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[Analysis of Free Pantothenic Acid in Foods by HPLC and LC-MS/MS]. [HPLC - LC-MS/MS法分析食品中游离泛酸]。
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.47
Masakazu Horie, Moe Watanabe, Atsuko Tada, Kyoko Sato

A simple and reliable analytical method has been developed for the determination of pantothenic acid in food. For the high-protein food, 20 mL of water was added to 2 g of sample, and after homogenization extraction, 1 mL of 15% zinc sulfate solution was added, mixed well, centrifuged, and the supernatant was filtered to make the test solution. For the low-protein food, 20 mL of 1% formic acid solution was added to 2 g of sample, homogenized, extracted, centrifuged, and the supernatant was filtered to make the test solution. The HPLC separation was carried out on a L-column2 ODS column with 0.02 mol/L phosphate solution (pH 3.0)- acetonitrile (95 : 5) as the mobile phase, and detected at 200 nm. The LC-MS/MS conditions were L-column2 ODS as the separation column, 5 mmol/L ammonium formate (containing 0.01% formic acid)-methanol (85 : 15) as the mobile phase, and multiple reaction monitoring (MRM) was used for detection. The recoveries of pantothenic acid in milk powder and nutritional food products were more than 88% with high precision. As a result of analyzing commetrcially available foods labeled as containing pantothenic acid, analytical values almost identical to the labeled values were obtained, and a high correlation was observed between the values obtained by HPLC and LC-MS/MS.

建立了一种简便、可靠的测定食品中泛酸的分析方法。高蛋白食品,2 g样品中加入20 mL水,匀浆提取后,加入1 mL 15%硫酸锌溶液,混合均匀,离心,过滤上清制成试验溶液。对于低蛋白食品,取20 mL 1%甲酸溶液加入2 g样品中,匀浆、提取、离心,过滤上清制成试验溶液。以0.02 mol/L磷酸盐溶液(pH 3.0)-乙腈(95:5)为流动相,采用L-柱2 ODS柱进行高效液相色谱分离,在200 nm处检测。采用L-柱2 ODS为分离柱,5 mmol/L甲酸铵(含0.01%甲酸)-甲醇(85∶15)为流动相,多重反应监测(MRM)进行检测。奶粉和营养食品中泛酸的回收率可达88%以上,精密度高。通过对市售的标记为含泛酸的食品进行分析,得到的分析值与标记值几乎一致,且HPLC法与LC-MS/MS法的分析值具有高度的相关性。
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引用次数: 0
[Surveillance of the Naturally Derived Benzoic Acid Levels in Fruits and Fruit Products, and Comparison of Analytical Methods]. [水果和水果制品中天然苯甲酸含量的监测及分析方法的比较]。
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.94
Yu Shiozawa, Itoko Baba, Keiko Iwakoshi, Rina Nakamura, Yukiko Yamajima, Narue Sakamaki, Chigusa Kobayashi, Kenji Otsuka

Benzoic acid (BA) is typically found in natural food; therefore, naturally occurring BA must be distinguished from added BA preservatives. In this study, we investigated BA levels in 100 samples of fruit products and their fresh fruits as raw materials using dialysis and steam distillation approaches. BA was detected in the range (minimum-maximum) of 2.1-1380 μg/g and 2.2-1950 μg/g in dialysis and steam distillation, respectively. Steam distillation indicated higher BA levels than dialysis.

苯甲酸(BA)通常存在于天然食品中;因此,必须将天然存在的BA与添加的BA防腐剂区分开来。在本研究中,我们用透析和蒸汽蒸馏法研究了100个水果制品样品及其新鲜水果中的BA含量。在透析和蒸馏法中BA的检出范围(最小-最大)分别为2.1 ~ 1380 μg和2.2 ~ 1950 μg。蒸汽蒸馏法的BA含量高于透析法。
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引用次数: 0
[Validation of Method for Nitrite Determination in Foods]. [食品中亚硝酸盐测定方法的验证]。
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.240
Kyoko Sato, Shoko Terami, Takahiro Sasaki, Hikaru Sakurai, Akira Shimoyama, Haruko Sekido, Shoichi Tahara, Takahiko Hara, Takudo Ito, Shinji Yamamoto, Mika Yoshida, Takahiro Watanabe, Chiye Tatebe, Hiroki Kubota, Atsuko Tada

In general, nitrite in food is extracted under slightly alkaline conditions, deproteinized, and analyzed by a colorimetric method using color development by diazotization. However, depending on the sample, the sample solution may become cloudy and difficult to filter by the deproteinization treatment of the analytical method. Recently, an improved analytical method that solves these problems has been reported. Therefore, a validation study was performed on the improved analytical method was performed. The concentrations of sodium nitrite added to cod roe, fish sausage, and ham, which were not labeled with sodium nitrite, were set at the upper limits of the standards for use. We set the target values of 70-120% for trueness, less than 15% for intralaboratory reproducibility, and less than intralaboratory reproducibility for repeatability. As a result, the target values were met for the three samples verified: 88-92% for trueness, 2.0-3.0% for repeatability, and 3.2-4.3% for intralaboratory reproducibility. In addition, an interlaboratory study was conducted by eight institutes on the improved analytical method for nitrite. At each institution, sodium nitrite was added to the same three samples as in the validation study, at concentrations equivalent to twice the lower limit of quantification and the upper limit of the standards for use and analyzed in triplicate. The estimated trueness from the obtained analyses ranged from 82 to 95%, the repeatability ranged from 2.3 to 5.8%, and the inter-room reproducibility ranged from 3.5 to 11%. Thus, the improved analytical method could be useful for determining nitrite in foods.

一般来说,食品中的亚硝酸盐是在微碱性条件下提取的,经过去蛋白处理后,用重氮显色的比色法进行分析。然而,根据样品的不同,样品溶液可能会变得浑浊,难以通过分析方法的去蛋白处理进行过滤。最近,有报道称一种改进的分析方法可以解决这些问题。因此,我们对改进后的分析方法进行了验证研究。在未标注亚硝酸钠的鳕鱼子、鱼香肠和火腿中添加的亚硝酸钠浓度被设定为使用标准的上限。我们将真实度的目标值设定为 70%-120%,实验室内重现性的目标值设定为小于 15%,重复性的目标值设定为小于实验室内重现性。结果,我们验证的三个样本都达到了目标值:真实度为 88-92%,重复性为 2.0-3.0%,实验室内重复性为 3.2-4.3%。此外,八个机构还对改进后的亚硝酸盐分析方法进行了实验室间研究。每个机构都在与验证研究相同的三个样品中加入亚硝酸钠,浓度相当于定量下限和使用标准上限的两倍,一式三份进行分析。分析结果的真实度估计为 82% 至 95%,重复性为 2.3% 至 5.8%,室间重现性为 3.5% 至 11%。因此,改进后的分析方法可用于测定食品中的亚硝酸盐。
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引用次数: 0
[Characteristics of Adverse events of Dietary Supplements Provided byMedical Professionals and their Application in Causality Evaluation Algorithm]. 医学专业人员提供的膳食补充剂不良事件特征及其在因果评价算法中的应用
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.13
Keizo Umegaki, Hirotomo Nakamura, Hiroshi Yamada

This study aimed to characterize the adverse events of dietary supplements provided by medical professionals and to examine whether there are challenges when applying each case to the causality evaluation algorithm. Data from 290 individual cases collected by the Tokyo Metropolitan Government in cooperation with the Tokyo Medical Association and Tokyo Pharmaceutical Association were analyzed. The causality evaluation algorithm that was used in this study was reported previously. Female patients accounted for 73% of those who experienced adverse events. Both male and female patients who had adverse events were in their 60s and 70s. Many of the participants had underlying diseases and aimed to improve their medical conditions. Furthermore, skin symptoms were the most common. Many of the supplements were made from natural substances, with an average of 7.7 ingredients in each product. More than half of the products were used for less than one month. In most cases, symptoms improved after discontinuation of the products or after the administration of medications. When each event was applied to the causality assessment algorithm, it was necessary to understand the information as follows: in cases of product discontinuation with simultaneous medications recovery was not concluding the product discontinuation, and the physician's judgement should be place as objective evidence. The algorithm was successfully applicable to cases provided by medical professionals and the evaluated results for all cases were 30% possible and 62% highly possible. The evaluated results indicate the relationship between products/ingredients and the symptom, and by adding information on the symptom and its severity, it is possible to clarify the phenomenon to be noted.

本研究旨在描述由医疗专业人员提供的膳食补充剂的不良事件,并检查在将每个案例应用于因果关系评估算法时是否存在挑战。对东京都政府与东京医学协会和东京医药协会合作收集的290个个案的数据进行了分析。本研究中使用的因果关系评价算法已在之前报道过。女性患者占出现不良事件的患者的73%。出现不良事件的男性和女性患者年龄均在六七十岁。许多参与者有潜在的疾病,他们的目标是改善他们的医疗条件。此外,皮肤症状最为常见。许多补品都是由天然物质制成的,每种产品平均含有7.7种成分。超过一半的产品使用时间不到一个月。在大多数情况下,停药或服药后症状得到改善。当将每个事件应用于因果关系评估算法时,有必要了解以下信息:在产品停药同时药物恢复的情况下,不确定产品停药,医生的判断应作为客观证据。该算法成功应用于医疗专业人员提供的病例,所有病例的评估结果均为30%可能和62%高度可能。评估结果表明产品/成分与症状之间的关系,并且通过添加有关症状及其严重程度的信息,可以澄清需要注意的现象。
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引用次数: 0
[A Simple and Rapid Analysis Method for Nonvolatile Amines via LC-MS/MS]. 非挥发性胺的LC-MS/MS快速分析方法
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.136
Yoshitsugu Okubo, Tomotada Iwamoto
In order to quickly analyze 8 types of nonvolatile amine, such as histamine, a simple analytical method was developed. A test solution was prepared only by diluting and filtering a trichloroacetic acid extract before analysis via LC-MS/MS.As a result of the additive recovery test with 11 types of food, including fresh seafood, seafood processed products, and other processed foods, all amines had an accuracy in the range of 70 to 120% with a repeatability of less than 15% RSD in 9 types of food. This confirmed the validity of the analytical method with the lower limit of quantification between 5 to 6 mg/kg.
为了快速分析组胺等8种非挥发性胺,建立了一种简便的分析方法。在LC-MS/MS分析之前,仅将三氯乙酸提取物稀释过滤制备测试溶液。对包括新鲜海鲜、海鲜加工产品和其他加工食品在内的11种食品进行添加剂回收率测试,结果表明,所有胺在9种食品中的准确度在70 - 120%之间,重复性小于15% RSD。验证了该分析方法的有效性,定量下限为5 ~ 6mg /kg。
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引用次数: 0
[Storage Stability of Nitrite in Nitrite Analysis of Meat Products]. [肉制品亚硝酸盐分析中亚硝酸盐的储存稳定性]。
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.226
Sumiyo Yamamoto, Shoichi Tahara, Etsuko Ishii, Yuko Takagi, Chigusa Kobayashi

For the analysis of nitrite ions in food, the stabilities of nitrite ions in meat products and their standard solutions were evaluated. Nitrite is easily oxidized or reduced; hence, products with standard solutions or colour retention agent must be carefully handled. To assess the stability and decreasing trend of nitrite, we examined the storage stability of standard solutions using calibration curves, the time course of nitrite in chopped meat products stored under different conditions, and the time course of nitrite in the sample solutions. Regarding calibration curves, the storage stability was determined for standard solutions that were prepared with ultrapure water at concentrations of 0.025 and 0.4 μg/mL and were stored at 5℃ for one year. The results revealed no changes in concentration of any solution over time, suggesting that no readjustments to the standard solution concentration were necessary before testing until one year after their preparation. Time course of nitrite in chopped meat products stored under different conditions showed a significant decrease in nitrite in refrigerated storage (5℃), whereas stability of nitrite was maintained for up to 1 day in frozen storage (-20℃) and for 14 days in frozen storage (-40℃). The time course of nitrite in the sample solutions showed that the quantitative values of nitrite in the extract remained unchanged within one week of extraction for the meat products tested in the study.

为了分析食品中的亚硝酸根离子,对肉制品中亚硝酸根离子及其标准溶液的稳定性进行了评估。亚硝酸盐很容易被氧化或还原,因此必须小心处理含有标准溶液或保色剂的产品。为了评估亚硝酸盐的稳定性和下降趋势,我们利用校准曲线检测了标准溶液的储存稳定性、在不同条件下储存的切碎肉制品中亚硝酸盐的时间变化以及样品溶液中亚硝酸盐的时间变化。在校准曲线方面,测定了用超纯水配制的浓度为 0.025 和 0.4 μg/mL 的标准溶液在 5℃下存放一年的稳定性。结果显示,任何溶液的浓度都没有随着时间的推移而发生变化,这表明在制备标准溶液一年后进行检测之前,无需重新调整标准溶液的浓度。在不同条件下贮存的切碎肉制品中亚硝酸盐的时间变化表明,冷藏贮存(5℃)时亚硝酸盐显著下降,而冷冻贮存(-20℃)和冷冻贮存(-40℃)14 天内亚硝酸盐保持稳定。样品溶液中亚硝酸盐的时间变化过程表明,在本研究中测试的肉制品,提取物中亚硝酸盐的定量值在提取后一周内保持不变。
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引用次数: 0
[The Validity of the Poisson Distribution to Analyze Microbial Colony Counts on Agar Plates for Food Samples]. [泊松分布分析食品样品琼脂平板上微生物菌落计数的有效性]。
IF 0.2 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.174
Hiroshi Fujikawa

Microbial colony counts of food samples in microbiological examinations are one of the most important items. The probability distributions for the colony counts per agar plate at the dilution of counting had not been intensively studied so far. Recently we analyzed the colony counts of food samples with several probability distributions using the Pearson's chi-square value by the "traditional" statistics as the index of fit [Fujikawa and Tsubaki, Food Hyg.Saf.Sc., 60, 88-95 (2019)]. As a result, the selected probability distributions depended on the samples. In this study we newly selected a probability distribution, namely a statistical model, suitable for the above data with the method of maximum likelihood from the probabilistic point of view. The Akaike's Information Criterion (AIC) was used as the index of fit. Consequently, the Poisson model were better than the negative binomial model for all of four food samples. The Poisson model was also better than the binomial for three of four microbial culture samples. With Baysian Information Criterion (BIC), the Poisson model was also better than these two models for all the samples. These results suggested that the Poisson distribution would be the best model to estimate the colony counts of food samples. The present study would be the first report on the statistical model selection for the colony counts of food samples with AIC and BIC.

食品样品微生物菌落计数是微生物检验中最重要的项目之一。到目前为止,还没有深入研究计数稀释时每个琼脂平板菌落计数的概率分布。最近,我们使用“传统”统计学的皮尔逊卡方值作为拟合指数,分析了具有几种概率分布的食品样本的菌落计数[Fjikawa和Tsubaki,food Hyg.Saf.Sc.,6088-95(2019)]。因此,所选择的概率分布取决于样本。在本研究中,我们从概率的角度,用最大似然的方法,新选择了一种适用于上述数据的概率分布,即统计模型。采用Akaike信息准则(AIC)作为拟合指标。因此,对于所有四个食品样本,泊松模型都优于负二项模型。对于四个微生物培养样品中的三个,泊松模型也优于二项式模型。在Baysian信息准则(BIC)下,泊松模型在所有样本中也优于这两个模型。这些结果表明,泊松分布将是估计食品样本菌落数的最佳模型。本研究将是第一份关于AIC和BIC食品样本菌落计数统计模型选择的报告。
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引用次数: 0
[Determination of Flubendazole and Metabolite in Livestock Products Using LC-MS/MS]. 畜产品中氟苯达唑及其代谢物的LC-MS/MS测定
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.130
Ryo Okabe, Satoru Nemoto, Mitsutoshi Aoyagi

This study proposes a method to determine flubendazole and metabolite R35475 in livestock products using tandem mass spectrometry coupled with positive ion electrospray ionization. Acetone is used to extract flubendazole and metabolite R35475 from the livestock samples. These extracts were purified using an SCX cartridge column (500 mg). Furthermore, high-performance liquid chromatography was performed on an Inertsil ODS-4 column with a gradient formed using methanol and water, both of which contain 5 mmol/L of ammonium acetate. The recovery tests using bovine muscle, fat, liver, milk, and egg fortified at the maximum residue limits of analytes or 0.005 mg/kg revealed that the trueness (n=5) of flubendazole and metabolite R35475 ranged from 89.4 to 106.4% with a repeatability rate of 1.7-7.8%.

本研究提出了一种用正离子电喷雾串联质谱法测定畜产品中氟苯达唑及其代谢物R35475的方法。用丙酮从家畜样品中提取氟苯达唑及其代谢物R35475。这些提取物用SCX柱(500 mg)纯化。在含有5 mmol/L乙酸铵的甲醇和水形成梯度的Inertsil ODS-4柱上进行高效液相色谱。以牛肌肉、脂肪、肝脏、牛奶和鸡蛋为样品,在分析物最大残留限量(0.005 mg/kg)下进行回收率试验,结果表明,氟苯达唑及其代谢物R35475的准确度(n=5)为89.4 ~ 106.4%,重复性为1.7 ~ 7.8%。
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引用次数: 0
[Validation Study on Developed Methods for Anions and Bromic Acid in Various Mineral Waters by Ion Chromatography]. [离子色谱法测定各种矿泉水中阴离子和溴酸方法的验证研究]。
IF 0.3 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.161
Hiroshi Sakuragi, Masako Suzuki, Hiroyuki Ohno

Five kinds of anions namely fluoride, chlorate, chlorite, nitrate and nitrite ions, and bromic acid were determined in various mineral waters (MWs), and the methods were validated. MWs are varying in the degree of hardness and contents of carbonate. When the five anions were measured based on the official method of tap water, the peak shape of fluoride ion in MWs with high degree of hardness was different from the standard solution, making it difficult to determine. The same phenomenon was also observed when bromic acid was measured. In order to achieve accurate determination, five-fold dilution with ultrapure water was carried out on the samples. With the additional step, the abnormal peak of both analytes was improved, and no difference in the retention times between standard and sample solutions was observed. The validation tests were performed using the developed methods with the additional diluting step, and the results of all target substances met the criteria of the guideline on analytical method validation for MW in Japan. Our results suggested that the methods we developed could be useful for the accurate determination of the anions and bromic acid in various MWs on the market.

对各种矿泉水中氟化物、氯酸盐、亚氯酸盐、硝酸盐和亚硝酸盐离子、溴酸等5种阴离子进行了测定,并对方法进行了验证。MWs的硬度和碳酸盐含量各不相同。根据自来水的官方方法测定五阴离子时,高硬度的MWs中氟离子的峰形与标准溶液不同,难以测定。测定溴酸时也观察到同样的现象。为了准确测定,样品经超纯水稀释5倍。通过增加步骤,两种分析物的异常峰得到改善,标准溶液和样品溶液的保留时间没有差异。使用开发的方法进行了验证试验,并增加了稀释步骤,所有目标物质的结果都符合日本MW分析方法验证指南的标准。结果表明,所建立的方法可用于市场上各种MWs中阴离子和溴酸的准确测定。
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引用次数: 0
[Efficacy of Bright Greenish-Yellow Fluorescence Sorting on Mycotoxin-Contaminated Nutmeg Selection and Characterization of Fungal Flora Related to Mycotoxin Production]. 【明亮绿黄色荧光分选对真菌毒素污染的肉豆蔻的效果——与真菌毒素产生相关的真菌区系的选择和鉴定】。
IF 0.2 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Pub Date : 2023-01-01 DOI: 10.3358/shokueishi.64.179
Naoki Kobayashi, Kiyoshi Okano, Yoshiko Sugita-Konishi

Spices have been known to be highly contaminated commodities with mycotoxins. The Codex Alimentarius reports that nutmeg is particularly contaminated with aflatoxins (AFs) and ochratoxin A (OTA). To eliminate contaminated commodities, visual sorting and bright greenish-yellow fluorescence (BGYF) sorting are used as low-cost technologies in production engineering. In Indonesia, nutmeg is mainly sorted by visual sorting and classified into three grades according to the Indonesian national standards, with importers further defining their own brand as imported products. In this study, we evaluate the efficacy of BGYF sorting as a further selection method to reduce AFs and OTA using the importer's own brand. Further, the level of these mycotoxins and the relationship between fungal flora and mycotoxin contamination were examined. These results showed that BGYF sorting effectively reduces AFs as well as OTA. In addition, BGYF-positive groups were infected by Aspergillus sections Flavi, Nigri, and Circumdati.

众所周知,香料是受真菌毒素高度污染的商品。食品法典委员会报告称,肉豆蔻特别受到黄曲霉毒素(AF)和赭曲霉毒素A(OTA)的污染。为了消除被污染的商品,视觉分选和亮绿黄荧光(BGYF)分选被用作生产工程中的低成本技术。在印度尼西亚,肉豆蔻主要通过视觉分类进行分类,并根据印尼国家标准分为三个等级,进口商进一步将自己的品牌定义为进口产品。在这项研究中,我们评估了BGYF分拣作为使用进口商自有品牌减少AF和OTA的进一步选择方法的功效。此外,还检测了这些真菌毒素的水平以及真菌菌群与真菌毒素污染之间的关系。这些结果表明,BGYF分选有效地减少了AF以及OTA。此外,BGYF阳性组被Flavi、Nigri和Circodati曲霉菌感染。
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引用次数: 0
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Food Hygiene and Safety Science
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