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.

When evaluating the particle size and structure of fine particles dispersed in a liquid, conventional methods involved drying the liquid to extract the fine particles as a powder, which were then measured using an electron microscope. However, this method was not suitable for investigating how fine particles are actually dispersed in the liquid used. Therefore, we will introduce a case where cryo-processing and SEM observation were performed to directly evaluate how fine particles are dispersed within a liquid sample.

Glucosylceramide (plant ceramide), one of the glycosphingolipids, has been reported to have moisturizing effects and improvements for atopic dermatitis, making it a component of interest in the beauty field. Although the main structural components of glucosylceramide vary among plants, qualitative analysis can be performed using LC/MS. Additionally, since glucosylceramide has multiple molecular species even from the same plant source, quantitative analysis can be conducted with high precision using an evaporative light scattering detector (ELSD).

Measuring hair and obtaining the distribution of components within it is effective when investigating the effects of hair care and dyeing. We will introduce a case where gray and black hair were collected from the same individual and the internal component distribution was evaluated. A cross-section of the hair was created, and TOF-SIMS measurements were conducted. TOF-SIMS can provide distribution information on inorganic substances such as metals and organic molecules. This time, we focused on measuring the distribution of metals in the hair cross-section.

Using TOF-SIMS for ion imaging analysis of hair (beard) cross-sections, we investigated the distribution of long-chain fatty acids, which are also detected as sebum. As a result, it was found that the distribution varies depending on the type of fatty acid.

The way makeup is removed varies depending on the type of cleansing oil, even with the same washing method. To investigate the cleansing effect, we evaluated the remaining components after washing lipstick with oil using TOF-SIMS. This report introduces a case where the differences in cleansing effects due to the type of cleansing oil were assessed by conducting relative comparisons of the components of the lipstick (such as pigments and oils) between samples.

Emulsification technology is a fundamental technology in cosmetic development and is utilized across various cosmetics. Changes in the structure of emulsifiers are closely related to the balance of water and oil in the product, the permeability of encapsulated active ingredients, cleansing power, and changes in user experience, making its analysis very important.

Transmission electron microscopy (TEM) allows for morphological observation and elemental analysis on the order of μm to nm. Since eyeshadows are aggregates of solid particles, we conducted the analysis directly using TEM. After TEM observation, we performed EDX analysis on specific areas within the field of view to estimate the materials based on the constituent elements. Furthermore, it is possible to distinguish crystal types through EELS analysis.

We analyzed the hair cross-sections of five individuals (A to E) who use different hair care products in their daily lives using TOF-SIMS. As a result, it was found that the types of hair care products lead to differences in the detected components and their distribution within the hair.

We investigated the penetration state of components under various immersion conditions by soaking unconditioned hair, specifically facial hair, in a conditioner or treatment. In the facial hair soaked in conditioner, it was observed that siloxanes penetrated to the hair cortex over time, while high fatty acids appeared to be lost. In the facial hair soaked in treatment, nitrogen-containing organic substances did not penetrate the hair cortex and were only distributed around the cuticle.

The hair roots of human hair (both shed hair and pulled hair) were pressed against a Si wafer, and imaging measurements (surface analysis) were conducted on the transferred components. Shed hair shows a strong tendency for ■K and ●phospholipids to be present only at the tip of the hair root. Additionally, it is believed that the entire hair root contains ■CnHmCOOH (n=17–31) fatty acids (derived from human sebum), ●amide components derived from keratin plugs, ◆nitrogen-containing organic acids with a mass of 500–700, and ◆organic substances with a mass around 800 that are aggregated. However, the organic substances containing two COOH groups derived from human sebum, which are observed in pulled hair, show a weak tendency.

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.

Pyrolysis GC/MS is a gas chromatography-mass spectrometer equipped with a pyrolysis device in the sample introduction section. For polymer materials that previously required complex pretreatment, samples can now be introduced into the GC for analysis without pretreatment by heating and decomposing them with the pyrolysis device. Additionally, by varying the temperature conditions of the pyrolysis device and the sampling conditions (double-shot method), it is possible to obtain two different types of information, such as additives and polymer materials, separately from the same sample, making the analysis of unknown polymer materials easier.

To observe and analyze the internal structure of organic materials and liquid samples that are sensitive to heat, it is necessary to suppress temperature increases caused by processing or electron beam irradiation and to conduct a series of analyses while maintaining the original structure of the sample. In this case study, we will introduce an example where a cosmetic was used as an evaluation sample, and structural analysis was performed from cross-section FIB processing to SEM observation and EDX analysis while maintaining a cooling environment.

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.

The surface shape of foundation puffs and the adhesion of cosmetics were evaluated using a digital microscope. The digital microscope has a greater depth of field compared to optical microscopes, allowing for accurate observation of large uneven objects that could not be focused on with a microscope. The observation results of commercially available foreign puffs are shown in Figures 1 to 4. The surface shape of the puffs and the adherence of the foundation can be confirmed. Additionally, as shown in Figure 5, it is also possible to directly observe the surface of the hand.

The functionality of films is known to be determined by factors such as material, thickness, and layer structure. In this study, we evaluated the layer structure of polyethylene-based multilayer films commonly used as food wrap. By confirming that the film is primarily composed of polyethylene using FT-IR, and employing GCIB (Ar cluster) for sputtering, we were able to clearly visualize the structure where polyethylene and nylon 6 are layered within a thickness of 10μm through depth profiling with TOF-SIMS.

Odors are commonly expressed in various ways, such as "fragrance" that gives pleasure and "stench" that causes discomfort. Odors rarely exist as a single type of odor component; instead, they are typically a mixture of various odor components. To visualize these complex odors, instrumental analysis using gas chromatography-mass spectrometry (GC/MS) is effective. This document introduces the flow of odor component analysis and presents a case study of simultaneous analysis of unpleasant odors.

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.

Geosmin and 2-methylisoborneol (2-MIB) are produced by cyanobacteria or actinomycetes and are considered substances that cause odor and taste disturbances in drinking water sourced from surface water such as dams, lakes, and rivers, as well as being known as substances that cause musty odors. This case presents the results of measuring geosmin and 2-MIB contained in water. Detection at ppt (ng/L) levels is possible using GC/MS.

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.

Volatile organic compounds (VOCs) are used during the cleaning of semiconductors and industrial products and may be present in trace amounts in cleaning water, etc. VOCs in water are a concern because even in trace amounts, they can cause odors and health issues. Therefore, environmental standards and discharge standards have been established, and methods capable of measuring low concentrations are required. This case presents an example of detecting trace VOC components (sub-ppb level) in water by introducing components concentrated by P&T (Purge & Trap) into GC/MS.

The concentration of volatile components that humans perceive as odors can be very low, and they may not be detectable using the conventional HS (Headspace) method for GC/MS measurements used for analyzing volatile components. By using Solid-Phase Micro Extraction (SPME), it becomes possible to concentrate the volatile components and introduce them into GC/MS, allowing for the detection of many trace components. This document presents a case study analyzing odor components in trace amounts of essential oils.

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.

Hydrogen water is said to be able to remove active oxygen in the body, and attention is being drawn to its antioxidant effects. However, the amount of hydrogen that dissolves in water is minimal, and when left in the air, hydrogen gradually escapes. Additionally, because hydrogen is a very small molecule, it is known that some storage containers cannot maintain it for long periods. Therefore, the choice of storage container and method is considered important. This case presents the results of a GC (TCD) analysis showing how much hydrogen has escaped from hydrogen water transferred to a paper cup compared to a pouch-type storage container.

TOF-SIMS is a highly effective method for investigating the causes of foreign substances, contamination, and discoloration in various processes, as it allows for localized analysis of specific areas and simultaneous analysis of elemental composition and molecular information of organic and inorganic substances through the obtained mass spectrum. Additionally, it enables image analysis, making the visualization of molecular information of organic substances possible. This document summarizes the analysis results of discoloration in clean suits, which are textile products. From the qualitative results obtained by TOF-SIMS, it was inferred that the discolored areas may be due to sebum.

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.

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.

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.

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).

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.

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.

In Raman analysis, the component distribution in the depth direction can be confirmed through measurements from the surface. It is effective for materials that easily transmit light, allowing for non-destructive evaluation without the need for cross-section processing or ion sputter etching. This document presents an example of evaluating each layer of an organic multilayer film using Raman 3D mapping. The results indicated that the organic multilayer film is composed of four layers. Additionally, by comparing with library data, the components of each layer were identified.

In recent years, the market size for soft drinks has been expanding, and various studies are being conducted to further enhance their flavor. One report suggests that including an appropriate amount of dehydroascorbic acid in soft drinks can improve their taste. Dehydroascorbic acid is also produced by the oxidation of L-ascorbic acid, which is used as an antioxidant in beverages, so prompt analysis after opening the sample is necessary to obtain accurate values. This document measures the amount of dehydroascorbic acid over time after the sample has been opened.