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

Ergothioneine, an amino acid homologue found abundantly in edible mushrooms of the Pleurotaceae family, is gaining attention in the fields of food, medicine, and beauty as a natural substance with high antioxidant properties. Recently, chemical synthesis techniques have also been established, but there is still a need for the development of high-efficiency separation and purification techniques from natural food resources, and it is required to accurately measure the yield and evaluate the level of purification.

Incidents of foreign substances contaminating food have frequently caused public uproar, and in a Cabinet Office survey conducted in January 2014 regarding the promotion of consumer administration, the consumer issue that garnered the most attention was "food safety." To ensure food safety, MST conducts highly accurate analyses for cause investigation, making it possible to determine whether pesticide levels in food exceed the acceptable daily intake. An analysis of miso soup with a small amount of the herbicide glyphosate added revealed that the contaminant could be detected without overlooking any components.

Resveratrol is a type of polyphenol found in red wine and the skins of peanuts, and it is believed to have antioxidant and anti-inflammatory effects. It is known that resveratrol is absorbed in the stomach after ingestion and is rapidly metabolized. During the metabolic process, it becomes glucuronide and sulfate conjugates, but by converting those metabolites back to resveratrol for quantification, the amount of resveratrol absorbed can be calculated.

We conducted LC/MS analysis to compare how the components in commercially available tablet-type headache medications change before and after harsh testing. The LC/MS total ion chromatogram (TIC) revealed the presence of characteristic components that were not found in the new product after the harsh testing, and the precise mass was identified through the MS spectrum. Furthermore, by performing LC/MS/MS analysis, we were able to estimate the structure based on the information from fragment ions. The combination of LC/MS and LC/MS/MS allows for the structural estimation of unknown components.

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.

Chitosan is used in a wide range of fields such as medicine, food, cosmetics, and clothing due to its antibacterial and moisturizing properties. Some cotton swabs, which are everyday items, contain chitosan to provide antibacterial effects. Therefore, we evaluated the chitosan contained in cotton swabs using TOF-SIMS, which allows for visualization through mapping and component assessment through spectral measurement.

On the surface of cell culture dishes, treatments are performed to convert hydrophobic plastic surfaces to hydrophilic ones in order to enhance cell adhesion. In this study, the surfaces of dishes that underwent hydrophilic treatment were evaluated using XPS and TOF-SIMS, revealing an increase in OH and CHO groups. By conducting quantitative evaluations with XPS and qualitative evaluations with TOF-SIMS, it is possible to capture how the surface has changed.

XRF is an analytical method used to evaluate the composition and distribution of constituent elements. A notable feature is that it does not require any special pretreatment for measurements, and it can be performed non-destructively over a wide range from 1.2 mm to several centimeters. As an example of elemental analysis using XRF, we will introduce a case where measurements were conducted focusing on the metal components contained in polymer materials of chemical storage containers, investigating metal contamination that adhered to the container surface during the storage period.

Ion chromatography is a method for detecting ionic components in liquid samples. Additionally, these components that adhere to the surface of solids (materials) are measured by extracting them by immersing in pure water. MST enables qualitative and quantitative analysis of ions and organic acids contained in liquid samples, evaluation of the amount of ions eluted from material surfaces, and investigation of the causes of material corrosion.

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.

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.

Nitrogen is utilized in various forms across a wide range of fields including chemistry, materials, food, and pharmaceuticals. Nitrogen compounds consist of inorganic nitrogen compounds such as nitrates, nitrites, and ammonia, as well as organic nitrogen compounds like amino acids. In the case of samples in aqueous solution, inorganic nitrogen compounds such as nitrate ions, nitrite ions, and ammonium ions can be evaluated using ion chromatography, while organic nitrogen can be assessed using HPLC or LC/MS. Total nitrogen, which includes both inorganic and organic nitrogen compounds, can be evaluated using spectrophotometry.

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.

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.

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.

When describing cleaning methods in brochures for medical devices, it is necessary to confirm the validity of those cleaning methods. In this case, as a verification experiment for the wiping method of medical devices, we applied bovine serum albumin (BSA), a blood model drug, to sheets of acetyl cellulose (TAC), SUS-made scalpels, and glass, and evaluated the residual components before and after wiping using TOF-SIMS. As a result, it was found that ethanol is more suitable than water for wiping BSA, and that the wiping effectiveness varies depending on the substrate. Measurement method: TOF-SIMS Product field: Medical devices and pharmaceuticals Analysis purpose: Composition evaluation, identification, composition distribution evaluation, failure analysis, defect analysis For more details, please download the materials or contact us.

TOF-SIMS is an effective method for analyzing the distribution and penetration of target components in samples, as it can simultaneously perform elemental analysis and molecular information analysis of organic and inorganic substances, as well as image analysis. This document presents the results of image analysis of the "cross-section and surface" of hair and the "surface" of hair using siloxane-based hair care agents. It was confirmed that there are differences in the distribution of components between the cuticles of the tip and the root of the hair. Measurement method: TOF-SIMS Product field: Pharmaceuticals and cosmetics Analysis purpose: Composition evaluation, identification, composition distribution evaluation For more details, please download the document or contact us.

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.

TOF-SIMS identifies components from the mass of molecular ions, eliminating the need for labels such as fluorescent substances, allowing for imaging without their influence. Additionally, cross-sectional imaging enables the evaluation of distribution in the depth direction. In this study, a gel formulation of indomethacin was applied to three-dimensional cultured human skin, visualizing the distribution of the permeated active ingredient. As a result, it was found that indomethacin is concentrated on the surface side of the stratum corneum. Furthermore, depth profile analysis observed a gradual penetration towards the cell layers.

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.

Medical injection needles reduce puncture resistance and lessen the physical burden on patients by coating the surface of the metal tube with silicone. To maintain the performance of the needle, it is important that the entire surface is covered with a coating film. This report introduces a case where imaging analysis of the opening at the tip of the injection needle was conducted using TOF-SIMS to evaluate whether the coating film was applied. Since TOF-SIMS detects information from the very surface, it can assess the condition of the coating film without detecting the underlying elements.

The majority of pharmaceuticals are crystalline and are known to have multiple crystal forms. Even for the same substance, the physical and chemical properties, such as solubility, can differ depending on the crystal form, which can also affect the efficacy and safety of the drug. Therefore, the identification of crystal forms is extremely important. In this case, XRD analysis was conducted to evaluate the crystal forms of the active pharmaceutical ingredient in question, both for the pure active pharmaceutical powder and for the commercial products.

This case study introduces an analysis of the condition of the cuticle on the hair surface using AFM. AFM is a method for three-dimensional measurement of nanoscale surface roughness. Since the analysis is conducted in the atmosphere, it does not cause degradation or gas release of organic materials, allowing for an evaluation of the sample's original shape. In this case study, we assessed the degree of cuticle opening, the distribution of adhered substances, and the roughness evaluation of different areas through images, as well as quantitatively evaluated the surface roughness through numerical processing. This method is effective for evaluating the condition of hair after shampooing and the application state after applying styling products.

In MST, atomic-level TEM analysis is possible under atmosphere control (and cooling). This document presents a case where LiCoO2 particles, extracted from a lithium-ion secondary battery without exposure to the atmosphere, were processed using FIB and analyzed with TEM under atmosphere control and cooling. STEM observation and EDX analysis were conducted while cooling to -174°C, allowing for a visual confirmation of the atomic arrangement. This method can be applied to materials with low thermal stability and crystalline materials that undergo changes in the atmosphere for high-resolution analysis.

When materials undergo chemical reactions and phase changes with increasing temperature, performing XRD measurements while heating is effective. We present a case where high-temperature XRD measurements were used to identify the decomposition products of copper(II) sulfate pentahydrate. The results showed that the diffraction peaks changed at the temperature where decomposition occurred, clearly confirming the changes in the crystal structure. In MST, it is possible to conduct Out-of-plane XRD measurements and In-plane XRD measurements while heating.

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.

TOF-SIMS identifies components based on the mass of molecular ions, eliminating the need for labels such as fluorescent substances, allowing for imaging evaluations without their influence. Additionally, by performing cross-sectional imaging, it is possible to assess distribution in the depth direction. In this study, a gel formulation of indomethacin was applied to rat skin for 2 hours, and the distribution of the permeated active ingredient was visualized. As a result, indomethacin was found to be highly concentrated at approximately 5μm on the stratum corneum surface, and the depth profile analysis showed that it was gradually permeating.

TOF-SIMS allows mass imaging analysis of samples ranging from micrometers to centimeters in size. We conducted mass imaging analysis using TOF-SIMS on the cross-section of a capsule-type drug. We performed cross-section processing and present imaging examples focusing on the entire drug (approximately 7mm x 20mm) and a single granule inside it (approximately 500μm in diameter).

Aluminum oxide is used in various industrial machinery and manufacturing equipment parts due to its excellent wear resistance and heat resistance. Additionally, its chemical stability and high insulation properties make its thin films suitable for applications such as catalyst supports and insulating layers in magnetic tunnel junctions. The evaluation of the fine structure of aluminum oxide films, which can take on amorphous structures or various crystalline structures depending on the film formation conditions, is effectively conducted using XAFS. This document presents a case study of the quantitative separation of coordination structures (AlO4, AlO6) in amorphous aluminum oxide thin films.

To understand the pharmacokinetics of drugs, it is important to know the concentration of drugs in body fluids. While blood is generally used for quantitative analysis of drugs absorbed into the body, recent years have seen a growing interest in the analysis of body fluids such as tears and saliva, which are less burdensome to collect than blood. At MST, it is possible to quantitatively analyze components contained in not only blood and urine but also tears and saliva with high sensitivity using LC/MS/MS. Below are examples of glucose analysis in tears and 5-fluorouracil analysis in saliva.

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).

The metal processing surfaces of injection needles are generally rough, but it is known that using injection needles with rough surfaces can cause discomfort to patients. Therefore, to reduce surface friction caused by rough surfaces, biologically inert silicone lubricants are used on injection needles. This document presents a case study evaluating roughness using AFM (Atomic Force Microscopy) based on the presence or absence of surface processing with silicone lubricants.

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.

Polymers are known to exhibit diverse functions by altering their composition and structure, and they are utilized in various products. In the evaluation of polymers, assessment in real environments is crucial. This time, we will introduce a case where the shape of polymers on a substrate was visualized in the atmosphere and in aqueous solution using an environmental control atomic force microscope (AFM). Additionally, by combining data analysis, we quantified the dispersion of polymer particles.

Dental implants are artificial devices that are embedded in the jawbone when teeth are lost due to cavities or periodontal disease. Since they are implanted in the body, evaluating the condition of the surface area that comes into direct contact with biological tissue is important. TOF-SIMS not only provides qualitative analysis of the top surface but also excels in depth resolution at the top surface, allowing for highly sensitive evaluation of the condition in the depth direction. This case summarizes the results of evaluating the state of titanium in dental implants in the depth direction.

Dental implants are artificial devices that are embedded in the jawbone when teeth are lost due to cavities or periodontal disease. The materials used for implants are often titanium or titanium alloys, and various coatings are applied to the surface to promote the bonding between the implant and the bone. Since implants are embedded in living organisms, the safety assessment of the surface area that comes into direct contact with biological tissues is crucial. XPS can evaluate the composition and bonding state of the very surface (approximately 5 nm). This document presents examples of evaluations conducted using XPS.

The Karl Fischer titration method is a way to evaluate the moisture content, and the method of introducing the sample into the device varies depending on the properties of the sample. Here, we will introduce two sample introduction methods for titration.

Dental implants are artificial devices that are embedded in the jawbone when teeth are lost due to cavities or periodontal disease. Since implants are directly embedded in the body, evaluating their safety is crucial. This document presents a case where the quantification of impurity elements was conducted using Dynamic-SIMS. The analysis results revealed that, in addition to the main component Ti, O and Fe were also present. Dynamic-SIMS can evaluate the elemental distribution in a depth of several micrometers at the order of ppm to ppb.

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.