JP4150365B2 - 農薬の分析方法および分析システム - Google Patents
農薬の分析方法および分析システム Download PDFInfo
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Description
キュウリ(O,O−ジメチル−O−4−ニトロ−m−トリルホスホロチオエート(一般名:フェニトロチオン、以下、フェニトロチオンと称す。)が含まれていないことを確認済みのもの)2kgを4分割法により分割した。分割試料500gに、水250mLを加え、ミキサーにより磨砕均一化し、均一化試料750gを得た。そのうちの75g(キュウリ50g相当)を遠心分離管に入れ、さらに、フェニトロチオン濃度が10μg/mLであるフェニトロチオン/アセトン溶液1mLを加え、フェニトロチオン10μgを含むモデル試料A(フェニトロチオン含有量:0.2mg/kg)を調製した。
機器:株式会社島津製作所製GC−17AおよびQP−5000
カラム:DB−5 内径0.53mm、膜厚1.5μm、長さ15m
キャリアガス(流速):ヘリウム(15mL/分)
注入口温度:250℃
昇温条件:170℃で1分保持した後、10℃/分で210℃まで昇温
イオン化法:電子イオン化法(EI法)
イオン化電圧:70ev
イオン源温度:250℃
実施例1において、フェニトロチオン10μgを含むモデル試料Aに代えて、フェニトロチオン5μgを含むモデル試料B(フェニトロチオン含有量:0.1mg/kg)を調製した以外は、実施例1と同様に実施して、図5に示す質量(マス)クロマトグラムを得た。図5に示した質量(マス)クロマトグラムにおいて、フェニトロチオンの質量数に対応するピークのピーク面積は87159、フェニトロチオン−d6の質量数に対応するピークのピーク面積は102830であることから、実施例1で算出したフェニトロチオン−d6を基準とするフェニトロチオンの検出感度比=1.719を考慮すると、102830×1.719=176765>87159となり、モデル試料B中のフェニトロチオンは含有上限値以下であり、モデル試料Bは残留基準値を満足していると判断された。
実施例1において、フェニトロチオン10μgを含むモデル試料Aに代えて、フェニトロチオン2μgを含むモデル試料C(フェニトロチオン含有量:0.04mg/kg)を調製した以外は、実施例1と同様に実施して、図6に示す質量(マス)クロマトグラムを得た。図6に示した質量(マス)クロマトグラムにおいて、フェニトロチオンの質量数に対応するピークのピーク面積は33840、フェニトロチオン−d6の質量数に対応するピークのピーク面積は101947であることから、実施例1で算出したフェニトロチオン−d6を基準とするフェニトロチオンの検出感度比=1.719を考慮すると、101947×1.719=175247>33840となり、モデル試料C中のフェニトロチオンは含有上限値以下であり、モデル試料Cは残留基準値を満足していると判断された。
Claims (2)
- (a)含有上限値もしくは含有上限値に1以下の任意の正数を乗じた値に相当する量の安定同位体で標識された分析対象農薬と、所定量の被検試料とを混合するステップと、
(b)前記ステップ(a)で得られた安定同位体で標識された分析対象農薬を含む被検試料を抽出処理し、有機層を得るステップと、
(c)前記ステップ(b)で得られた有機層をガスクロマトグラフィー質量分析処理もしくは液体クロマトグラフィー質量分析処理するステップと、
(d)前記ステップ(c)で得られた分析結果に基づき、分析対象農薬および安定同位体で標識された分析対象農薬の質量数もしくはフラグメントに対応するピークを比較するステップとを含むことを特徴とする農薬の分析方法。 - 含有上限値もしくは含有上限値に1以下の任意の正数を乗じた値に相当する量の安定同位体で標識された分析対象農薬と、所定量の被検試料とを混合する混合手段と、
安定同位体で標識された分析対象農薬を含む被検試料を抽出処理する抽出手段と、
抽出処理して得られた有機層をガスクロマトグラフィー質量分析処理もしくは液体クロマトグラフィー質量分析処理する質量分析手段と、
質量分析手段により得られた分析結果に基づき、分析対象農薬および安定同位体で標識された分析対象農薬の質量数もしくはフラグメントに対応するピークを比較する比較手段とを備えてなることを特徴とする農薬の分析システム。
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JP2004264936A JP4150365B2 (ja) | 2004-09-13 | 2004-09-13 | 農薬の分析方法および分析システム |
CN 200510131545 CN1790011A (zh) | 2004-09-13 | 2005-09-13 | 农药的分析方法及分析系统 |
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Cited By (3)
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CN102854271A (zh) * | 2012-10-17 | 2013-01-02 | 国家烟草质量监督检验中心 | 烟草及烟草制品中三种苯氧羧酸类农药残留量的测定方法 |
CN103698463A (zh) * | 2014-01-16 | 2014-04-02 | 国家烟草质量监督检验中心 | 一种分析烟草中三种苯氧羧酸类除草剂残留量的lc-ms/ms方法 |
CN104569251A (zh) * | 2014-12-12 | 2015-04-29 | 浙江海洋学院 | 一种微量农药类环境激素混合污染水样同步检测方法 |
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EP2071950A1 (de) * | 2007-12-20 | 2009-06-24 | Bayer CropScience AG | Verfahren zur Authentizitätsprüfung von Pflanzenschutzmitteln mittels Isotopen |
JP4915623B2 (ja) * | 2008-08-19 | 2012-04-11 | 西川計測株式会社 | 化学剤検出・定量方法 |
CN101975845A (zh) * | 2010-09-21 | 2011-02-16 | 成都中医药大学 | 中药品质自动检测系统 |
CN105745534B (zh) * | 2013-10-28 | 2018-04-13 | 株式会社岛津制作所 | 使用色谱仪的多组分定量分析方法 |
CN103645079B (zh) * | 2013-12-05 | 2016-03-30 | 山东出入境检验检疫局检验检疫技术中心 | 以辣椒粉为基质的农药残留检测用标准样品的制备方法与应用 |
CN109157867B (zh) * | 2018-08-28 | 2020-12-29 | 延边大学 | 一种人参提取液中残留农药的快速消除方法 |
CN109342584A (zh) * | 2018-09-29 | 2019-02-15 | 景宁畲族自治县食品药品检验检测中心 | 一种柳叶蜡梅果实中农药残留检测方法 |
JPWO2023026330A1 (ja) * | 2021-08-23 | 2023-03-02 | ||
CN115144514A (zh) * | 2022-07-25 | 2022-10-04 | 生态环境部南京环境科学研究所 | 基于色谱-质谱联用的农用化学品残留检测分析设备及方法 |
CN116859025B (zh) * | 2023-07-18 | 2024-04-12 | 众德肥料(平原)有限公司 | 一种土壤农药残留检测方法 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102854271A (zh) * | 2012-10-17 | 2013-01-02 | 国家烟草质量监督检验中心 | 烟草及烟草制品中三种苯氧羧酸类农药残留量的测定方法 |
CN103698463A (zh) * | 2014-01-16 | 2014-04-02 | 国家烟草质量监督检验中心 | 一种分析烟草中三种苯氧羧酸类除草剂残留量的lc-ms/ms方法 |
CN104569251A (zh) * | 2014-12-12 | 2015-04-29 | 浙江海洋学院 | 一种微量农药类环境激素混合污染水样同步检测方法 |
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