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[Multiresidue analysis of organophosphorus pesticides in vegetables and fruits using dual-column GC-FPD, -NPD]. [双柱GC-FPD, -NPD法分析蔬菜水果中有机磷农药的多重残留]。
Pub Date : 2001-12-25 DOI: 10.3358/SHOKUEISHI.42.385
英二 上野, 晴美 大島, 勲 斎藤, 浩 松本
野菜・果実中の農薬残留モニタリングのための多成分分析法を検討した.極性農薬を含む63種の有機リン系農薬を対象として,アセトニトリル抽出,メスシリンダーを用いたろ過・塩析及び有機層の分取操作に加えて,GPCの農薬流出画分を2分し,それにシリカゲル及びフロリジルミニカラムを組み合わせた精製条件を確立し,多数の試料を連続してGC測定することが可能となった.GC装置には主として定量用にRtx®-OPPesticides (FPD, Pモード)を,確認用にRtx®-200 (NPD)を用いたデュアルカラム-デュアル検出器方式を採用し,1回の注入により対象としたすべての農薬の迅速な分析を可能とした.添加回収率は全農薬で 70% 以上,相対標準偏差は60種の農薬で 20% 未満,検出限界は0.5~2 ppbと良好であった.本法を用いて野菜・果実中の農薬残留モニタリングを行ったところ30検体中20検体から15種類の農薬(平均2.0種類/検体)が検出された.
研究了用于蔬菜、果实中农药残留监测的多成分分析法。以包括极性农药在内的63种有机磷农药为对象,除了进行乙腈提取、使用雌缸的过滤和盐析以及有机层的分离操作之外,还对GPC的农药流出画进行了2份。另外,还确立了有机硅和氟氧化锆的组合提纯条件,可以连续对多个样品进行GC测定。GC装置主要采用定量用Rtx®-OPPesticides (FPD, P模式),确认用Rtx®-200 (NPD)的双列-双检测器方式,通过1次的注入可以迅速分析作为对象的所有农药。所有农药的添加回收率均在70%以上,60种农药的相对标准差小于20%,检出界限为0.5 ~ 2ppb,表现良好。利用本法对蔬菜、水果中的农药残留进行了监测,在30个样品中从20个样品中检测出15种农药(平均2.0种/样品)。
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引用次数: 18
全国の行政検査結果(1998年度)を基にした食品中の防かび剤の濃度実態及び摂取量の推定 以全国行政检查结果(1998年)为基础的食品中防霉剂的浓度实态及摄取量的推测。
Pub Date : 2001-12-25 DOI: 10.3358/SHOKUEISHI.42.404
肇 石綿, 基弘 西島, 喜延 深澤
The mean concentration and daily intake of five preservatives were estimated based on the results of an analysis of 89,927 samples of food obtained in official inspections by Japanese local governments in fiscal year 1998. The mean concentration of benzoic acid was 9.5% of the allowable limit, and those of dehydroacetic acid, p-hydroxybenzoic acid, propionic acid, and sorbic acid were 1.5%, 5.7%, 1.7%, and 23.9%, respectively. Daily intake levels of these preservatives per person estimated from the concentration and daily consumption of foods were 6.23 mg, 0.0303 mg, 1.02 mg, 8.10 mg, and 25.0 mg, respectively, and assuming a body weight of 50 kg, the amounts of benzoic acid, p-hydroxybenzoic acid, and sorbic acid consumed were 2.5%, 0.2%, and 2.0% of their acceptable daily intakes, respectively. These values were similar to those obtained based on the results of the official inspections in fiscal years 1994 and 1996.
这五种防腐剂的平均浓度和每日摄入量是根据1998财政年度日本地方政府在官方检查中获得的89,927份食品样本的分析结果得出的。苯甲酸的平均浓度为允许限量的9.5%,脱氢乙酸、对羟基苯甲酸、丙酸和山梨酸的平均浓度分别为1.5%、5.7%、1.7%和23.9%。这些防腐剂的人均每日摄入量分别为6.23毫克、0.0303毫克、1.02毫克、8.10毫克和25.0毫克,假设体重为50公斤,苯甲酸、对羟基苯甲酸和山梨酸的摄入量分别为其每日可接受摄入量的2.5%、0.2%和2.0%。这些数值与根据1994和1996财政年度官方视察结果所得的数值相似。
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引用次数: 1
食用赤色40号(アルラレッドAC)及び黄色5号(サンセットイエローFCF)のアルミニウムレーキ中有機性不純物のHPLC定量用試験液調製法の検討 食用红色40号(allared AC)和黄色5号(sunset yellow FCF)铝树脂中有机性杂质的HPLC定量用试验液配制方法的讨论
Pub Date : 2001-12-25 DOI: 10.3358/SHOKUEISHI.42.379
S. Tsuji, Y. Umino, Y. Amakura, Y. Tonogai
第7版食品添加物公定書に従った食用赤色40号アルミニウムレーキ(R-40Al)中の副成色素などの有機性不純物のHPLC定量では再現性などに問題があった.これは試験液に存在する高濃度のアルミニウムが原因と考えられた.そこで,R-40Alをアンモニアアルカリ性で煮沸し,水酸化アルミニウムのコロイド状沈殿を除去した上清を試験液とする試験液調製法を開発した.本法により,再現性のある定量結果が得られ,添加回収率も改善された.また,食用黄色5号アルミニウムレーキについても適用可能であった.
根据第7版食品添加剂说明书的食用红色40号铝浆(R-40Al)中副色素等有机性杂质的HPLC定量存在再现性等问题。这被认为是测试液中存在的高浓度铝的原因。因此,开发了将R-40Al以氨碱性煮沸,除去氢氧化铝的胶体状沉淀的上清作为试验液的试验液配制法。根据本法,得到了可再现的定量结果,并改善了添加回收率。另外,还可适用于食用黄色5号铝雷基。
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引用次数: 2
食品中の2,4,6-トリ-tert-ブチルフェノール及び関連化合物の分析 食品中2,4,6-三叔丁基酚及相关化合物的分析
Pub Date : 2001-12-25 DOI: 10.3358/SHOKUEISHI.42.359
S. Nemoto, M. Omura, S. Takatsuki, K. Sasaki, M. Toyoda
An analytical method has been developed for the determination of 2,4,6-tri-tert-butylphenol (TTBP) in foods. TTBP was determined by GC/MS (SIM) after extraction from food samples using a steam distillation technique. The developed method was able to determine simultaneously 2,4-di-tert-butylphenol (2,4-DTBP), 2,6-di-tert-butylphenol (2,6-DTBP), 3,5-di-tert-butylphenol (3,5-DTBP) and 2,4-di-tert-pentylphenol (2,4-DTPP). The method was applied to analyze the residues of the 5 phenolic compounds in 101 food samples purchased from markets. TTBP was found in some samples of meat, liver and fish (muscle) at the levels of trace (tr)-0.50 ng/g, tr and tr-1.83 ng/g, respectively. 2,4-DTBP was found in some samples of vegetables, meat, liver, fish (muscle) and fish (viscera) at the levels of 1.4-10.6 ng/g, 2.7-26.4 ng/g, tr-34.2 ng/g, tr-21.6 ng/g and tr, respectively. 2,6-DTBP was found in some samples of fish (muscle) and fish (viscera) at the levels of tr-3.9 ng/g and tr, respectively. 3,5-DTBP and 2,4-DTPP were not found in any of the analyzed samples.
建立了食品中2,4,6-三叔丁基酚(TTBP)的测定方法。采用蒸汽蒸馏法从食品样品中提取TTBP,采用气相色谱/质谱法(GC/MS)测定TTBP含量。该方法可同时测定2,4-二叔丁基苯酚(2,4- dtbp)、2,6-二叔丁基苯酚(2,6- dtbp)、3,5-二叔丁基苯酚(3,5- dtbp)和2,4-二叔戊基苯酚(2,4- dtpp)。采用该方法对从市场购买的101个食物样本中5种酚类化合物的残留量进行了分析。部分肉、肝和鱼(肌肉)样品中TTBP含量分别为痕量(tr)-0.50 ng/g、tr和tr-1.83 ng/g。2,4- dtbp在部分蔬菜、肉类、肝脏、鱼(肌肉)和鱼(内脏)样品中的含量分别为1.4-10.6 ng/g、2.7-26.4 ng/g、tr-34.2 ng/g、tr-21.6 ng/g和tr。在一些鱼(肌肉)和鱼(内脏)样品中分别发现了tr-3.9 ng/g和tr水平的2,6- dtbp。在所有分析样品中均未发现3,5- dtbp和2,4- dtpp。
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引用次数: 7
ラット排泄物中でのTrp-P-1及びその代謝物の挙動 Trp-P-1及其代谢物在大鼠排泄物中的行为
Pub Date : 2001-08-25 DOI: 10.3358/SHOKUEISHI.42.220
K. Egoshi, H. Nakaoka, T. Oka, K. Abo
To study of the behavior of Trp-P-1 and its metabolites in rat feces and urine, rats were orally administered with Trp-P-1 (750, 1,500 and 2,500 micrograms/rat), and excreted Trp-P-1 was analyzed using HPLC assay and bacterial mutagenicity assay. The extraction of Trp-P-1 from urine was performed by using the chloroform extraction method, and blue rayon was used for the extraction from feces. When Trp-P-1 was added to rat feces and urine, the recoveries of Trp-P-1 were 85.9 +/- 3.9% and 91.3 +/- 3.7%, respectively. The extracts of feces and urine from rats administered with Trp-P-1 were individually fractionated by thin layer chromatography on C18 gel. The major mutagenic zone corresponding to Trp-P-1 was found at Rf 0.09 in both extracts, while the feces extract gave two additional mutagenic zones at Rf 0.15 and 0.20. More than 97% of the fecal mutagenic activity was due to unchanged Trp-P-1. In rats administered with 750 micrograms of Trp-P-1, the amount of extracted Trp-P-1 and the number of His+ colonies induced by whole excreta were 81.6 +/- 7.1 micrograms (n = 6) and (432 +/- 77) x 10(4) for feces, and 28.7 +/- 4.9 micrograms and (171 +/- 28) x 10(4) for urine. The recoveries of Trp-P-1 in the feces and urine were 10.8 +/- 0.9% and 3.8 +/- 0.7% by HPLC analysis, and 11.1 +/- 2.0% and 4.4 +/- 0.7% by mutagenicity assay respectively. The results of the two assays seemed to show similar patterns of recovery.
对Wistar类大鼠口服Trp-P-1 750、1500及2,500 μg,粪便和尿液的Trp-P-1采用HPLC及沙门氏菌Ames法,通过TLC分图进一步调查了排泄物中的代谢物。从粪便中提取Trp-P-1使用蓝蜡笔,从尿液中提取使用氯仿,两种提取方法的添加回收率粪便为85.9±3.9%,尿液为91.3±3.7%。对粪便和尿液提取物的TLC成分的变异源性进行调查发现,粪便提取物中除Trp-P-1外,还发现了2个具有变异源性的成分,而尿液提取物中没有发现。Trp-P-1 750 μg给药组的粪便和尿液的Trp-P-1量分别为81.6±7.1 μg和28.7±4.9 μg,给药量的10.8±0.9%在粪便中;3.8±0.7%在尿液中排泄,变异性试验中也得到了类似的结果。1500 μg注射组的粪便和尿液中的Trp-P-1含量和变异源性明显高于750 μg注射组。
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引用次数: 1
ラット好塩基球白血病細胞内の β-ヘキソサミニダーゼ遊離に及ぼす含窒素及びカーバメイト系農薬等の影響 对大鼠嗜盐粒细胞白血病细胞内β-己参氨酸酶游离的含氮及碳胺类农药等影响
Pub Date : 2001-08-25 DOI: 10.3358/SHOKUEISHI.42.257
之雄 田中, 修三 田口, 精作 吉田, 堀 伸二郎, 裕 高垣
12種類の含窒素農薬,14種類のカーバメイト系農薬及びその他の農薬4種類について,in vitro におけるラット好塩基球白血病細胞からの顆粒内酵素β-ヘキソサミニダーゼの遊離を指標として,即時型アレルギー反応に及ぼす影響を検討した.その結果,β-ヘキソサミニダーゼの遊離を亢進させる農薬として,含窒素農薬のビテルタノール,ピリダベンと有機スズ農薬のシヘキサチン,酸化フェンブタスズが見いだされ,また,遊離を抑制させる農薬として,含窒素農薬のプロピコナゾール,トリアジメノールとそのほかの農薬のイマザリルが見いだされた.一方,カーバメイト系農薬は遊離に対してほとんど影響を及ぼさなかった.
12种含氮农药、14种碳胺类农药及其他4种农药,以体外大鼠嗜盐粒细胞白血病细胞中游离的颗粒内酶β-己参氨酸酶为指标,研究了对即时型过敏反应的影响。结果发现,作为使游离β-己参氨酸酶亢进的农药,有含氮农药比特坦醇、吡达本和有机锡农药西己汀、三苯丁胺素。另外,作为抑制游离的农药,有:发现了含氮农药丙康唑、三聚氰胺和其他农药。而曲霉胺类农药对游离物质几乎没有影响。
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引用次数: 3
和菓子「最中」製造における微生物汚染の解析事例 日式点心“最中”制造过程中的微生物污染解析案例
Pub Date : 2001-08-25 DOI: 10.3358/SHOKUEISHI.42.262
H. Fujikawa, T. Wauke, T. Arai, S. Sekine, S. Morozumi, Y. Naito, S. Ono, M. Shiraishi, H. Shiomi
: Food hygiene in Japanese-style confectionery factories is hard to practice because the businesses are small. In a supporting system of voluntary-based hygienic management in this field, we microbiologically investigated the production processes of "Monaka" in a workshop in Tokyo. We microbiologically assessed the processing environments as well as the products in the workshop, then proposed some improvements in the production of the confectionery. After the improvements, microbial contamination of the processing environments was reduced and no microbial contamination was found in the sugared bean, or "An" produced, though the product "Monaka" was still contaminated, especially by molds. It was clarified that the molds came from contaminated baked wheat shells, or "Kawa" and further that the wheat shells were contaminated by molds during storage.
由于企业规模小,日式糖果工厂的食品卫生很难做到。在该领域自愿卫生管理的支持系统中,我们在东京的一个车间对“Monaka”的生产过程进行了微生物学研究。我们对车间的加工环境和产品进行了微生物学评估,然后提出了一些改进糖果生产的建议。经过改进后,加工环境的微生物污染减少了,在糖豆或生产的“An”中没有发现微生物污染,但产品“Monaka”仍然受到污染,特别是霉菌。结果表明,霉菌来自被污染的烤小麦壳,或“Kawa”,并且小麦壳在储存过程中被霉菌污染。
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引用次数: 0
ドクササコ(Clitocybe acromelalga)の毒性発現機構解明のためのモデル動物の作成 为了弄清楚毒蝶子(Clitocybe acromelalga)的毒性表达机制,制作模型动物
Pub Date : 2001-06-25 DOI: 10.3358/SHOKUEISHI.42.185
Tsutomu Fukuwatari, Etsuro Sugimoto, Kazumasa Yokoyama, Katsumi Shibata
Dietary intake of a poisonous mushroom, Clitocybe acromelalga, causes acromelalgia. The symptom continues for over a month. Some papers reported that treatment with nicotinic acid is effective. We have established an animal model to elucidate the mechanism of toxicity of the poisonous mushroom Clitocybe acromelalga. Diet containing Clitocybe acromelalga was fed to niacin-deficient rats for 24 hours (designated as day 0). The food intake decreased to about one-half compared with that of day before, and body weight loss was noted. Although the diet was returned to the control diet on day 1, the food intake did not recover until day 7, and body weight gain was not seen until day 6. A severe symptom resembling acromelalgia in humans started to appear on day 3. This is the first report of an animal model for the intoxication of Clitocybe acromelalga in humans. Since no similar symptom resembling human intoxication was seen in a previous rodent study, the niacin-free/tryptophan-limited diet used in the present study may have contributed to the result.
饮食中摄入一种有毒的蘑菇,阴蒂菇,会引起肢端痛。这种症状持续了一个多月。一些论文报道用烟酸治疗是有效的。我们建立了动物模型来阐明毒蘑菇尖肢藻的毒性作用机制。以烟酸缺乏大鼠为研究对象,喂食含尖肢藻的日粮24小时(第0天),摄取量比前一天减少一半左右,体重下降。虽然在第1天饮食恢复到对照饮食,但食物摄入量直到第7天才恢复,体重直到第6天才出现增加。第3天开始出现类似人类肢端痛的严重症状。这是首次报道的动物模型中毒的阴蒂胞肢端藻在人类。由于在先前的啮齿动物研究中没有发现类似人类中毒的类似症状,因此本研究中使用的无烟酸/限制色氨酸饮食可能对结果有所贡献。
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引用次数: 9
ドクササコ(Clitocybe acromelalga)の投与がトリプトファン–ナイアシン代謝に及ぼす影響 服用毒蝶子(Clitocybe acromelalga)对色氨酸-烟酸代谢的影响
Pub Date : 2001-06-25 DOI: 10.3358/SHOKUEISHI.42.190
努 福渡, 悦郎 杉本, 克己 柴田
ドクササコにはクリチジンと4-アミノキノリン酸が含まれている.両化合物ともにトリプトファン–ナイアシン代謝経路中間体の構造類似体である.そこで、ドクササコの投与が本代謝にどのような影響を与えるのかを調べた.ドクササコを混餌により24時間投与した(投与日=Day 0).本代謝経路の代謝産物量はDay 0~Day 1,Day 1~Day 2で有意に上昇した,血液中にトリプトファン含量とNAD含量もDay 1で有意に上昇した.したがって,ドクササコの摂取によって本転換経路が阻害されることは認められず,むしろ,代謝産物を増大させる化合物の存在を示唆する結果が得られた.
毒草中含有克里替丁和4-氨基喹啉酸。两种化合物都是色氨酸-烟酸代谢途径中间体的结构类似体。因此,我们调查了毒草的注射会对人体代谢产生怎样的影响。通过混食24小时给毒草喂食(喂食日=Day 0)。本代谢途径的代谢产物量在Day 0 ~ Day 1、Day 1 ~ Day 2显著上升,血液中色氨酸含量和NAD含量也在Day 1显著上升。因此,摄取毒草并没有阻碍本转换途径,反而表明存在使代谢产物增大的化合物。
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引用次数: 3
調理用PVC製手袋使用規制後における市販弁当中のフタル酸エステル類及びアジピン酸ジ(2-エチルヘキシル)濃度 限制烹饪用PVC手套使用后,市售便当中的邻苯二甲酸酯和叠氮平酸二(2-乙基己基)浓度
Pub Date : 2001-04-25 DOI: 10.3358/SHOKUEISHI.42.128
Yukari Tsumura, Susumu Ishimitsu, Yumiko Nakamura, Kimihiko Yoshii, A. Kaihara, Yasuhide Tonogai
調理用PVC製手袋の使用が規制されて2か月経過した2000年8月に,市販弁当(いわゆるコンビニ弁当)10検体中のフタル酸エステル類 (PhE) 11種及びアジピン酸ジ(2-エチルヘキシル)(DEHA)を測定し,規制前と比較した.試験期間中の検出下限値は,フタル酸ジ(2-エチルヘキシル)(DEHP)が 14.9 ng/g,フタル酸ジn-ブチル(DBP)が 18.6 ng/g であった.市販弁当中の各PhEの濃度は,DEHPが 45~517 ng/g(平均 198 ng/g),DEHAが不検出~90 ng/g,BBP が不検出~10.0 ng/g,フタル酸ジイソノニル(DINP)は1検体のみで検出され,その濃度は 76 ng/g であった.DEHP濃度は平均で前年調査時の22分の1に減少し,その他の化合物も減少した.DBPはすべての試料で不検出であった.
在限制使用烹饪用PVC手套两个月后的2000年8月,对市售便当(即便利店便当)10个样品中的11种邻苯二甲酸酯(PhE)和叠氮平酸二(2-乙基己基)(DEHA)进行了检测,并与规定实施前进行了比较。测试期间的检测下限为邻苯二甲酸二(2-乙基己基)(DEHP) 14.9 ng/g,邻苯二甲酸二正-丁酯(DBP) 18.6 ng/g。市售便当中各PhE的浓度为DEHP 45 ~ 517ng /g(平均198ng /g), DEHA未检出~ 90ng /g, BBP未检出~ 10.0 ng/g;邻苯二甲酸二异诺酰(DINP)仅检测出1个样本,其浓度为76ng /g。DEHP浓度平均减少到上年调查时的1 / 22,其他化合物也有所减少。在所有的样品中都没有检测出DBP。
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引用次数: 12
期刊
Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)
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