一般財団法人材料科学技術振興財団　MST List of Products and Services

In dental caries treatment, adhesives are used to integrate the filling material used to fill the "cavity" with the tooth structure. The adhesive must have a strong bonding strength with the tooth and the ability to withstand acids and heat that may occur in the oral cavity over a long period after treatment. Observing the adhesive interface is an effective means for evaluation and consideration. By using a manufacturing method that employs FIB processing technology, we were able to achieve effective results that could not be obtained with conventional ultra-thin sections made with diamond knives, and we would like to introduce this.

To evaluate the component distribution in mouse tibia, we prepared tibial sections and conducted imaging analysis using TOF-SIMS. The distribution of components derived from mice, such as K, Ca, calcium phosphate, and phospholipids, was confirmed. Since TOF-SIMS identifies components based on the mass of molecular ions, it does not require labeling substances like fluorescent materials, allowing for distribution evaluation without the influence of labeling agents. This technique can be applied to drug dynamics analysis and research on Drug Delivery Systems (DDS), enabling imaging of drug distribution within organs.

To evaluate the components contained in commercially available tablet-type headache medications and their distribution, mass imaging analysis of the tablet cross-section was performed using TOF-SIMS. It was found that Al and Mg, derived from antacids, and the active ingredient acetylsalicylic acid were separated into two distinct regions. Additionally, as a harsh test, the tablets were placed in an environment of 50°C and 75% humidity for four weeks to assess changes in the components. This is effective for visualizing formulation research and stability evaluation. Measurement method: TOF-SIMS Product field: Biotechnology and Pharmaceuticals Analysis purpose: Composition evaluation, identification, and composition distribution evaluation For more details, please download the materials or contact us.

The sample concentration needle is a device that concentrates volatile components by sucking them from vials or sampling bags and adsorbing the volatile components passing through the needle onto an adsorbent medium, which is then introduced into GC/MS. There are different adsorbent media available, such as "for organic solvents," "for fatty acids," and "for amines," which are used depending on the target components. In the headspace method used for the analysis of volatile components, it is common to heat the sample to obtain sensitivity; however, in analyses using the sample concentration needle, heating is not necessary, allowing only the volatile components to be supplied for GC/MS analysis at room temperature.

The ionization method for LC/MS is commonly ESI (Electrospray Ionization). In ESI, if low-polarity components cannot be ionized, APCI (Atmospheric Pressure Chemical Ionization) is available as a highly sensitive detection method. It is important to choose the optimal ionization method according to the target components in order to obtain data that aligns with the objectives.

The electron diffraction method using an electron microscope is classified into three types based on the way the electron beam is incident on the sample. The characteristics of each type and examples of data are presented. It is necessary to choose the appropriate method according to the size of the evaluation object and the analysis purpose.

In XPS analysis, the binding state evaluation of the material surface is conducted by observing the energy of photoelectrons obtained through X-ray irradiation. It allows for the assessment of whether metal elements are in an oxidized state, and for elements with significant energy shifts (chemical shifts) due to oxidation, it also enables the evaluation of the presence and proportion of multiple valences. Below are the main metal elements and oxides for which multiple valence evaluations are possible.

In XPS analysis, in addition to the photoelectron peaks used for evaluation, photoelectron peaks from other orbitals and Auger peaks from X-ray excitation are also detected. Depending on the combination of elements, these sub-peaks can overlap with the target peak and interfere with the evaluation. *Typically, a strong photoelectron peak emitted from an inner shell level close to the outer shell is used. In the quantitative calculations of XPS analysis, the removal of such interfering peaks is primarily performed using the following two methods: 1. Removal using sensitivity coefficient ratios 2. Removal using waveform separation

HF (hydrofluoric acid) is widely used in processes such as wet etching of SiO2 and plays a very important role in semiconductor manufacturing. However, it is also a very dangerous chemical that can penetrate the skin and damage bones, so care must be taken when handling it. The bone erosion caused by HF occurs because Ca, which exists in the bone as apatite, reacts with HF to produce CaF2. This document presents a case study evaluating the changes in this reaction using Raman analysis.

Samples such as lithium-ion secondary battery materials that deteriorate when exposed to the atmosphere, and organic materials that change due to heat during processing and observation, are difficult to observe structurally using TEM under normal environmental conditions. Our organization has established a system that controls the atmosphere to minimize exposure to air, and further cools the samples for processing, observation, and analysis, allowing us to prepare TEM thin film samples while preserving the original structure of the samples for observation and analysis.

Samples such as lithium-ion secondary battery materials that deteriorate when exposed to the atmosphere and organic materials that change due to heat during processing and observation have made it difficult to observe their original structures using TEM and SEM. By observing them with a high-resolution SEM equipped with FIB under controlled atmospheres without exposure to the air, we can understand the original states of particles and electrolytes. Additionally, it is compatible with cooling, which helps to suppress deterioration caused by heat.

When analyzing samples containing nitrogen compounds using GC, simultaneous measurement with MS (mass spectrometer) and NPD (nitrogen-phosphorus detector) allows for the detection of components that do not appear as peaks in the MS, enabling the acquisition of MS spectra from their retention times for qualitative analysis. In this case, a sample containing trace amounts of the nitrogen-containing compound trimethylamine was measured using GC/MS/NPD. A peak that was buried in the baseline in the MS was confirmed by the NPD, allowing for the qualitative identification of trimethylamine from the mass spectrum at the same retention time.

Biological samples and foods contain multiple triglycerides with different fatty acid compositions. In the analysis of total fatty acids, triglycerides are broken down into glycerol and fatty acids for measurement, but information about the combination of fatty acids in the triglyceride state is lost. Here, we present a case study that analyzes the fatty acid composition of triglycerides in food by directly analyzing them using GC/MS.

Titanium tetraalkoxide is an essential reagent for the Katsuki-Sharpless asymmetric epoxidation and is affected by oxidation in the atmosphere. In this case, we present an investigation using TOF-SIMS on how titanium tetraalkoxide (titanium tetra-isopropoxide) changes under controlled atmosphere and after exposure to air. In MST, the evaluation of the complex can be performed without the influence of atmospheric oxidation due to atmosphere control. Measurement method: TOF-SIMS Product fields: Biotechnology, Pharmaceuticals, Cosmetics, Daily necessities Analysis purpose: Deterioration investigation, Reliability assessment For more details, please download the materials or contact us.

When peptides are measured using LC/MS/MS, characteristic fragment ions are obtained, allowing for the analysis of the amino acid sequence that makes up the peptide. Additionally, because peptides are separated and analyzed by LC, it is possible to analyze the sequences even in samples containing multiple peptides or impurities. Here, we present a case study where low molecular weight peptides were analyzed using LC/MS/MS, and the amino acid sequences were estimated.

In this document, we prepared cross-sectional slices of mouse brain, heart, liver, kidneys, and teeth, and performed imaging using TOF-SIMS. The imaging area can range from approximately 10 μm to several centimeters, allowing for high-resolution analysis tailored to the focus of interest. Slices can be prepared according to the various organs of the organism, enabling imaging of their components. Additionally, this method is effective for visualizing the distribution of administered components within biological materials in pharmacokinetic studies and pharmaceutical research and development. Measurement method: TOF-SIMS Product field: Biotechnology, Pharmaceuticals Analysis purpose: Composition distribution evaluation For more details, please download the document or contact us.

In protein composition analysis, there are methods to examine only the target protein after electrophoresis, but this document introduces "shotgun analysis," which comprehensively investigates proteins. In shotgun analysis, after separating proteins and obtaining mass information using LC/MS/MS measurements, a database search is conducted to comprehensively analyze the proteins present in the solution.

GPC (Gel Permeation Chromatography) is one of the separation modes of HPLC and is a method for evaluating the molecular weight of polymer compounds. It can determine several average molecular weights (Mn), weight average molecular weight (Mw), and polydispersity (Mw/Mn) in a single analysis, and it is also possible to compare the distribution profiles. It is also referred to as SEC (Size Exclusion Chromatography).

In recent years, the development of alternative methods to animal testing for the efficacy and safety testing of pharmaceuticals and cosmetics has been progressing, with particular attention being paid to testing methods using three-dimensional cultured skin. In this case study, a percutaneous absorption test of a cosmetic (lotion) was conducted using three-dimensional cultured human skin, which was measured using AFM (Atomic Force Microscopy). This allows for a visual evaluation of the microstructure of the skin surface, and it is also possible to quantitatively assess the roughness of any specific area. By measuring under atmospheric conditions, it is possible to observe the samples while minimizing alterations that would occur under vacuum conditions.

In recent years, the development of alternative methods to animal testing has progressed in the efficacy and safety testing of pharmaceuticals and cosmetics, with particular attention being paid to testing methods using three-dimensional cultured human skin. In this case study, a permeation test of indomethacin was conducted using a Franz cell, and TOF-SIMS and LC/MS/MS measurements were performed on the same skin sample. LC/MS/MS was used to quantify skin concentration and skin permeation, while TOF-SIMS was used to evaluate the component distribution within the skin. Measurement methods: TOF-SIMS, LC/MS, cryo-processing, cutting Product fields: Biotechnology, pharmaceuticals, cosmetics Analysis objectives: Composition distribution evaluation, safety testing For more details, please download the materials or contact us.

TDS can evaluate the temperature dependence of the desorption of inorganic and organic gases that are released with increasing temperature. Therefore, it is effective for assessing the degassing of samples based on the baking temperature. The results of TDS analysis after baking the resist film at 50°C and 200°C are shown. It was confirmed that the degassing peaks detected up to 200°C after "baking at 50°C" were not detected after "baking at 200°C."

TDS is a method that heats samples in high vacuum (1E-7 Pa) and investigates the gases released from the samples using a mass spectrometer. Since it is a vacuum system, it is not suitable for the large release of organic substances, but it can be evaluated by adjusting the sample amount. Below is an example of TDS analysis conducted on a resist film. Desorption gases originating from the resist film, such as organic substances, water, H2S, and SO2, were detected. It was also found that the desorption temperatures varied depending on the components.

We will introduce a case where a sheet coated with graphite negative electrode particles used in lithium-ion secondary batteries was analyzed using TOF-SIMS. It was confirmed that graphite and PVDF are distributed on the surface of a single powder particle. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a method suitable for qualitative analysis and imaging of organic and inorganic substances on surfaces from the mass spectrum of secondary ions. It is effective for evaluating the distribution of minute foreign substances and stains due to its high resolution. Measurement method: TOF-SIMS Product field: Secondary batteries Analysis purpose: Composition distribution evaluation For more details, please download the materials or contact us.

By using high-sensitivity LC-MS (Q-TOF type), qualitative analysis of low-concentration components such as metabolites in biological samples is possible. It allows for the search for components that have undergone metabolism such as addition or conjugation in the body, as well as inter-sample comparisons aimed at investigating temporal changes and individual differences. After consuming a high-concentration catechin beverage and collecting urine, both unchanged catechin and the metabolite catechin-glucuronide conjugate were confirmed. The amounts of catechin and metabolites in the urine of eight individuals were plotted for excretion over 0.5 to 8 hours post-consumption, and comparisons were made.

Lithium carbonate, widely used in the treatment of mania and bipolar disorder, must be administered while maintaining an appropriate blood concentration to prevent lithium toxicity. Therefore, regular measurement of blood concentration (therapeutic drug monitoring: TDM) is required. Analysis using ICP-MS (inductively coupled plasma mass spectrometry) allows for the quantification of lithium concentrations in the blood across a wide range, from subtherapeutic levels to toxic levels.

Organic acids are a general term for acidic organic compounds. In addition to components found in food, such as citric acid, which contributes to sourness, and inosine acid, which contributes to umami, they are used as raw materials and additives in cosmetics, pharmaceuticals, and industrial fields, with a wide range of applications. This document introduces simultaneous analysis of 12 organic acid components using HPLC and case studies of soft drink analysis. After separating each component in the column, selective analysis can be performed without being affected by interfering components by reacting with a color reagent (BTB solution) for detection. It is possible to simultaneously qualitatively and quantitatively analyze organic acids in liquid samples as well as in extracts from solids.

Hair that has been damaged by factors such as hair color, ultraviolet rays, and aging undergoes structural changes, and measuring these structural changes is important for the research and development of hair care products. In this case, we observed the structure of hair using X-ray CT. Furthermore, by performing image analysis on the obtained CT cross-sectional images, we created histograms of the void volume in the cortex and the spacing of the cuticles. By combining X-ray CT and image analysis in this way, it is possible to quantitatively evaluate the three-dimensional structure of hair. Measurement methods: X-ray CT, computational science, AI, data analysis Product fields: Biotechnology, pharmaceuticals, cosmetics Analysis objectives: Shape evaluation, structural evaluation For more details, please download the materials or contact us.

We observed a sample mixed with three types of lactic acid bacteria using SEM, and extracted the bacteria by type using deep learning from the obtained images. Furthermore, we conducted data analysis to determine the presence ratio on the cell cycle based on the shape of the lactic acid bacteria. Measurement methods: SEM, computational science, AI, data analysis Product fields: Biotechnology, pharmaceuticals, daily necessities, cosmetics, food Analysis purpose: Shape evaluation, product investigation For more details, please download the materials or contact us.

Saturation Transfer Difference (STD) NMR is a type of NMR analytical method used to identify low molecular weight compounds that interact with proteins, demonstrating significant power in drug screening and other applications. This document presents a case study where specific compounds that interact with a particular protein were identified from multiple compound groups using STD-NMR measurements. Measurement method: Nuclear Magnetic Resonance Spectroscopy (NMR) Product fields: Biotechnology, Pharmaceuticals, Cosmetics, Food Analysis purpose: Screening, Drug Design, Interaction Evaluation For more details, please download the document or contact us.

Nuclear Magnetic Resonance Spectroscopy (NMR) is an analytical method that can obtain various information about molecular structure, intermolecular interactions, and molecular mobility, targeting various compounds including organic substances. This document presents examples of measurements conducted with a super low-temperature probe, which achieved higher sensitivity compared to a general-purpose room temperature probe.

Polymers can change shape depending on environmental factors such as temperature, humidity, and solvents, and by varying the environmental conditions during evaluation, we can deepen our understanding of their physical properties. In this study, we conducted heating and cooling experiments using polycaprolactone (PCL), which is known for its biodegradability. PCL has a melting point of approximately 60°C, and we continuously observed through video how it changes from a crystalline state to an amorphous state upon heating, and how it recrystallizes upon cooling. Measurement method: AFM Product fields: Biotechnology, Pharmaceuticals, Daily Goods, Food Analysis purpose: Shape evaluation For more details, please download the materials or contact us.

NMN, a type of niacin derivative, is known to be involved in the function of sirtuin genes, often referred to as longevity genes, and has gained attention in recent years. This document presents a case where the NMN content of commercially available capsules was quantitatively analyzed using NMR without the use of standard samples. Measurement method: NMR Product fields: Biotechnology, Pharmaceuticals, Cosmetics, Food Analysis purpose: Impurity evaluation, Product investigation, Safety testing For more details, please download the document or contact us.

Both TOF-SIMS and MALDI-MS are techniques capable of imaging mass spectrometry (IMS), each with different strengths in terms of components, mass, and spatial resolution. TOF-SIMS excels in low-mass components and allows for imaging with high surface resolution. On the other hand, MALDI-MS specializes in high-mass components and has a wide variety of lipids that can be imaged. Here, we will introduce examples of measurements taken with TOF-SIMS and MALDI-MS, using the results of imaging mass spectrometry of lipids in mouse testes as an example.

LDI (Laser Desorption Ionization) is a method that uses only the energy of ultraviolet lasers to sublime and ionize molecules. On the other hand, MALDI (Matrix-Assisted Laser Desorption Ionization) is a method that sublimates and ionizes molecules by exposing a sample mixed with a matrix to ultraviolet lasers.

In this method, the differences in the mass of bases are analyzed using MALDI-TOF-MS to determine the DNA base sequence. This allows for the detection of SNPs (single nucleotide polymorphisms), INDELs (insertions/deletions), CNVs (copy number variations), and more. It is characterized by the ability to analyze a large number of samples and detect a wide range of genes at once. - Multiplex PCR and MALDI-TOF-MS enable simultaneous analysis of up to 40 mutation sites. - Mass spectrometry specialized for the detection of bases (A/T/G/C) is possible. - A variety of analytical tools are available that have been pre-designed to detect target genes based on specific purposes. - Custom designs for analytical tools are also possible.

NMN (β-nicotinamide mononucleotide) is known to be involved in the function of sirtuin genes, which are also referred to as longevity genes, and has garnered attention in recent years. This document focuses on NMN, monitoring the changes in 1H-NMR spectra due to heating treatment in water, and presents an analysis of the decomposition and changes of NMN caused by heat. Measurement method: NMR Product fields: Biotechnology, Pharmaceuticals, Cosmetics, Food Analysis objectives: Composition evaluation, Identification, Impurity evaluation, Deterioration investigation For more details, please download the document or contact us.

This method is a gene analysis technique that utilizes mass spectrometry with MALDI-TOF-MS, allowing for the analysis of multiple SNP sites in a single measurement. Up to 40 SNPs can be measured simultaneously across 190 samples. The overall analysis follows the flow outlined below. Primers designed to amplify the target SNP regions without overlapping mass peaks, along with primers designed to extend only one base at each SNP site, are used to create mass differences in the DNA fragments, from which the bases are determined based on the detected mass peaks.

Among physiological active compounds, there are many that act by targeting proteins. Therefore, obtaining structural insights into the interactions between small molecules and proteins is very important for drug development. This document presents a case study analyzing the interactions between L-tryptophan and bovine serum albumin (BSA) in solution using NMR and molecular dynamics calculations.

Real-time PCR is a method that detects the amplification of DNA fragments from PCR reactions as a fluorescent signal for each cycle. This introduces SNP (Single Nucleotide Polymorphism) analysis using the probe method of real-time PCR. Specific base sequences (probes) labeled with a reporter (fluorescent dye) and a quencher (quenching substance) are used to repeat the three steps shown below: 1) to 3). By using different reporters for each base, the SNP base is identified from the fluorescence intensity. Reactions at each step: 1) Thermal denaturation DNA is converted from double-stranded to single-stranded. 2) Annealing and hybridization Primers and probes specifically bind to single-stranded DNA. 3) Extension reaction The probe is degraded by the extension reaction of the primer, releasing the reporter from the quencher, resulting in fluorescence.

SNP (Single Nucleotide Polymorphism) refers to the parts of the DNA sequence that differ by a single nucleotide among individuals. It is believed that SNPs can lead to different characteristics such as physical traits and are also related to drug response. Therefore, SNP analysis is expected to be applied in personalized medicine. This document introduces the characteristics of real-time PCR and mass array methods among SNP analysis techniques. It is effective to choose the method according to the specific SNP locations, number of SNPs, and their frequencies that need to be investigated.

Tensile Test It is possible to perform X-ray CT measurements while applying stress in the direction of pulling the sample. Compression Test It is possible to perform X-ray CT measurements while applying pressure in the direction of compressing the sample. Temperature Control It is possible to perform X-ray CT measurements while adjusting the temperature of the stage.

TOF-SIMS and MALDI-MS, which are representative mass spectrometry methods for solid sample surfaces, both enable qualitative analysis and imaging analysis. TOF-SIMS, which utilizes hard ionization methods, can detect inorganic and organic components with masses up to several hundred with high sensitivity. On the other hand, MALDI-MS, which employs soft ionization methods, can detect polymers in the range of thousands to tens of thousands. Additionally, the spatial resolution of the images also varies depending on the diameter of the irradiation beam.

NMR is typically performed using the resonance signals of deuterium (2H or D) nuclei in deuterated solvents for reasons such as ensuring the stability of the magnetic field. However, by using the resonance signals of proton (1H) nuclei, measurements can also be conducted with light solvents (i.e., regular solvents) (No-D measurement method). The effective measurements for the No-D method are as follows: - Measurements to evaluate interactions with light solvents (e.g., degradation studies in light solvents) - Measurements of samples that cannot use deuterated solvents (e.g., samples in the biochemical field such as proteins) - Measurements of samples containing volatile components - Measurements of samples for which no dissolvable deuterated solvents are available.

We created skin tissue samples and evaluated the distribution of biogenic components in freeze-dried samples using TOF-SIMS. Since TOF-SIMS identifies components based on the mass of molecular ions, it does not require labels such as fluorescent substances, allowing for the evaluation of distribution without the influence of labeled materials. The mapping results confirmed that arginine, a natural moisturizing factor (NMF), and cholesterol, which retains moisture as an intercellular lipid, are localized in the stratum corneum. This method is also effective for assessing the permeation state during drug application.

This document presents a case study of Rietveld analysis applied to the powder X-ray diffraction data of Li(Ni, Mn, Co)O2, which is used as a positive electrode active material in lithium-ion secondary batteries. By seeking a crystal structure model that reproduces the measured powder X-ray diffraction data through simulation, it is possible to precisely calculate crystal structure parameters such as lattice constants, site occupancy rates, and the proportion of cation mixing, which can then be used to discuss the material properties.