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.

The main component of Korean ginseng, which is widely used as a herbal medicine, is a saponin called ginsenoside. Ginsenosides are classified based on the way sugars are attached, and currently, about 30 types have been discovered. In this case, we will introduce an example of analyzing ginsenosides using LC/MS/MS. With LC/MS/MS, we confirmed that the double filtering effect of MRM allows for the separation of peaks from six structurally similar compounds, enabling simultaneous qualitative and quantitative analysis.

Diosgenin is a component that has recently been reported to have not only nourishing and strengthening effects but also improvements in Alzheimer's disease and enhancements in motor function, making it a focus of attention. Natural diosgenin primarily exists as glycosides, and is abundantly found in foods such as yam. In this case, qualitative analysis of yam extract was performed using LC/MS, confirming multiple diosgenin glycosides. Additionally, by hydrolyzing the glycosides to unify them into aglycones (non-glycosides), quantitative analysis of diosgenin also becomes possible.

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).

The main component of green tea, catechins, is known to have functions such as antioxidant effects, promoting fat burning, and lowering blood cholesterol levels, and it is designated as a specific health use food (Tokuho). Natural green tea contains four types of catechins (EC, EGC, ECG, EGCG), but commercially available tea also contains a significant amount of heat-isomerized catechins (C, GC, CG, GCG) produced during the heating sterilization process. This document presents a case study of analyzing commercially available green tea using LC/MS/MS to separate and identify eight types of catechins, including heat-isomerized forms.

In MST, qualitative and quantitative analysis of tea catechins can be performed using LC/MS/MS. This document observed the changes in EGCG concentration based on the temperature and time of brewing tea (Figure 1). It was found that the higher the temperature, the greater the extraction efficiency of EGCG, with a significant amount extracted up to 5 minutes. Additionally, a comparison of the catechin content in six commercially available tea products confirmed that green tea contains more catechins than black tea or oolong tea (Figure 2). Benifuki green tea contains a high amount of methylated catechin (ECCG3"Me), which has strong anti-allergic effects against conditions such as hay fever.

TBHQ (tert-Butylhydroquinone) is a compound used as an antioxidant in foods in countries such as the United States and China. However, in Japan, the import and sale of foods containing TBHQ is not permitted. As a result, imported foods may contain TBHQ, and if detected domestically, measures such as voluntary recalls are taken. This document presents examples of adding 0.1 ppm of TBHQ to various foods and measuring it using LC/MS/MS. In all cases, TBHQ was analyzed with a recovery rate of over 80%. We hope this will help ensure the safety and security of imported foods and raw materials.

Emulsions are dispersion systems in which water-soluble and fat-soluble components are mixed without separation due to the action of emulsifiers, and various emulsion technologies are widely used in processed foods. Mayonnaise is a representative processed food of the O/W type (oil-in-water emulsion). As a result of evaluation using cryo FIB-SEM observation, we were able to visualize the distribution of water, oil, emulsifiers, and other components. By conducting magnified observations, we can evaluate the fine structure, which is expected to be applied to sensory evaluations such as the smoothness and flavor of food.

The OPA post-column method is a technique that reacts amino acids with the fluorescent reagent OPA after separation in a column and detects the fluorescence (Figures 1, 2). This method allows for high-sensitivity analysis compared to the ninhydrin method. The fluorescent reagent OPA selectively reacts with primary amines, making it less susceptible to interference from contaminants and enabling highly selective analysis. Proline is a secondary amino acid, but it can be converted into a primary amine by adding sodium hypochlorite to the reaction solution, allowing for measurement. This document presents a case study of simultaneous measurement of 17 amino acid components, including proline (Figure 3).

This document presents a case study of the quantitative analysis of free amino acids contained in alcoholic beverages using the OPA post-column method. It was found that sake, a brewed alcoholic beverage, contains a rich and well-balanced variety of free amino acids, including alanine and arginine. Furthermore, when comparing three sake products, differences were observed in both the content and balance of free amino acids. Although draft beer is also a brewed beverage like sake, it showed a lower content of free amino acids compared to sake. On the other hand, distilled spirits such as whiskey and awamori contained almost none.

In recent years, with the increase in health consciousness, various health foods have been attracting attention. One of these, Du Zhong tea, is suitable for individuals with high blood pressure and is designated as a Food for Specified Health Uses (Tokubetsu Hōshō). In this case study, Du Zhong tea was analyzed using LC/MS/MS, and five polyphenols were detected: geniposidic acid, chlorogenic acid, asperuloside, p-coumaric acid, and quercetin. Among these components, geniposidic acid, one of the glycosides from Du Zhong leaves, serves as a benchmark for the effective ingredient of Foods for Specified Health Uses.

Ergothioneine is an amino acid homolog discovered in ergot, known for its strong antioxidant properties and anti-photoaging effects, and research and development are ongoing in the fields of medicine and beauty. Since humans cannot produce ergothioneine in their bodies, they obtain it from sources rich in it, such as certain mushrooms. An analysis of eight types of mushrooms using LC/MS/MS revealed that ergothioneine was detected in all of them. Quantitative analysis was conducted on three types of mushrooms from the Pleurotaceae family, which are said to have high ergothioneine content.

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.

In 2002, it was announced that acrylamide, which may have carcinogenic properties, is generated when foods high in carbohydrates are heated at temperatures above 120°C (Figure 1), attracting attention. According to the Ministry of Agriculture, Forestry and Fisheries (MAFF) website, acrylamide is found in many foods, including fried potato snacks, toast, and coffee. At MST, we participate in the proficiency testing FAPAS and confirm that the absolute value of the z-score is 2 or below (satisfactory), allowing us to accurately quantify acrylamide in food using LC/MS/MS.

Water-soluble vitamins can be divided into about 10 types based on their functions in the body. For example, vitamin B1 consists of multiple components (thiamine, hydroxymethylthiazole, and its derivatives) that have the same function, and the total amount of these components determines the content. In this case, a multivitamin supplement was measured using LC/MS/MS, and qualitative analysis was conducted for each component of five types of water-soluble vitamins. By performing simultaneous analysis, it is possible to efficiently confirm the presence or absence of the target components. Analysis of other water-soluble vitamins is also possible, so please feel free to inquire.

Foods such as pork and eggs are rich in vitamin B1 (thiamine, HET) and vitamin B2 (riboflavin). These are often present as derivatives such as phosphate esters. The content of vitamin B1 and vitamin B2 can be quantified by performing enzymatic treatment as a pretreatment to convert them to their free forms, followed by analysis using HPLC with a fluorescence detector. Although vitamin B1 itself is not fluorescent, it is possible to detect fluorescence by reacting it with a red blood salt alkaline solution in a post-column method, converting it to the oxidized form of thiocrome.

When an unusual odor arises from food, it is important to identify the components that cause it. In foods containing various odor components, trace elements can significantly contribute to the overall smell, and the balance of component quantities can lead to substantial differences in odor. Therefore, it is necessary to narrow down the candidate components by comparing the odorous product with a normal product. Here, we present a case study that compares new olive oil and old olive oil using GC/MS to analyze the odor components responsible for the unusual smell.

To observe the structure of liquid samples, it is necessary to conduct a series of analyses while maintaining the original structure of the sample. In cryo-SEM, the sample can be observed by rapidly freezing it to create a cross-section. Furthermore, by combining this with cross-section fabrication techniques using FIB processing, it is possible to obtain more detailed information about the internal structure.

The vitamin C contained in food refers to the total amount of reduced L-ascorbic acid and oxidized dehydroascorbic acid. Its applications include not only nutritional enhancement but also use as an antioxidant. When measuring vitamin C using HPLC, it is common to convert the oxidized form after noting that dehydroascorbic acid has no UV absorption, and then derivatize it for measurement. By quantifying dehydroascorbic acid using LC/MS/MS, it becomes possible to simplify the pretreatment and analyze with high sensitivity.

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.

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.

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.

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.

PET bottles allow a small amount of air (oxygen) to permeate, making the beverages inside susceptible to the effects of oxygen intrusion from the outside, which leads to a deterioration in quality. To address this, various innovations have been made in PET bottles. For example, by inserting an oxygen-absorbing layer between the PET layers, as shown in Figure 1, the deterioration of beverages is prevented, preserving their taste. This document presents the results of analyses conducted using TOF-SIMS to confirm what the oxygen-absorbing layer is composed of.

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.

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.

Organic acids such as citric acid and malic acid are widely used in various fields, including the semiconductor industry as additives in etching and plating solutions, as well as in food as sour agents and emulsifying stabilizers. In particular, the concentration of organic acids in plating solutions changes over time during use, and this balance affects the quality of the plating, making precise control important. Here, we will introduce a case study of organic acid analysis using IC (ion chromatography).

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.

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.

Food wrap films may use additives to ensure stability against thermal exposure during the manufacturing process and to impart plasticity. These additives are required to remain stable under cooking conditions without changing. In this case, we present the results of an investigation using TOF-SIMS to examine whether the state of one of the additives, Irgafos168, changes (bleeds out) before and after heating. *GCIB: Gas Cluster Ion Beam

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.

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.

Aluminum foil is produced by rolling two sheets together, where the outer side in contact with the rollers has a glossy surface, while the inner side, where the aluminum sheets touch each other, has a matte surface. We compared the components present on the extreme surfaces of each side. Common organic secondary pollutants such as PDMS (polydimethylsiloxane), BHT (antioxidant), DOP (plasticizer), amines (m/z 182, 242), amides (m/z 256, 284), and carboxylic acids (m/z 255, 283) were not observed. There was a slight tendency for Fe and organic materials (such as hydrocarbons) to be stronger on the glossy side, while substances like SO4 showed a slightly stronger tendency on the matte side.

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.

The large-scale pet food recall incident in 2007 and the melamine-contaminated milk powder incident in 2008 led to the detection of melamine in dairy products, livestock feed, and other foods, prompting nationwide measures to address the issue. MST has established a method for extracting and recovering melamine from food with high precision, and quantifying it using LC/MS/MS analysis. Below are the LC/MS/MS analysis results. We hope this helps alleviate your concerns about food safety.

Fucoidan is a type of high molecular weight polysaccharide that is said to have effects such as boosting immunity, anti-cancer properties, and lowering cholesterol, and it has gained attention in recent years. It is considered a type of soluble dietary fiber and is found in seaweeds such as kelp and wakame. In this method, fucoidan in supplements and drinks is analyzed by breaking it down into monosaccharides. In addition to the main component, fucose, xylose, mannose, galactose, rhamnose, and glucuronic acid are simultaneously measured to calculate the quantitative values of each sugar.

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).

Glucosylceramide is one of the glycosphingolipids found in food, and due to its moisturizing effects and improvement effects on atopic dermatitis, it has gained attention in recent years. Not only in cosmetics applied directly to the skin, but also in health foods and general foods, as well as beverages that contain glucosylceramide, many processed products are being sold. By using HPLC, it is possible to analyze the amount of glucosylceramide contained in raw crops and processed foods with high precision. Here, we will introduce an analysis case of konjac.

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.

Plastic containers, such as PET bottles used in many food products, have features like being lightweight and unbreakable; however, a challenge has been their lower gas barrier properties compared to cans and bottles. In recent years, technologies have been developed to coat PET bottles with gas barrier films to prevent quality degradation due to oxygen intrusion and carbonation loss, and these technologies are now widely used. This document presents a case study on the measurement of commercially available PET bottles, along with an evaluation of the composition and chemical bonding state of the gas barrier films.

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.