2014). MSNPs hve the ability to change their physical forms. To explore this ability, scientistsconductedanexperimentinwhichtheyheavilydopedMSNPswith photosensitising chlorin e6. Heavy doping led to the change of shape in these nanoparticles from spherical to rod-shaped. It was then seen that these rod-shaped nanoparticles have the ability to emit singlet oxygen molecules that are used in photodynamic therapy and these molecules also have high drug loading capability. Owing to it’s larger aspect ratio than the spherical molecules, it can uptake the cancer cells much faster. This was further tested with
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION doxorubicin a chemotherapy drug, and it resulted in dual action including chemotherapy as well as photodynamic therapy. Thus, it resulted in having much better efficiency of inhibiting cancer cells in both in vitro and in vivo conditions (Yanget al.2015). Saint-Cricqet al.(2015) researched and prepared a thermally disintegrable drug delivery nanoparticle that set to work when required on exposing it to a magnetic field. The mesopores of the nanoparticles are blocked at first at body temperature by applying an azo functionalized PEG so that the drug inside can not leak out. Azo-PEG allows the drug to escape from the pores when exposed to a narrow range of temperature by breaking the covalent bonds present. Then it was subjected to heat by a magnetic field in nanoscopic level so that the surrounding tissues are not destroyed. The result showed that it did not cause any cytotoxicityonfibroblastsandthuscanbeusedtodeliverdrugsandvariousother therapeutics, making it a safer choice for drug delivery system in different treatment procedures. A study was conducted to investigate the synergistic effects of using mesoporous molecules. The synergistic therapy included various ways of treatments including magnetic hyperthermia, photothermal therapy and controlled drug release. The system used magnetic mesoporous silica nanoparticles (MMSN) as magnetic thermoseeds and drug carriers and Graphene Quantum Dots (GQD) as caps along with photothermal generators. The experiment results showed that these nanoparticles could release drugs doxorubicin when present in low pH range. It also showed that MMSN/GQD nanoparticles could emit heat at an alternating magnetic field to the hypothermic temperature range. 4T1 cells of breast cancer were taken as a model system to study the effects in more details, and it showed that the combined impact ofchemo-magnetichyperthermiatherapyandchemo-photothermaltherapyalongwith
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION doxorubicin resulted in an increased number of cancer cell death than the therapies applied alone (Yaoet al.2017). Another technique was developed and studied to reduce the effect of doxorubicin by producingbiodegradableandenzymeresponsivemesoporoussilicananoparticleswith tumourspecificity.Forblockingthemesoporetopreventtheleakageofdrugs,the researchers used α-cyclodextrin and alkoxysilane tether. Further treatments and modifications were done with cathepsin B- responsive functions and GFLGR7RGDS with tumour target and membrane penetration so that the blocking material gets more potent and can prevent the exit of the drug doxorubicin from the mesopores. Then the normal and tumour cells were incubated with the prepared drug loaded MSNPs. This resulted in the action of surface RGDS along with the seven arginine molecules to target and penetrate the membrane and enter the tumour cells. It was also seen that cathespsin B gets poverexpressed in lysosomes and endosomes of tumour cells and thus can hydrolyse the GFLG part. It further led to observations that the doxorubicin loaded mesopores released about 80% drug within a day and resulted in an increase in apoptosis rate. It was also observed that the drug loaded MSNPs profoundly inhibited the growth of αvβ3-positive HeLa cells that causes cancer (Chenget al.2015). Another research was conducted to reduce the side effects or toxic effects of cancer drugs. In this research, the scientists produced a redox responsive nanoparticle for triplex therapy of tumour. The mesopores were sealed with cytochrome c on the MSNP molecules by disulphide bonds for intracellular drug delivery in a redox-sensitive way. To ease the process of drug targetting, AS1411aptamer was attached to the MSNPs. The structure was then confirmed and checked by TEM, fluorescence spectroscopy and BET/BJH analysis. This process led to the observation that the drug secretion from the nanoparticle could be done by
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INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION a redox reaction and thus can initiate in vitro apoptosis. On performing various tests like HE staining assays and TUNEL staining it showed that the nanoparticle exhibited high tumour targeting property and triplex therapy which inhibited the growth of tumours (Zhanget al. 2014). There quite a few processes by which drug loading can be done which include spray drying, rotary evaporation, solvent impregnation, and for testing the character or end product techniqueslikedifferentialscanningcalorimetry,scanningelectronmicroscopyand dissolution testing can be used (Sharma 2016). Spray drying can be defined as the technique used to prepare amorphous solid dispersion that can be used effectively to deliver the group of drugs that are not water-soluble (Singh and Van den Mooter 2016). An experiment was conducted using the spray drying technique to produce monodisperse mesoporous silica. The particles showed a hexagonal structure, and the size could be altered from 50 to 100μm by altering the content of initial solute and by bringing a change in the temperature of drying. It was observed that the amount of water and the ratio between surfactant and silica affected the ordering degree by self- assembly of the surfactant-silica micelles. The mesoporous molecules produced from spray drying were seen to have larger sizes and had a higher speed of synthesis than the conventional methods of production (Singh and Van den Mooter 2016). An attempt was taken to increase the dissolution and solubility of a drug named lapatinib ditosylate using hot melt extrusion and solvent rotary evaporation. A broad study was done based on the solid liquid equilibrium to find the interaction between drug and polymer. Thus, nine formulas of the drug were derived and were characterised by powder X- Ray diffraction, SEM, differential scanning calorimetry, dissolution and solubility. This study resulted in finding out that process parameter that included extrusion temperature and
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION physical attributes that included solid state and drug loading made effects on the dissolution and solubility of the drug. One of the formulas was identified as the best one. Thus, formula prepared by solvent rotary evaporation can help to determine the amorphicity, and therefore the dissolution and solubility can be found out from that (Hu, Lou and Hageman 2018). There is an increased demand for optimised and effective drug loading and delivery system for improved biocompatibily and bioavailability, and thus, various microdevices are being prepared for storage of ingredients that are insoluble in water. These microdevices are synthesised in such a way that it can prevent deactivation of the drug inside it and allow the drug to release whenever the necessity arises. This is when the solvent impregnation technique came into the play. Here, the insoluble or poorly soluble drug is put into the micro containers by dual application of supercritical fluid impregnation and inkjet printing. The scientists took polyvinyl pyrolidine solutions and inserted it in the micro containers by inkjet printing technique. This process is followed by impregnation of ketoprofen by supercritical carbon dioxide as the loading medium. This technique proved to be much beneficial as these micro containers exhibited a faster rate of drug dissolution and loading, and tbhus the release of drug can be regulated. This technique thus allows much higher fabrication of the microdevices delivery of oral drugs safely (Marizaet al.2014). Marin, Mallepally and McHugh (2014) conducted an experiment by using silk fibroin derived fromBombyx morias a medium for drug loading because of its bioavailability and biodegradability. Silk fibroin aerogels were loaded with Ibuprofen, an anti-inflammatory drug by superficial carbon dioxide impregnation technique. Then it was characterised under Differential Scanning Calorimetry and the result indicated of it being amorphous. Scanning Electron Microscopy was also used for the identification of textural and morphological properties. When this is analysed in vitro, it was found that ibuprofen got released from the
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION aerosol at the temperature of 37°C and pH of 7.4 and took about 6 hours time to release completely and the dissolution took about 15 minutes proving it to be a worthy procedure to follow. The increase in concern for the non-solubility of active pharmaceutical drugs has to lead to the shelving of many potent molecules. From a review done by Grohganzet al. (2014), it came to the vision that amorphous drugs are extremely unstable and thus it has to be stabilised before use. But, it was also seen that the amorphous counterpart of the drug is much more stable than the crystalline counterpart. To stabilise the amorphous forms, polymer-based solid dispersion technique is used. Thus, various other methods are also used to form amorphouscounterpartswhicharemuch morestableby maintainingin situ condition. Another research was conducted to understand the effect of pH on drug release and functioning. Metformine hydrochloride tablets were taken and by using the USP I test basket apparatus at 100 rotations per minute, the dissolution was conducted. The result showed that the tablets dissolved in HCl of pH 6.8 faster than in HCl of pH 4.5 (Desaiet al.2015). ICH Stability Testing is a set of guidelines that are used and followed to test the stability of any new drugs and the drugs with improved versions. It is also used to test thresholds for different impurities present in the drug. This test is compulsory before making any drug available in the market (Teasdale, Elder and Nims 2017). CONCLUSION From this study, it can be concluded that there is a considerable chance of newer discoveries in this field of production of newer varieties of mesopore molecules which can facilitate the working of a large variety of drugs. The different characterising techniques
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INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION available can also help in the production of optimised and effective mesopore molecules with high drug loading and delivering efficiency.
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION REFERENCES Ahmadi, E., Dehghannejad, N., Hashemikia, S., Ghasemnejad, M. and Tabebordbar, H., 2014. Synthesis and surface modification of mesoporous silica nanoparticles and its application as carriers for sustained drug delivery.Drug delivery,21(3), pp.164-172. Bharti, C., Nagaich, U., Pal, A.K. and Gulati, N., 2015. Mesoporous silica nanoparticles in targetdrugdeliverysystem:Areview.Internationaljournalofpharmaceutical investigation,5(3), p.124. Cheng, Y.J., Luo, G.F., Zhu, J.Y., Xu, X.D., Zeng, X., Cheng, D.B., Li, Y.M., Wu, Y., Zhang, X.Z., Zhuo, R.X. and He, F., 2015. Enzyme-induced and tumor-targeted drug delivery system based on multifunctional mesoporous silica nanoparticles.ACS applied materials & interfaces,7(17), pp.9078-9087. Choudhari, Y., Hoefer, H., Libanati, C., Monsuur, F. and McCarthy, W., 2014. Mesoporous silica drug delivery systems. InAmorphous Solid Dispersions(pp. 665-693). Springer, New York, NY. Costanzo, M., Carton, F., Marengo, A., Berlier, G., Stella, B., Arpicco, S. and Malatesta, M., 2016.Fluorescenceandelectronmicroscopytovisualizetheintracellularfateof nanoparticles for drug delivery.European journal of histochemistry: EJH,60(2). Desai, D., Wong, B., Huang, Y., Tang, D., Hemenway, J., Paruchuri, S., Guo, H., Hsieh, D. and Timmins, P., 2015. Influence of dissolution media pH and USP1 basket speed on erosion and disintegration characteristics of immediate release metformin hydrochloride tablets.Pharmaceutical development and technology,20(5), pp.540-545.
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION Grohganz, H., Priemel, P.A., Löbmann, K., Nielsen, L.H., Laitinen, R., Mullertz, A., Van den Mooter, G. and Rades, T., 2014. Refining stability and dissolution rate of amorphous drug formulations.Expert opinion on drug delivery,11(6), pp.977-989. Hu, X.Y., Lou, H. and Hageman, M.J., 2018. Preparation of lapatinib ditosylate solid dispersions using solvent rotary evaporation and hot melt extrusion for solubility and dissolution enhancement.International journal of pharmaceutics,552(1-2), pp.154-163. Jafari, S., Derakhshankhah, H., Alaei, L., Fattahi, A., Varnamkhasti, B.S. and Saboury, A.A., 2019. Mesoporous silica nanoparticles for therapeutic/diagnostic applications.Biomedicine & Pharmacotherapy,109, pp.1100-1111. Kiwilsza, A., Milanowski, B., Drużbicki, K., Coy, L.E., Grzeszkowiak, M., Jarek, M., Mielcarek, J., Lulek, J., Pajzderska, A. and Wąsicki, J., 2015. Mesoporous drug carrier systems for enhanced delivery rate of poorly water-soluble drug: nimodipine.Journal of Porous Materials,22(3), pp.817-829. Le, T.T., Elyafi, E., Khaliq, A., Mohammed, A.R. and Al-Khattawi, A., 2019. Delivery of poorly soluble drugs via mesoporous silica: Impact of drug overloading on release and thermal profiles.Pharmaceutics,11(6), p.269. Li, X., Zhao, W., Liu, X., Chen, K., Zhu, S., Shi, P., Chen, Y. and Shi, J., 2016. Mesoporous manganese silicate coated silica nanoparticles as multi-stimuli-responsive T1-MRI contrast agents and drug delivery carriers.Acta biomaterialia,30, pp.378-387. Liu, J., Luo, Z., Zhang, J., Luo, T., Zhou, J., Zhao, X. and Cai, K., 2016. Hollow mesoporous silica nanoparticles facilitated drug delivery via cascade pH stimuli in tumor microenvironment for tumor therapy.Biomaterials,83, pp.51-65.
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INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION Marin, M.A., Mallepally, R.R. and McHugh, M.A., 2014. Silk fibroin aerogels for drug delivery applications.The Journal of Supercritical Fluids,91, pp.84-89. Marizza, P., Keller, S.S., Müllertz, A. and Boisen, A., 2014. Polymer-filled microcontainers for oral delivery loaded using supercritical impregnation.Journal of Controlled Release,173, pp.1-9. Morris, S.A. and Slesnick, T.C., 2018. Magnetic resonance imaging.Visual Guide to Neonatal Cardiology, pp.104-108. Saint-Cricq, P., Deshayes, S., Zink, J.I. and Kasko, A.M., 2015. Magnetic field activated drug delivery using thermodegradable azo-functionalised PEG-coated core–shell mesoporous silica nanoparticles.Nanoscale,7(31), pp.13168-13172. Sharma, D.K., 2016. Solubility enhancement strategies for poorly water-soluble drugs in solid dispersions: A review.Asian Journal of Pharmaceutics (AJP): Free full text articles from Asian J Pharm,1(1). Singh, A. and Van den Mooter, G., 2016. Spray drying formulation of amorphous solid dispersions.Advanced drug delivery reviews,100, pp.27-50. Teasdale, A., Elder, D. and Nims, R.W., 2017.ICH Quality Guidelines. John Wiley & Sons, Inc., Hoboken, NJ, USA. Wang, Y., Zhao, Q., Han, N., Bai, L., Li, J., Liu, J., Che, E., Hu, L., Zhang, Q., Jiang, T. and Wang, S., 2015. Mesoporous silica nanoparticles in drug delivery and biomedical applications.Nanomedicine: Nanotechnology, Biology and Medicine,11(2), pp.313-327.
INFLUENCE OF DRUG LOADING, EFFICIENCY AND DISSOLUTION Yang, G., Gong, H., Qian, X., Tan, P., Li, Z., Liu, T., Liu, J., Li, Y. and Liu, Z., 2015. Mesoporous silica nanorods intrinsically doped with photosensitizers as a multifunctional drug carrier for combination therapy of cancer.Nano Research,8(3), pp.751-764. Yao, X., Niu, X., Ma, K., Huang, P., Grothe, J., Kaskel, S. and Zhu, Y., 2017. Graphene quantum dots‐capped magnetic mesoporous silica nanoparticles as a multifunctional platform for controlled drug delivery, magnetic hyperthermia, and photothermal therapy.Small,13(2), p.1602225. Zhang, B., Luo, Z., Liu, J., Ding, X., Li, J. and Cai, K., 2014. Cytochrome c end-capped mesoporous silica nanoparticles as redox-responsive drug delivery vehicles for liver tumor- targeted triplex therapy in vitro and in vivo.Journal of Controlled Release,192, pp.192-201. Zhang, Q., Wang, X., Li, P.Z., Nguyen, K.T., Wang, X.J., Luo, Z., Zhang, H., Tan, N.S. and Zhao, Y., 2014. Biocompatible, uniform, and redispersible mesoporous silica nanoparticles for cancer‐targeted drug delivery in vivo.Advanced Functional Materials,24(17), pp.2450- 2461.