JP2019015728A - 分析試料調製のための器具 - Google Patents
分析試料調製のための器具 Download PDFInfo
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- JP2019015728A JP2019015728A JP2018128268A JP2018128268A JP2019015728A JP 2019015728 A JP2019015728 A JP 2019015728A JP 2018128268 A JP2018128268 A JP 2018128268A JP 2018128268 A JP2018128268 A JP 2018128268A JP 2019015728 A JP2019015728 A JP 2019015728A
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- 229920003176 water-insoluble polymer Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Abstract
Description
本出願は、本出願と同時に出願された出願第______号、Rapid Sample Preparation for Analytical Analysis Using Dispersive Energized Extraction、及び本出願と同時に出願された出願第______号、Rapid Energized Dispersive Solid Phase Extraction(SPE)for Analytical Analysisに関連する。
抽出溶媒及び試料マトリックスは、チャンバ42内の試料カップ45内で混合される。本器具の利点は、密に充填された試料とは対照的に緩い試料で抽出を行う能力である。「緩い」という用語が相対的であるが、この用語は、拘束もしくは抑制するものがなく、かつ締結もしくは付着なしまたはそれから解放されたものとして、その通常の意味で、本明細書で使用される(Urdang,The Random House College Dictionary,Random House Inc.(1972))。試料マトリックスが緩いため、上部、底部、またはこれらの両方からの溶媒の添加は、試料マトリックスを溶媒中に分散させる助けとなる。
す。加えて、保持時間10.36でのASEピーク(2−メチルナフタレン)の不在は、ASEがこの分析物を特定することができなかったことを実証する。
1.10〜15gの均質化試料を50mLの遠心分離管に移す。
2.試料15g当たり、15mLのアセトニトリル中1%酢酸及び酢酸管の内容物を添加する。
3.1分間活発に振盪する。
4.1500U/分超で1分間遠心分離する。
1.1mLのアセトニトリル層を2mLのdSPE管に移す。
2.1分間活発に振盪する。
3.1500U/分超で1分間遠心分離する。
4.上清を同時GCMS分析のためにGCバイアルに移す。
1.均質化食品試料を試料カップに移し、dSPE吸着剤を添加する。
2.試料カップを加熱耐圧チャンバ内に設置する。
3.耐圧チャンバ内の試料カップを5分間加熱する。
4.抽出物を同時GC−MS分析のためにGCバイアルに移す。
Claims (28)
- 溶媒抽出のための組み合わせであって、
加熱圧力密閉反応チャンバと、
前記反応チャンバ内の熱伝導性試料カップであって、前記反応槽が、1つの開放濾過端及び前記開放濾過端と反対側の口部を含む、前記熱伝導性試料カップと、
前記試料カップ内の抽出試料と、
前記試料カップの内部及び前記試料カップの外側と前記反応チャンバの内側との間の前記試料カップの外部の抽出溶媒と、を備える、前記組み合わせ。 - 前記反応チャンバが、熱伝導材料から形成される、請求項1に記載の組み合わせ。
- 前記開放濾過端が、小孔フロア及び小孔フロア上の濾過媒体である、請求項1に記載の組み合わせ。
- 前記濾過媒体が、濾紙、ガラス繊維、石英繊維、不織ポリマー、及びそれらの組み合わせからなる群から選択される、請求項3に記載の組み合わせ。
- 前記抽出試料が、土壌、プラスチック、加工食品、食品包装、農産物、及びそれらの混合物からなる群から選択される、請求項1に記載の組み合わせ。
- 前記抽出溶媒が、水、弱酸、弱塩基、酢酸エチル、メチル第三ブチルエーテル(「MTBE」)、塩化メチレン、ヘキサン、アセトン、ヘキサン、2−プロパノール、シクロヘキサン、アセトニトリル、メタノール、及びそれらの混合物からなる群から選択される、請求項1に記載の組み合わせ。
- 抽出に基づく分子試料調製及び関連プロセスのための器具であって、
熱伝導耐圧加熱チャンバと、
前記熱伝導耐圧加熱チャンバ内に位置付けられた熱伝導試料カップであって、前記熱伝導試料カップ内の液体及び固体を一緒に加熱するための、前記熱伝導試料カップと、
供給物から前記熱伝導耐圧加熱チャンバ内の前記熱伝導試料カップに液体を送達するための、前記熱伝導耐圧加熱チャンバ内の液体送達入口取付具と、
前記チャンバが大気圧に開放されているときに前記熱伝導耐圧加熱チャンバから加熱液体を受容するための、前記熱伝導耐圧加熱チャンバ内の前記熱伝導試料カップと液体連通したチラーと、を備える、前記器具。 - 前記耐圧加熱チャンバが、供給物から前記熱伝導試料カップ及び前記反応チャンバに不活性ガスを送達して、前記加熱チャンバ及び前記試料カップ内の圧力を増加させるための、前記熱伝導試料カップの上部または上部付近に位置付けられた前記熱伝導耐圧加熱チャンバ内のガス送達入口取付具をさらに備える、請求項7に記載の分子試料調製器具。
- 超音波発生器が、前記試料カップ内で材料の二次撹拌を行うために前記熱伝導耐圧加熱チャンバと連通する、請求項7に記載の分子試料調製器具。
- 前記超音波発生器が、圧電変換器である、請求項7に記載の分子試料調製器具。
- 前記チラーが、前記ドレインと液体連通した冷却コイルを備え、前記冷却コイルが、共通抽出溶媒が前記冷却コイルの長さを移動するときに前記溶媒の温度を約50℃〜180℃から約25℃〜40℃まで低下させるのに十分な前記長さを有する、請求項7に記載の分子試料調製器具。
- 前記耐圧加熱チャンバが、耐圧チャンバクロージャをさらに備える、請求項7に記載の分子試料調製器具。
- 供給物から前記熱伝導試料カップに不活性ガスを送達して、前記熱伝導試料カップの内容物を撹拌するための、前記熱伝導試料カップの底部または底部付近に位置付けられた前記熱伝導耐圧加熱チャンバ内のガス送達入口取付具をさらに備える、請求項7に記載の分子試料調製器具。
- 抽出に基づく分子試料調製及び関連プロセスのための器具であって、
共通ラック内に担持された複数の試料カップ及び複数の収集バイアルと、
前記試料カップのうちの1つを前記ラックと開放圧力チャンバとの間で移動させるためのロボットアームと、
垂直に往復して前記圧力チャンバを開閉する耐圧チャンバクロージャと、
前記圧力チャンバが閉鎖されているときに液体を前記圧力チャンバに送達するための液体入口取付具と、
前記圧力チャンバが閉鎖されているときに前記圧力チャンバ内の液体の温度を上昇させるための加熱器と、
前記圧力チャンバが閉鎖されているときに撹拌ガス流を前記圧力チャンバに送達するためのガス入口取付具と、
前記チャンバ内の送達された加熱液体により発生した圧力下で液体を前記圧力チャンバから放出するためのドレインと、を備える、前記器具。 - 前記ドレインと液体連通した冷却コイルをさらに備え、前記冷却コイルが、共通抽出溶媒が前記冷却コイルの長さを移動するときに前記溶媒の温度を約50℃〜180℃から約25℃〜40℃まで低下させるのに十分な前記長さを有する、請求項14に記載の抽出に基づく分子試料調製器具。
- 前記ロボットアーム上の液体送達栓と、
前記栓から前記収集バイアルのうちの1つに冷却液体を送達するための、前記冷却コイルと前記栓との間の管と、をさらに備える、請求項14に記載の抽出に基づく分子試料調製器具。 - 前記加熱圧力チャンバから前記冷却コイル内に溶媒を排出するための、前記加熱圧力チャンバと前記冷却コイルとの間の第1の弁をさらに備える、請求項15に記載の抽出に基づく分子試料調製器具。
- 前記熱伝導チャンバ内の加熱溶媒の蒸気圧が液体溶媒を前記冷却コイル内に押し込むように、前記冷却コイルの末端に第2の弁をさらに備える、請求項17に記載の抽出に基づく分子試料調製器具。
- 前記圧力チャンバが閉鎖及び加熱されているときに前記圧力チャンバ内の前記試料カップの底部または底部付近の位置に撹拌ガス流を送達するためのガス取付具をさらに備える、請求項14に記載の抽出に基づく分子試料調製器具。
- 前記試料カップの内容物を撹拌するための、前記チャンバに隣接して位置付けられた超音波発生器をさらに備える、請求項14に記載の抽出に基づく分子試料調製器具。
- 前記超音波発生器が、圧電変換器を備える、請求項20に記載の抽出に基づく分子試料調製器具。
- 前記超音波発生器が、圧電変換器と、前記変換器を前記圧力チャンバの壁に接続するロッドと、を備える、請求項20に記載の抽出に基づく分子試料調製器具。
- 抽出関連技法に特に好適な試料調製器具であって、前記器具が、
1つの開放濾過端及び前記濾過端と反対側の口部を有する試料カップと、
前記試料カップを包囲する反応チャンバであって、前記反応チャンバ及び前記試料カップが、前記反応チャンバの内面と前記試料カップの外面との間に開放ジャケット部分を画定し、前記反応チャンバが、
前記試料カップの前記開放濾過端と連通したドレインフロアと、
前記試料カップの前記口部上の圧力密閉蓋と、
前記圧力密閉蓋から前記試料カップの内側への第1の溶媒入口と、
前記ドレインフロアから前記反応チャンバ内への第2の溶媒入口と、を含む、前記反応チャンバと、
前記反応チャンバと熱接触した反応チャンバ加熱器と、を備え、
これにより、溶媒が、前記第1の溶媒入口及び前記第2の溶媒入口の両方から前記試料カップ内に、かつ前記第2の溶媒入口から前記ジャケット部分内に添加され得ることになり、前記加熱器が、前記反応チャンバ及び前記ジャケット部分内の溶媒を加熱することができるようになり、前記ジャケット部分内の加熱された溶媒が、前記試料カップを加熱し、前記試料カップの内部の溶媒及び抽出試料を加熱することができるようになり、前記第2の入口からの溶媒が、前記開放濾過端を通って前記試料カップに入り、前記試料カップ内の抽出溶媒及び試料を有利に撹拌することができるようになる、前記試料調製器具。 - 前記ドレインフロアが大気圧に開放されているときに前記反応チャンバから加熱液体を受容するための、前記試料カップ内の前記ドレインフロアと液体連通したチラーをさらに備える、請求項23に記載の分子試料調製器具。
- 前記チラーが、前記ドレインフロアと液体連通した冷却コイルであり、前記冷却コイルが、共通抽出溶媒が前記冷却コイルの長さを移動するときに前記溶媒の温度を約50℃〜180℃から約25℃〜40℃まで低下させるのに十分な前記長さを有する、請求項24に記載の分子試料調製器具。
- 前記試料カップがシリンダーであり、前記開放濾過端が小孔フロアである、請求項23に記載の分子試料調製器具。
- 前記小孔フロア及び前記試料カップが、前記小孔フロアの除去のために螺設される、請求項26に記載の分子試料調製器具。
- 前記試料カップ内の前記小孔フロア上に静置する濾過媒体をさらに備え、
前記濾過媒体が、濾紙、石英繊維フィルタ、膜フィルタ、及び濾過マイクロプレートからなる群から選択される、請求項23に記載の分子試料調製器具。
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