JP2014218511A5 - - Google Patents

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Publication number
JP2014218511A5
JP2014218511A5 JP2014163640A JP2014163640A JP2014218511A5 JP 2014218511 A5 JP2014218511 A5 JP 2014218511A5 JP 2014163640 A JP2014163640 A JP 2014163640A JP 2014163640 A JP2014163640 A JP 2014163640A JP 2014218511 A5 JP2014218511 A5 JP 2014218511A5
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JP
Japan
Prior art keywords
crystal
free energy
surface free
less
luliconazole
Prior art date
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JP2014163640A
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Japanese (ja)
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JP2014218511A (en
JP6268060B2 (en
Filing date
Publication date
Priority claimed from PCT/JP2013/063094 external-priority patent/WO2014041846A1/en
Application filed filed Critical
Priority to JP2014163640A priority Critical patent/JP6268060B2/en
Priority claimed from JP2014163640A external-priority patent/JP6268060B2/en
Publication of JP2014218511A publication Critical patent/JP2014218511A/en
Publication of JP2014218511A5 publication Critical patent/JP2014218511A5/ja
Application granted granted Critical
Publication of JP6268060B2 publication Critical patent/JP6268060B2/en
Expired - Fee Related legal-status Critical Current
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Claims (4)

酢酸エチル−ｎ−ヘキサンの混合溶媒、又はエタノール−水の混合溶媒から選択される溶媒を用いた再結晶によって得られるルリコナゾールの結晶が、次に示す表面自由エネルギーの条件を充足するか否かを鑑別する工程、及び、前記工程で表面自由エネルギーの条件を充足した結晶を、製剤適格性があると判別する工程、により、製剤適格性を有すると判断された結晶を準備する工程、
を含む、ルリコナゾールの結晶の製造方法。
（表面自由エネルギーの条件）
ルリコナゾールの結晶の表面自由エネルギーが２８ｍＪ／ｍ 2 以下であり、表面自由エ
ネルギーにおける極性成分の割合が３５％以下である。 A mixed solvent of -n- ethyl acetate-hexane, or ethanol - crystallization Le Rikonazoru obtained by recrystallization from a solvent selected from a mixed solvent of water, whether or not to satisfy the following surface free energy condition And a step of discriminating that the crystal satisfying the condition of surface free energy in the above step has a formulation suitability, a step of preparing a crystal judged to have a formulation suitability ,
Including, method for producing crystals of luliconazole.
(Surface free energy conditions)
The surface free energy of the crystal of luliconazole is 28 mJ / m 2 or less, and the surface free energy
The ratio of polar components in energy is 35% or less. 前記判別する工程において、固体製剤に適した結晶であると判別される、請求項１に記載の結晶の製造方法。 In the step of the judging, Ru is judged that crystals suitable for solid formulations, method for producing a crystal according to claim 1. 前記結晶は、酢酸エチル−ｎ−ヘキサンの混合溶媒、又はエタノール−水の混合溶媒から選択される溶媒を用いた再結晶によって得られる、ルリコナゾールの結晶であって、以下の１〜４の条件を備えた、請求項１又は２に記載の結晶の製造方法。
１．結晶の表面自由エネルギーにおける極性成分の割合が３１％以下であること。
２．結晶の表面自由エネルギーにおける分散成分が１８ｍＪ／ｍ2以上であること。
３．結晶の表面自由エネルギーにおける極性成分が８．２ｍＪ／ｍ2以下であること。
４．結晶の表面自由エネルギーが、２７．４ｍＪ／ｍ2以下であること。 The crystal is a crystal of luliconazole obtained by recrystallization using a solvent selected from a mixed solvent of ethyl acetate-n-hexane or a mixed solvent of ethanol-water, and the following conditions 1 to 4 are satisfied. The manufacturing method of the crystal | crystallization of Claim 1 or 2 provided.
1. The ratio of the polar component in the surface free energy of the crystal is 31% or less.
2. The dispersion component in the surface free energy of the crystal is 18 mJ / m 2 or more.
3. The polar component in the surface free energy of the crystal is 8.2 mJ / m 2 or less.
4). The surface free energy of the crystal is 27.4 mJ / m 2 or less. 前記結晶は、８０℃６時間、水懸濁（浸潤条件又は加湿条件）及び６０００ｌｘの曝光条件保存後の、ルリコナゾールの結晶におけるＺ体の生成率が、ルリコナゾールの結晶の０．１１質量％未満である、請求項１〜３のいずれか一項に記載の結晶の製造方法。 The crystals, 80 ° C. 6 hours, water suspensions after storage light exposure conditions (infiltration conditions or humidification conditions) and 6000 lx, the production rate of the Z-isomer in the crystals of luliconazole is less than 0.11 wt% of the crystals of luliconazole The manufacturing method of the crystal | crystallization as described in any one of Claims 1-3.
JP2014163640A 2013-04-30 2014-08-11 Crystals evaluated using surface free energy of crystals as an index, and pharmaceutical compositions containing the crystals Expired - Fee Related JP6268060B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2014163640A JP6268060B2 (en) 2013-04-30 2014-08-11 Crystals evaluated using surface free energy of crystals as an index, and pharmaceutical compositions containing the crystals

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
PCT/JP2013/063094 WO2014041846A1 (en) 2012-09-14 2013-04-30 Use of surface free energy for differential evaluation of crystal, crystal evaluated on basis of surface free energy as index, and phrmaceutical composition prepared by containing the crystal
WOPCT/JP2013/063094 2013-04-30
JP2014163640A JP6268060B2 (en) 2013-04-30 2014-08-11 Crystals evaluated using surface free energy of crystals as an index, and pharmaceutical compositions containing the crystals

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
JP2014046406A Division JP5686914B2 (en) 2013-04-30 2014-03-10 Crystals evaluated using surface free energy of crystals as an index, and pharmaceutical compositions containing the crystals

Publications (3)

Publication Number Publication Date
JP2014218511A JP2014218511A (en) 2014-11-20
JP2014218511A5 true JP2014218511A5 (en) 2017-04-20
JP6268060B2 JP6268060B2 (en) 2018-01-24

Family

ID=51937308

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2014163640A Expired - Fee Related JP6268060B2 (en) 2013-04-30 2014-08-11 Crystals evaluated using surface free energy of crystals as an index, and pharmaceutical compositions containing the crystals

Country Status (1)

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JP (1) JP6268060B2 (en)

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3278738B2 (en) * 1995-07-08 2002-04-30 日本農薬株式会社 Antifungal agent
CN103012385B (en) * 2012-02-17 2015-07-08 山东威智医药工业有限公司 Crystal form of luliconazole and preparation method thereof

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