JP7257968B2 - トリフルリジン及び/又はチピラシル由来の類縁物質の検出方法 - Google Patents
トリフルリジン及び/又はチピラシル由来の類縁物質の検出方法 Download PDFInfo
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Description
類縁物質1:トリフルオロチミン、
類縁物質2:2-イミノピロリジン、
類縁物質3:5-クロロ-6-{(2-オキソピロリジン-1-イル)メチル}ピリミジン-2,4-(1H、3H)-ジオン、
類縁物質4:2’-デオキシ-5-メトキシカルボニルウリジン、
類縁物質5:5-カルボキシウラシル。
より好ましくは、有機相がアセトニトリルからなり、かつ類縁物質3及びチピラシルの保持時間におけるアセトニトリルが移動相全体の5~20容量%である高速液体クロマトグラフィーによる方法である。
より好ましくは、移動相がアセトニトリル及びリン酸又はリン酸二水素カリウムを含む水相からなり、かつ類縁物質3及びチピラシルの保持時間におけるアセトニトリルが移動相全体の7~15%である高速液体クロマトグラフィーによる方法である。
・検出器:紫外吸光光度計(波長は210nm)
・カラム:内径4.6mm,長さ15cmのステンレス管に5μmの液体クロマトグラフィー用オクタデシルシリル化シリカゲルカラム
・カラム温度:40℃
・流量:0.6~1.0mL/分
・移動相:各実施例に記載
・グラジエント:各実施例に記載
高速液体クロマトグラフィーで測定する試料は以下の通り調製した。
カラム:Inertsil ODS-4、GLサイエンス社製
移動相:リン酸二水素ナトリウム二水和物1.4g及び1-ヘプタンスルホン酸ナトリウム0.9gを水900mLに溶かし,リン酸を加えてpH2.7に調整した。この液にメタノール100mLを加えて移動相とした。
カラム:Inertsil ODS-4、GLサイエンス社製
移動相:リン酸二水素ナトリウム二水和物1.5g及び1-ヘプタンスルホン酸ナトリウム0.9gを水900mLに溶かし,リン酸を加えてpH2.7に調整した。この液にメタノール100mLを加えて移動相とした。
カラム:Inertsil ODS-4、GLサイエンス社製
移動相:リン酸二水素ナトリウム二水和物1.4g及び1-ヘプタンスルホン酸ナトリウム1.0gを水900mLに溶かし,リン酸を加えてpH2.8に調整した。この液にメタノール100mLを加えて移動相とした。
カラム:Inertsil ODS-4、GLサイエンス社製
移動相:リン酸二水素ナトリウム二水和物1.4g及び1-ヘプタンスルホン酸ナトリウム0.9gを水900mLに溶かし,リン酸を加えてpH2.7に調整した。この液にメタノール95mLを加えて移動相とした。
カラム:Wakosil-II 5C18 RS、和光純薬製
移動相:リン酸二水素ナトリウム二水和物1.4g及び1-ヘプタンスルホン酸ナトリウム0.9gを水900mLに溶かし,リン酸を加えてpH2.7に調整した。この液にメタノール100mLを加えて移動相とした。
カラム:Wakosil-II 5C18 RS、和光純薬製
移動相:リン酸二水素ナトリウム二水和物3.1g及び1-ヘプタンスルホン酸ナトリウム2.0gを水2000mLに溶かし,リン酸を加えてpH2.7に調整した。この液950mLにメタノール50mLを加えて移動相とした。
カラム:Wakosil-II 5C18 RS、和光純薬製
移動相:リン酸二水素カリウム1.25g及び1-ヘプタンスルホン酸ナトリウム1.01gを水920mLに溶かし,アセトニトリル80mLを加えて移動相とした。
カラム:Inertsil ODS-3、GLサイエンス社製
移動相:1-ヘプタンスルホン酸ナトリウム1.88gを水1860mLに溶かし,アセトニトリル140mLを加え,リン酸を加えてpH2.7に調整した。
カラム:Wakosil-II 5C18 RS、和光純薬製
移動相:1-ヘプタンスルホン酸ナトリウム1.01gをとり、水を加えて1000mLとした。この液850mLにメタノール150mLを加え、リン酸を加えてpH2.7に調整した。
チピラシル塩酸塩の濃度が約0.8mg/mLとなるよう水/アセトニトリル混合溶液(23:2)に溶解させ、適宜希釈した溶液をチピラシルのみ含む試料とした。
移動相:リン酸二水素カリウム1.25g及び1-ヘプタンスルホン酸ナトリウム1.01gを水920mLに溶かし,アセトニトリル80mLを加えて移動相とした。
Claims (7)
- トリフルリジン又はその塩、及びチピラシル又はその塩を含む試料を有機相及び水相からなる移動相を用いる高速液体クロマトグラフィーに供する工程を含む、トリフルリジン由来の類縁物質及びチピラシル由来の類縁物質の一方又は両方を検出するための方法であって、前記検出が試料中に含まれる少なくとも1つの類縁物質1~5の検出を含み、
類縁物質1:トリフルオロチミン、
類縁物質2:2-イミノピロリジン、
類縁物質3:5-クロロ-6-{(2-オキソピロリジン-1-イル)メチル}ピリミジン-2,4-(1H、3H)-ジオン、
類縁物質4:2’-デオキシ-5-メトキシカルボニルウリジン、
類縁物質5:5-カルボキシウラシル、
であり、類縁物質1~5、トリフルリジン及びチピラシルの保持時間における移動相全体に対する有機相の割合がいずれも7~15容量%である、方法。 - 前記類縁物質が類縁物質3を含み、高速液体クロマトグラフィーにおける類縁物質3とトリフルリジンとの保持時間が1.0分以上異なっている、請求項1に記載の方法。
- 前記有機相がメタノールを含む、請求項1又は2に記載の方法。
- 水相が、リン酸もしくはその塩またはこれらの混合物を含む、請求項1~3のいずれか1項に記載の方法。
- 類縁物質1、3、4及びトリフルリジンの保持時間における移動相全体に対する有機相の割合のうち、最も大きい値と最も小さい値との差が、移動相全体の5容量%以下である、請求項1~4のいずれか1項に記載の方法。
- 移動相のpHが2.0~5.0である、請求項1~5のいずれか1項に記載の方法。
- 移動相のpHが2.6~2.8である、請求項6に記載の方法。
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JP2017246043 | 2017-12-22 | ||
JP2017246043 | 2017-12-22 | ||
US15/952,367 | 2018-04-13 | ||
US15/952,367 US10866219B2 (en) | 2017-12-22 | 2018-04-13 | Method for detecting trifluridine- and/or tipiracil-related substance |
CN201810427364.6A CN109959733B (zh) | 2017-12-22 | 2018-05-07 | 源自曲氟尿苷及/或替吡嘧啶的类似物质的检测方法 |
CN201810427364.6 | 2018-05-07 | ||
PCT/JP2018/047223 WO2019124544A1 (ja) | 2017-12-22 | 2018-12-21 | トリフルリジン及び/又はチピラシル由来の類縁物質の検出方法 |
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WO2013122134A1 (ja) | 2012-02-15 | 2013-08-22 | 大鵬薬品工業株式会社 | 経口投与用医薬組成物 |
CN107271592A (zh) | 2017-06-07 | 2017-10-20 | 江苏悦兴医药技术有限公司 | 一种盐酸替吡拉西与其相关杂质完全分离的液相色谱纯度检测方法 |
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JPS6110565A (ja) | 1984-06-26 | 1986-01-18 | Takeda Chem Ind Ltd | ウラシル−5−カルボン酸エステル類の製造法 |
JPH0231686A (ja) * | 1988-07-22 | 1990-02-01 | Yuki Gosei Kogyo Co Ltd | トリフルオロチミジンの製造方法 |
JP3040200B2 (ja) * | 1991-07-03 | 2000-05-08 | 三井化学株式会社 | トリフルオロチミジン誘導体、その製造法およびそれを含有する抗腫瘍剤 |
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US10866219B2 (en) | 2020-12-15 |
CN109959733A (zh) | 2019-07-02 |
CN109959733B (zh) | 2024-04-09 |
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US20190195840A1 (en) | 2019-06-27 |
JPWO2019124544A1 (ja) | 2021-01-14 |
MA51332A (fr) | 2020-10-28 |
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