{"title":"[Analytical Method for Tylosin in Livestock Products and Honey Using LC-MS/MS].","authors":"Ryo Okabe, Satoru Nemoto, Mitsutoshi Aoyagi","doi":"10.3358/shokueishi.67.1","DOIUrl":"https://doi.org/10.3358/shokueishi.67.1","url":null,"abstract":"<p><p>This study proposes a method to determine tylosin A in livestock products and tylosin A and B in honey using LC-MS/MS. The chilled samples were homogenized with a chilled mixture of ethanol and 20% (v/v) acetic acid (1 : 1, v/v),which were further cooled with ice until extraction was initiated. Acetone was used to extract analytes from the samples. These extracts were defatted using n-hexane (this step was omitted for honey) and purified with an octadecyl silylated silica gel cartridge column (Bond Elut C18).HPLC was performed on an Inertsil ODS-4 column using a gradient formed from 0.1% (v/v) formic acid in 5 mmol/L ammonium formate and 0.1% (v/v) formic acid in acetonitrile. Tylosin A and B were detected using tandem mass spectrometry with positive ion electrospray ionization. Recovery tests for tylosin A were performed in bovine muscle, fat, liver, milk, egg, and honey and those for tylosin B were performed in honey. The samples were fortified at the maximum residue limits for the analytes or at quantitative limits: 0.005 and 0.004 mg/kg for tylosin A and B, respectively. The trueness (n=5) of the analytes ranged from 83.1% to 94.9%, with the repeatability of from 0.7% to 7.1%.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 1","pages":"1-7"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147312563","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Rio Suzuki, Yu Shiozawa, Shui Watanabe, Ayako Ito, Itoko Baba, Yukiko Yamajima, Toshiko Shimoi, Narue Sakamaki, Kenji Otsuka, Maki Kanda
{"title":"[Surveillance of the Levels of Naturally Derived Benzoic Acid in Fresh Foods ②Examination of Qualitative and Quantitative Improvements Using Citrus Fruits in the Dialysis Method].","authors":"Rio Suzuki, Yu Shiozawa, Shui Watanabe, Ayako Ito, Itoko Baba, Yukiko Yamajima, Toshiko Shimoi, Narue Sakamaki, Kenji Otsuka, Maki Kanda","doi":"10.3358/shokueishi.67.109","DOIUrl":"https://doi.org/10.3358/shokueishi.67.109","url":null,"abstract":"<p><p>In analyzing the content of naturally derived benzoic acid (BA) using the dialysis method, we optimized the analytical conditions to enhance both qualitative and quantitative capabilities. The dialysis method does not involve heating operations, so it reflects the actual content of BA without the influence of such as hydrolysis. However, in LC analysis, components derived from food affect the qualitative and quantitative analysis of BA. Therefore, in this study, we examined the selection of LC columns and detectors for 36 citrus samples, which are significantly affected by interference. As a result, using the Phenyl-Hexyl column in LC-PDA measurement allowed for result determination without interference in 7 samples. For the remaining 29 samples, it was possible to determine the presence of BA using LC-MS/MS measurement with improved selectivity. One orange sample was quantified using the standard addition method to correct for matrix effects and calculate the BA content.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 3","pages":"109-113"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148413748","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"[Validation of the Patulin Analysis in Apple Juice Using the Antibiotic Analytical Method].","authors":"Shotaro Hirata, Masato Yoshimitsu","doi":"10.3358/shokueishi.67.90","DOIUrl":"https://doi.org/10.3358/shokueishi.67.90","url":null,"abstract":"<p><p>Antibiotics and mycotoxins are both substances derived from microorganisms and occasionally share similar chemical properties. Test procedures used for residual antibiotic analysis might potentially be applied to mycotoxin analysis. This study validated a method for analyzing patulin in apple juice by adapting the analytical method for the antibiotic oxytetracycline. Method validation was performed by recovery tests at 0.05 ppm to evaluate the trueness, repeatability (RSD<sub>r</sub>), and within-laboratory reproducibility (RSD<sub>wr</sub>).The validation results for clarified apple juice and cloudy apple juice exhibited sufficient recovery (91% and 86%) and precision (RSD<sub>r</sub>≦4% and RSD<sub>wr</sub>≦4%).The interfering peaks were not observed in the chromatograms of blank extracts, indicating sufficient selectivity. The limit of detection was less than 0.01 ppm in both apple juices. This method can help inspect residual patulin in apple juices.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 2","pages":"90-93"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148320614","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"[Analysis of Angelica Root Marker Constituents and Furocoumarins in a Dietary Supplement Containing Angelica gigas by Liquid Chromatograph-Mass Spectrometer with a Photodiode Array Detector].","authors":"Seiko Shimizu, Yuki Kosugi, Atsuko Suzuki, Yuuka Maruyama, Misako Takahashi, Kou Nakamura, Tomoko Urade, Toshinari Suzuki, Akiko Inomata","doi":"10.3358/shokueishi.67.120","DOIUrl":"https://doi.org/10.3358/shokueishi.67.120","url":null,"abstract":"<p><p>An analytical method to detect Angelica root constituents described in the Japanese Pharmacopoeia (scopoletin and ligustilide), Korean Pharmacopoeia (nodakenin, decursin, and decursinol angelate), Pharmacopoeia of the People's Republic of China (ferulic acid and ligustilide), and furocoumarins (psoralen, xanthotoxin, and bergapten) using liquid chromatograph-mass spectrometer with photodiode array detector was examined and applied to a dietary supplement containing Angelica Gigas Root. All target analytes were separated in reversed-phase mode using a phenylhexyl column at a column temperature of 45℃. Two detection wavelengths (250 and 340 nm) were set, and instrument detection limits (S/N ≥ 3) for all analytes were between 0.03 and 0.1 μg/mL. For confirmation of each compound, the mass spectrometer's selected ion monitoring conditions were optimized. The analytes, ferulic acid, nodakenin, psoralen, xanthotoxin, bergapten, decursin, and decursinol angelate, were detected in the dietary supplement via this analytical method.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 3","pages":"120-125"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148413760","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"[Quantitative Evaluation of Sorbic Acid Isomers in Preservative Products Used as Food Additives by Single-Reference High-Performance Liquid Chromatography].","authors":"Shohei Takada, Fuyuko Hioki, Chie Maruta, Chiye Tatebe, Hiroki Kubota, Atsuko Tada, Naoki Sugimoto","doi":"10.3358/shokueishi.67.45","DOIUrl":"10.3358/shokueishi.67.45","url":null,"abstract":"<p><p>Sorbic acid and its salts, listed as Sorbic Acid (SOA) and Potassium Sorbate (SOK) in the current Japan's Standard and Specification for Food Additives (JSFA), are widely used as food additive preservatives. In the JSFA monographs, titration is used as a quantitative method, and the SOA or SOK contents are quantified as sorbic acid or its salt, including their stereoisomers. Although sorbic acid can be converted into its stereoisomers under certain conditions, the actual isomer content in food additive products has not been accurately analyzed on the JSFA titration assay. In this study, we used a previously developed single-reference high-performance liquid chromatography (SR-HPLC) method to accurately analyze sorbic acid and its three isomers, enabling the individual quantification of these components in commercial SOA and SOK products used as food additives. Analysis of five lots of the SOA products and eight lots of the SOK products revealed that the 2E,4Z-isomer was the predominant stereoisomer, with contents ranging up to 0.011% in SOA and up to 0.15% in SOK. Thus, the stereoisomer content was extremely low compared with that of sorbic acid or potassium sorbate. The total contents of sorbic acid and the isomers in SOA or those of potassium sorbate and the isomers in SOK obtained using SR-HPLC were equivalent to those determined using the JSFA titration method. This suggests that the SR-HPLC method is a viable alternative to the titration-based quantitative method, enabling simultaneous quantification of stereoisomers in food additives. These findings demonstrate the utility of SR-HPLC as an alternative assay for regulatory and quality-control purposes, offering improved chemical specificity and stereoisomeric profiles compared with conventional titration methods.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 2","pages":"45-52"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148320552","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Real-time PCR-based Method for Estimatingthe Thermal History of Cockroach in Processed Foods, Resistant to Enzymatic DNA Degradation.","authors":"Yoko Kadota, Tomoko Kogo, Junichi Mano","doi":"10.3358/shokueishi.67.8","DOIUrl":"10.3358/shokueishi.67.8","url":null,"abstract":"<p><p>We previously developed a real-time PCR-based analytical method to evaluate the thermal history of insects (cockroaches) found in processed foods by measuring the degree of genomic DNA fragmentation. However, in this study, we identified a challenge-postmortem enzymatic DNA degradation occurs in insect bodies, making it difficult to distinguish between heat-induced DNA fragmentation and enzymatic degradation. To address this issue, we developed another approach targeting mitochondrial DNA. The new method may be able to detect DNA fragmentation caused by heating even in the model sample by immersing Periplaneta fuliginosa in curry sauce products at 25℃ for three days, showing resistance to enzymatic degradation. Additionally, considering the limitation of available body parts in practical tests, we divided the bodies of model insects into nine different parts and analyzed them. The improved method showed smaller ΔΔCq values across all body parts, suggesting that the mitochondrial DNA is less prone to enzymatic DNA fragmentation than genomic DNA. The improved method enables the detection of DNA fragmentation at temperatures exceeding 100℃, making it particularly suitable for analyzing insect contaminants in retorted food products.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 1","pages":"8-15"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147312510","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"[Validation Study on a Rapid Method for Simultaneous Determination of Pesticide Residues in Livestock Products by LC-MS/MS].","authors":"Makiko Tonohara, Yurika Awano, Akio Itoh, Masumi Waki","doi":"10.3358/shokueishi.67.126","DOIUrl":"https://doi.org/10.3358/shokueishi.67.126","url":null,"abstract":"<p><p>A simultaneous rapid test method for pesticide residues in livestock products by LC-MS/MS was developed and validation tests were conducted. For the extraction method, the QuEChERS method was applied, and samples were extracted with acetonitrile, followed by salting out and dehydration. For purification, C18 and PSA columns were used instead of GPC. Based on the validity guidelines of the Ministry of Health, Labor and Welfare, 48 pesticide residues were evaluated at 0.01 μg/g and 0.1 μg/g for cattle muscle, swine muscle and milk. The trueness of the method for 43 pesticides in all three types of food samples was 70-120%, with satisfactory repeatability and within-laboratory reproducibility. Thus, this method demonstrated the usefulness of simultaneous rapid testing for pesticide residues in livestock products.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 3","pages":"126-132"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148413859","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"[Development and Validation of an Analytical Method for the Determination of Diethylstilbestrol, Dienestrol, Hexestrol, and Their Conjugates in Bovine Muscle].","authors":"Chikako Ikegawa, Hiroko Hata, Seiichiro Iizuka, Youichi Kouno, Rie Ito, Tomoaki Tsutsumi, Hiroshi Akiyama, Shizuka Saito-Shida","doi":"10.3358/shokueishi.67.174","DOIUrl":"https://doi.org/10.3358/shokueishi.67.174","url":null,"abstract":"<p><p>A reliable and sensitive analytical method was developed for the determination of stilbenes-namely diethylstilbestrol, dienestrol, hexestrol, and their conjugates-in bovine muscle. The method involves the addition of internal standards to samples, extraction with ethanol/water (9 : 1, v/v),enzymatic hydrolysis using β-glucuronidase and aryl sulfatase, cleanup using hydrophilic-modified styrene-divinylbenzene copolymer and aminopropyl silica solid-phase extraction cartridges, and subsequent LC-MS/MS analysis. The method was validated for diethylstilbestrol, dienestrol, and hexestrol in bovine muscle spiked at 0.5 μg/kg for each analyte. The results demonstrated satisfactory analytical performance, with trueness values of 94-100%, repeatability below 5%, and within-laboratory reproducibility below 8%. No interfering peaks were observed, confirming the high selectivity of the method, and matrix effects were negligible. The developed method is applicable not only to diethylstilbestrol and its conjugates regulated in Japan but also to dienestrol and hexestrol, whose use for growth promotion in food-producing animals is prohibited in the EU. Although the conjugates of dienestrol and hexestrol were not directly validated in this study, they were presumed to be quantifiable based on their structural similarity to diethylstilbestrol conjugates.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 4","pages":"174-180"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148882316","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"[Impact of Food Safety Education and Information Sources on Female Students' Perception of Food Additives and on Product Prices with Additive-Free Labeling].","authors":"Keizo Umegaki, Chiharu Nishijima, Kaori Yokotani, Shoko Tamai, Mineko Mashimo, Katsuhiro Chosho","doi":"10.3358/shokueishi.67.31","DOIUrl":"https://doi.org/10.3358/shokueishi.67.31","url":null,"abstract":"<p><p>Food additives are essential for food preservation and quality; however, consumers often perceive them as a potential health risk. The aim of this study was to investigate how educational background and information sources affect perceptions of food additive safety among female students, and to examine the relationship between additive use and product prices. A questionnaire survey was administered to 274 junior high school students, 145 high school students, 96 university freshmen who had not attended specialized lectures, and 137 university students who had attended such lectures. Additionally, 76 pairs of commercial food products were analyzed to compare the prices between those with and without food additives. More than 80% of the respondents expressed interest in food safety, and awareness of food additives was high across all groups, particularly for sweeteners, colorants, and preservatives. Students who had attended food safety lectures were significantly more likely to perceive additives as safe. The main sources of information differed by educational background: school education was the primary source among students who had attended lectures, the internet and social media were most common among those without specialized lectures, and parents and television were the predominant sources of information for junior high and high school students. Products without additives were, on average, 1.6 times more expensive than those with additives, and no price differences were observed across additive types. These findings suggest that specialized food safety education reduces excessive concerns about food additives, whereas \"additive-free\" labeling contributes to higher product prices by enhancing their perceived value.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 1","pages":"31-39"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147312576","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"[Effect of Incubation Temperature for Tetrathionate and Rappaport-Vassiliadis Broths on Salmonella Recovery from Food Additives].","authors":"Shouhei Hirose, Atsuko Tada, Tomoko Takeda, Kyoko Sato, Maiko Watanabe, Takahiro Ohnishi, Yukiko Hara-Kudo, Naoki Sugimoto","doi":"10.3358/shokueishi.67.95","DOIUrl":"10.3358/shokueishi.67.95","url":null,"abstract":"<p><p>The microbial safety of food additives is regulated under Japan's Specifications and Standards for Food Additives (JSFA), which includes detection tests for Salmonella. The current standard procedure in JSFA requires selective enrichment of Salmonella using tetrathionate (TT) and Rappaport-Vassiliadis (RV) broths with differing incubation temperatures: 43 ± 0.2℃ for TT broth under high microbial load conditions, 35 ± 2℃ for TT broth under low bacterial load conditions, and 42 ± 0.2℃ for RV broth. These distinct incubation requirements necessitate separate temperature control, thereby increasing the complexity of laboratory procedures. In this study, we evaluated the temperature-dependent enrichment behavior of Salmonella under a limited set of conditions relevant to the JSFA method. Salmonella enterica subsp. enterica serovars Abony and Typhimurium were inoculated into food additive products in lactose broth with or without Escherichia coli at 10<sup>2</sup>, 1.3×10<sup>5</sup>, and 1.3×10<sup>6</sup> CFU/sample as a competing bacterium. The inoculated mixtures were incubated at 35 ± 1℃ for 22 hr, after which aliquots (TT: 1 mL/RV: 0.1 mL) were inoculated into TT and RV broths and incubated at 42 ± 0.2℃ and 43 ± 0.2℃ for RV broth under none/low-level E. coli co-inoculation, whereas RV broth was incubated at 42 ± 0.2℃ under high-level E. coli co-inoculation, and at 35 ± 2℃, 42 ± 0.2℃, and 43 ± 0.2℃ for TT broth. The cultures were plated on selective agar to evaluate Salmonella recovery. For TT broth, no clear differences in recovery scores were observed among 35 ± 2℃, 42 ± 0.2℃, and 43 ± 0.2℃, regardless of E. coli co-inoculation. Under none/low-level E. coli co-inoculation, recovery after RV enrichment at 42 ± 0.2℃ and 43 ± 0.2℃ was comparable. In some food additive products, colonies were not recovered on one or more selective media in some replicate experiments; however, when three selective agars were used in parallel, the incubation temperature for TT broth did not markedly affect the overall test interpretation. The recovery of S. Typhimurium on some selective agars was reduced following incubation in RV broth containing food additives, protease and isoamylase co-inoculated with E. coli at high microbial loads. This suggests that high levels of bacterial contamination in certain food additive enzyme products, including protease and isoamylase, may suppress Salmonella recovery in RV broth. Further investigation using a broader range of contaminating microorganisms and food additive types is required to validate these findings.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"67 3","pages":"95-101"},"PeriodicalIF":0.2,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148413828","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}