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  • 1
    Language: Japanese
    In: Shokuhin eiseigaku zasshi. Journal of the Food Hygienic Society of Japan, 2013, Vol.54(4), pp.259-65
    Description: The effects of processing to produce various types of tea or infusion on the levels of pesticide residues in tea were investigated for three insecticides (chlorfenapyr, pyrimiphos-methyl, and clothianidin). Tea plants were sprayed with one of the three pesticides and cultivated under cover. The levels of pesticide residues in tea decreased after processing according to the time and temperature of heating, as well as fermentation. Although significant differences were not observed among the three pesticides in the ratio of decreased of pesticide concentration after processing to green tea, clothianidin, which is a neonicotinoid insecticide and has a lower log Pow value, tended to be transferred more than the other two insecticides into infusions. However, no significant difference in the ratios of clothianidin transferred to infusions was observed among green tea with three different leaf sizes.
    Keywords: Food Handling ; Camellia Sinensis -- Chemistry ; Food Contamination -- Analysis ; Guanidines -- Analysis ; Organothiophosphorus Compounds -- Analysis ; Pesticide Residues -- Analysis ; Pyrethrins -- Analysis ; Tea -- Chemistry ; Thiazoles -- Analysis
    ISSN: 00156426
    E-ISSN: 1882-1006
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  • 2
    Language: Japanese
    In: 食品衛生学雑誌, 2014, Vol.55(2), pp.117-134
    Description: ガラス製,陶磁器製またはホウロウ引きの器具・容器包装,ならびに金属缶のカドミウム(Cd)および鉛(Pb)溶出試験における各測定法の性能を評価するため,試験室間共同試験を行った.当試験には17機関が参加し,濃度非明示の8濃度16検体についてフレーム方式原子吸光光度法(AAS),電気加熱方式原子吸光光度法(GF-AAS),誘導結合プラズマ発光強度測定法(ICP-OES)および誘導結合プラズマ質量分析法(ICP-MS)によりCdおよびPbの定量を行った.その結果,AAS,ICP-OESおよびICP-MS(内標法)では真度が93~105%,併行精度(RSD〈sub〉r〈/sub〉)が0.7~8.4%,室間再現精度(RSD〈sub〉r〈/sub〉)が2.6~19.3%であり,規格試験法として十分な性能を有していることが判明した.一方,GF-AASではいくつかの結果でRSD〈sub〉r〈/sub〉が10%を超えており,適切な精度管理が必要であった.
    Description: An interlaboratory study was performed to evaluate a migration test method of cadmium (Cd) and lead (Pb), based on the Japanese Food Sanitation Law for glassware, ceramicware, enamelware and metal cans. Seventeen laboratories participated, and quantified Cd and Pb in eight test solutions as blind duplicates using flame atomic absorption spectrometry (AAS), graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma-optical emission spectrometry (ICP-OES) or induced coupled plasma-mass spectrometry (ICP-MS). Statistical analysis revealed that the trueness, repeatability (RSD〈sub〉r〈/sub〉) and reproducibility (RSD〈sub〉r〈/sub〉) were 93–105%, 0.7–8.4% and 2.6–19.3% by using AAS, ICP-OES and ICP-MS (internal standard method). The performance of these methods is sufficient for testing specifications. However, some of the RSD〈sub〉r〈/sub〉 values exceeded 10% in GF-AAS, and careful control of accuracy is required.
    Keywords: カドミウム ; 鉛 ; 溶出試験 ; 原子吸光光度法 ; 誘導結合プラズマ発光強度測定法 ; 誘導結合プラズマ質量分析法 ; 試験室間共同試験 ; Cadmium ; Lead ; Migration Test ; Atomic Absorption Spectrometry ; Induced Coupled Plasma-Optical Emission Spectrometry ; Induced Coupled Plasma-Mass Spectrometry ; Interlaboratory Study
    ISSN: 0015-6426
    E-ISSN: 18821006
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  • 3
    Language: English
    In: Food Hygiene and Safety Science (Shokuhin Eiseigaku Zasshi), 2014, Vol.55(6), pp.269-278
    Description: Based on the Japanese Food Sanitation Law, the performances of official and alternative material test methods for cadmium (Cd) and lead (Pb) in food contact plastics were compared. Nineteen laboratories participated to an interlaboratory study, and quantified Cd and Pb in three PVC pellets. in the official method, a sample is digested with H2SO4, taken up in HCl, and evaporated to dryness on a water bath, then measured by atomic absorption spectrometry (AAS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). Statistical treatment revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 86-95%, 3.1-9.4% and 8.6-22.1%, respectively. The values of the performance parameters fulfilled the requirements , and the performances met the test specifications. The combination of evaporation to dryness on a hot plate and measurement by AAS or ICP-OES is applicable as an alternative method. However, the trueness and RSDr were inferior to those of the official method. The performance parameters obtained by using the microwave digestion method (MW method) to prepare test solution were better than those of the official method. Thus, the MW method is available as an alternative method. Induced coupled plasma-mass spectrometry (ICP-MS) is also available as an alternative method. However, it is necessary to ensure complete digestion of the sample.
    Keywords: Public Health;
    ISSN: 0015-6426
    E-ISSN: 1882-1006
    Source: CrossRef
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  • 4
    Language: English
    In: Food Hygiene and Safety Science (Shokuhin Eiseigaku Zasshi), 2015, Vol.56(3), pp.123-131
    Description: Using six kinds of zinc solution in water and 4% acetic acid as samples, an interlaboratory study was performed to evaluate a zinc (Zn) test method for food-contact rubber products, based on the Japanese Food Sanitation Law. Eighteen laboratories participated, and quantified Zn in six test solutions as blind duplicates using flame atomic absorption spectrometry, induced coupled plasma-optical emission spectrometry or induced coupled plasma-mass spectrometry. Statistical analysis revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 97-103%, 0.7-4.9% and 1.7-8.9% by all measuring methods. The values of the performance parameter fulfilled the target value (trueness: 80-110%, RSDr: 10%, RSDr: 25%). The performance of these methods is sufficient for testing the adherence of samples to the specifications.
    Keywords: Public Health;
    ISSN: 0015-6426
    E-ISSN: 1882-1006
    Source: CrossRef
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  • 5
    Language: Japanese
    In: 食品衛生学雑誌, 2016, Vol.57(5), pp.169-178
    Description: 〈p〉食品衛生法におけるポリスチレン製器具・容器包装の揮発性物質試験の性能を評価するため,ポリスチレン,アクリロニトリル・スチレン共重合樹脂,アクリロニトリル・ブタジエン・スチレン共重合樹脂のペレットを検体として試験室間共同試験を行った.当試験には21機関が参加し,3検体(各2測定)について規制対象であるスチレン,トルエン,エチルベンゼン,イソプロピルベンゼンおよびプロピルベンゼンの含有量をGC-FID,GC-MSおよびヘッドスペース(HS)-GCにより定量した.GC-FIDを用いた方法による併行精度(RSDr)は1.0~2.6%,室間再現精度(RSDr)は2.5~5.8%であり,その性能は目標値を満たしており,規格試験法として十分であった.GC-MSにおけるRSDrは1.4~7.8%,RSDrは4.9~13%,HS-GCにおけるRSDrは2.0~2.6%,RSDrは3.3~6.9%であり,それらの定量値はGC-FIDとほぼ同等であった.そのため,これらは規格試験法の代替法として適用可能であった.〈/p〉
    Description: 〈p〉Using polystyrene, acrylonitrile-styrene resin and acrylonitrile–butadiene–styrene resin pellets as samples, an interlaboratory study was performed to evaluate the volatiles test method, based on the specifications described in the Japanese Food Sanitation Law for food-contacting polystyrene products. The study was conducted with the participation of twenty-one laboratories. Each laboratory quantified the contents of styrene, toluene, ethylbenzene, isopropylbenzene and propylbenzene in three test pellets using GC-FID, GC-MS or headspace-GC-FID. Statistical analysis revealed that the repeatability (RSDr) and reproducibility (RSDr) were 1.0–2.6 and 2.5–5.5% for the GC-FID method. The values of the performance parameters fulfilled the requirements (RSDr: 10%, RSDr: 25%), and the performance is sufficient for specifications testing. The RSDr and RSDr of results obtained using the GC-MS and HS-GC methods were 1.4–7.8 and 4.9–13%(GC-MS), and 2.0–2.6 and 3.3–6.9%(HS-GC-FID), respectively. The quantified levels were similar to those obtained with GC-FID. The study suggests that the GC-MS and HS-GC methods can be employed as alternative methods to the GC-FID method.〈/p〉
    Keywords: 器具・容器包装 ; ポリスチレン ; 揮発性物質 ; エチルベンゼン ; スチレン ; ガスクロマトグラフィー ; ヘッドスペースガスクロマトグラフィー ; 試験室間共同試験 ; Food Contact Utensils And Packages ; Polystyrene ; Volatile Substance ; Ethylbenzene ; Styrene ; Gc ; Headspace Gc ; Interlaboratory Study
    ISSN: 0015-6426
    E-ISSN: 18821006
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  • 6
    Language: Japanese
    In: 食品衛生学雑誌, 2016, Vol.57(6), pp.222-229
    Description: 〈p〉食品衛生法ではナイロン製器具・容器包装からのカプロラクタムの溶出量が規制されている.そこで,公定法であるGC-FID法とその代替法であるGC-MS法の性能を評価するため,20機関で試験室間共同試験を行った.各試験機関は,濃度非明示の20%エタノール溶液(3検体,各2測定)中のカプロラクタムをGC-FIDまたはGC-MSにより定量した.公定法(GC-FIDを用いた絶対検量線による定量)における真度は96~97%,併行精度(RSDr)は3.3~5.4%,室間再現精度(RSDr)は4.0~6.7%であり,これらの値は目標値(真度:80~110%,RSDr: 10%,RSDr: 25%)を満たしていた.さらに,ヘプタラクタムを用いて内標準補正を行うといずれの性能パラメーターも向上した.GC-MS法では,絶対検量線法において一部のRSDrが目標値の10%を超えた.しかし,内標準補正を行うと真度は94~96%,RSDrは2.0~4.4%,RSDrは7.0~9.4%であり,規格試験法の代替法として適用可能であった.〈/p〉
    Description: 〈p〉The Japanese Food Sanitation Law sets a limit on the migration level of caprolactam for food-contacting nylon products. Here, we carried out an interlaboratory study in twenty laboratories to evaluate the performance of the official GC-FID test method and a GC-MS method as an alternative test method to the official method. Each laboratory quantified caprolactam in three test solutions in 20% ethanol as blind duplicates using GC-FID or GC-MS. The official method (GC-FID with absolute calibration) gave trueness, repeatability (RSDr) and reproducibility (RSDr) values of 96–97%, 3.3–5.4% and 4.0–6.7%, respectively. These values met the target criteria (trueness: 80–110%, RSDr: 10%, RSDr: 25%). The performance of the method was further improved by the introduction of heptalactam as an internal standard. As for GC-MS method, some values of the RSDr exceeded 10% when absolute calibration was used. However, when an internal standard was introduced, the trueness, RSDr and RSDr of GC-MS method were all acceptable at 94–96%, 2.0–4.4% and 7.0–9.4%, respectively. Therefore, GC-MS with an internal standard is available as an alternative test method to the official method.〈/p〉
    Keywords: ナイロン ; カプロラクタム ; ガスクロマトグラフ水素炎イオン化検出器 ; ガスクロマトグラフ質量分析計 ; 試験室間共同試験 ; Nylon ; Caprolactam ; Gc-Fid ; Gc-Ms ; Interlaboratory Study
    ISSN: 0015-6426
    E-ISSN: 18821006
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  • 7
    Language: Japanese
    In: 食品衛生学雑誌, 2015, Vol.56(2), pp.57-67
    Description: ポリエチレンテレフタレート製器具・容器包装のアンチモン(Sb)およびゲルマニウム(Ge)溶出試験における各測定法の性能を評価するため,試験室間共同試験を行った.当試験には18機関が参加し,濃度非明示の3検体(各2測定)について電気加熱方式原子吸光光度法(GF-AAS),誘導結合プラズマ発光強度測定法(ICP-OES)および誘導結合プラズマ質量分析法(ICP-MS)によりSbおよびGeの定量を行った.その結果,GF-AASおよびICP-OESでは,真度が98~107%,併行精度(RSDr)が1.7~7.5%,室間再現精度(RSDr)が2.0~18.8%であり,これらの性能は規格試験法として十分であった.また,ICP-MSでは,真度が99~106%,RSDrが0.7~2.2%,RSDrが2.2~10.5%であり,代替法として適用可能であった.しかし,一部の試験機関ではSbの定量値が添加量よりも高かった.その一因として,検量線溶液中のSbがガラス器具に吸着したためと考えられた.そのため,Sbの試験を行う場合には,検量線溶液の濃度について細心の注意を払う必要があると考えられた.
    Description: An interlaboratory study was performed to evaluate a migration test method of antimony (Sb) and germanium (Ge), based on the Japanese Food Sanitation Law for food- contact polyethylene terephthalate. Eighteen laboratories participated, and quantified Sb and Ge in three test solutions as blind duplicates using graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma-optical emission spectrometry (ICP-OES) or induced coupled plasma-mass spectrometry (ICP-MS). Statistical analysis revealed that the trueness, repeatability and reproducibility were 98–107%, 1.7–7.5% and 2.0–18.8% by using GF-AAS and ICP-OES. The performance of these methods is sufficient for testing the specifications. The performance parameters of ICP-MS were 99–106%, 0.7–2.2% and 2.2–10.5%, respectively. ICP-MS is available as an alternative measuring method. However, in some laboratories, the quantitative values of Sb were higher than the addition levels. We found that Sb in working solutions is absorbed on glass vessels. Careful control of concentration in working solutions is required for Sb analysis.
    Keywords: アンチモン ; ゲルマニウム ; 溶出試験 ; 原子吸光光度法 ; 誘導結合プラズマ発光強度測定法 ; 誘導結合プラズマ質量分析法 ; 試験室間共同試験 ; Antimony ; Germanium ; Migration Test ; Atomic Absorption Spectrometry ; Induced Coupled Plasmaoptical Emission Spectrometry ; Induced Coupled Plasma-Mass Spectrometry ; Interlaboratory Study
    ISSN: 0015-6426
    E-ISSN: 18821006
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  • 8
    Language: Japanese
    In: 食品衛生学雑誌, 2013, Vol.54(4), pp.259-265
    Description: 3種の殺虫剤クロルフェナピル,ピリミホスメチルおよびクロチアニジンをチャに散布して被覆下で栽培し,摘採後の茶の加工工程および熱湯浸出時における農薬の消長を調査した.生茶葉に加熱や発酵などの加工工程が入ることで,加工茶における農薬残存率は減少したが,加熱時間や発酵時間が長く,熱が茶葉へ伝わりやすいほど減少した.また,普通煎茶において3農薬の農薬残存率に有意差は認められなかったが,ネオニコチノイド系のクロチアニジンのように,オクタノール/水分配係数が低く水溶性の高い農薬ほど,茶浸出液への移行率が高くなる傾向が見られた.一方,粒度による農薬移行率に有意な差は認められなかった.
    Description: The effects of processing to produce various types of tea or infusion on the levels of pesticide residues in tea were investigated for three insecticides (chlorfenapyr, pyrimiphos-methyl, and clothianidin). Tea plants were sprayed with one of the three pesticides and cultivated under cover. The levels of pesticide residues in tea decreased after processing according to the time and temperature of heating, as well as fermentation. Although significant differences were not observed among the three pesticides in the ratio of decreased of pesticide concentration after processing to green tea, clothianidin, which is a neonicotinoid insecticide and has a lower log 〈i〉P〈/i〉〈sub〉ow〈/sub〉 value, tended to be transferred more than the other two insecticides into infusions. However, no significant difference in the ratios of clothianidin transferred to infusions was observed among green tea with three different leaf sizes.
    Keywords: 残留農薬 ; クロルフェナピル ; ピリミホスメチル ; クロチアニジン ; 生茶葉 ; 加工茶 ; 茶浸出液 ; オクタノール/水分配係数 ; Pesticide Residue ; Chlorfenapyr ; Pyrimiphos-Methyl ; Clothianidin ; Raw Tea Leaves ; Processed Tea ; Tea Infusion ; Octanol&Amp;Ndash;Water Partition Coefficient (Log Pow)
    ISSN: 0015-6426
    E-ISSN: 18821006
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  • 9
    Language: Japanese
    In: 食品衛生学雑誌, 2015, Vol.56(3), pp.123-131
    Description: 食品衛生法におけるゴム製器具・容器包装の亜鉛(Zn)試験法の性能を評価するため,水または4%酢酸による亜鉛溶液6種を検体として用いた試験室間共同試験を行った.当試験には18機関が参加し,濃度非明示の6検体(各2測定)についてフレーム方式原子吸光光度法,誘導結合プラズマ発光強度測定法および誘導結合プラズマ質量分析法によりZnの定量を行った.その結果,いずれの測定法においても真度が97~103%,併行精度(RSDr)が0.7~4.9%,室間再現精度(RSDr)が1.7~8.9%であり,性能パラメーターの値は目標値(真度:80~110%,RSDr:10%以下,RSDr:25%以下)を満たしており,規格試験法として十分な性能を有していることが判明した.
    Description: Using six kinds of zinc solution in water and 4% acetic acid as samples, an interlaboratory study was performed to evaluate a zinc (Zn) test method for food-contact rubber products, based on the Japanese Food Sanitation Law. Eighteen laboratories participated, and quantified Zn in six test solutions as blind duplicates using flame atomic absorption spectrometry, induced coupled plasma-optical emission spectrometry or induced coupled plasma-mass spectrometry. Statistical analysis revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 97–103%, 0.7–4.9% and 1.7–8.9% by all measuring methods. The values of the performance parameter fulfilled the target value (trueness: 80–110%, RSDr: 10%, RSDr: 25%). The performance of these methods is sufficient for testing the adherence of samples to the specifications.
    Keywords: 亜鉛 ; 溶出試験 ; 原子吸光光度法 ; 誘導結合プラズマ発光強度測定法 ; 誘導結合プラズマ質量分析法 ; 試験室間共同試験 ; Zinc ; Migration Test ; Atomic Absorption Spectrometry ; Induced Coupled Plasma-Optical Emission Spectrometry ; Induced Coupled Plasma-Mass Spectrometry ; Interlaboratory Study
    ISSN: 0015-6426
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  • 10
    Language: Japanese
    In: 食品衛生学雑誌, 2014, Vol.55(6), pp.269-278
    Description: 食品衛生法における合成樹脂製器具・容器包装のカドミウム(Cd)および鉛(Pb)材質試験について,公定法と各種代替法の性能を比較した.19機関が試験室間共同試験に参加し,3種のポリ塩化ビニル製ペレット中のCdおよびPbを定量した.公定法は,試料を灰化後,塩酸に溶解した溶液を水浴上で蒸発乾固し,原子吸光光度法(AAS)または誘導結合プラズマ発光強度測定法(ICP-OES)で測定する.その真度は86~95%,併行精度(RSDr)は3.1~9.4%,室間再現精度(RSDr)は8.6~22.1%であり,その性能は規格試験法として十分であった.ホットプレート上で蒸発乾固しAASおよびICP-OESで測定する方法は,公定法よりも真度とRSDrが劣っていたが,代替法として適用可能である.マイクロウェーブ分解法(MW法)による試験溶液の調製は公定法よりも性能がよく,代替法として十分に適用可能である.また,誘導結合プラズマ質量分析(ICP-MS)法は測定法の代替法として適用可能であるが,試料を完全に灰化する必要がある.
    Description: Based on the Japanese Food Sanitation Law, the performances of official and alternative material test methods for cadmium (Cd) and lead (Pb) in food contact plastics were compared. Nineteen laboratories participated to an interlaboratory study, and quantified Cd and Pb in three PVC pellets. in the official method, a sample is digested with H2SO4, taken up in HCl, and evaporated to dryness on a water bath, then measured by atomic absorption spectrometry (AAS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). Statistical treatment revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 86–95%, 3.1–9.4% and 8.6–22.1%, respectively. The values of the performance parameters fulfilled the requirements , and the performances met the test specifications. The combination of evaporation to dryness on a hot plate and measurement by AAS or ICP-OES is applicable as an alternative method. However, the trueness and RSDr were inferior to those of the official method. The performance parameters obtained by using the microwave digestion method (MW method) to prepare test solution were better than those of the official method. Thus, the MW method is available as an alternative method. Induced coupled plasma-mass spectrometry (ICP-MS) is also available as an alternative method. However, it is necessary to ensure complete digestion of the sample.
    Keywords: カドミウム ; 鉛 ; 合成樹脂製器具・容器包装 ; 材質試験 ; 試験室間共同試験 ; Cadmium ; Lead ; Food Contact Synthetic Resin ; Material Test ; Interlaboratory Study
    ISSN: 0015-6426
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