JP2007532477A5 - - Google Patents
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- Publication number
- JP2007532477A5 JP2007532477A5 JP2006538022A JP2006538022A JP2007532477A5 JP 2007532477 A5 JP2007532477 A5 JP 2007532477A5 JP 2006538022 A JP2006538022 A JP 2006538022A JP 2006538022 A JP2006538022 A JP 2006538022A JP 2007532477 A5 JP2007532477 A5 JP 2007532477A5
- Authority
- JP
- Japan
- Prior art keywords
- antibody
- protein
- substrate
- ion exchange
- hydroxyapatite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 26
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 26
- 102000004169 proteins and genes Human genes 0.000 claims description 24
- 108090000623 proteins and genes Proteins 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 22
- 239000011347 resin Substances 0.000 claims description 22
- 229920005989 resin Polymers 0.000 claims description 22
- 238000005342 ion exchange Methods 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 239000011534 wash buffer Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000004587 chromatography analysis Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000012149 elution buffer Substances 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- 239000012160 loading buffer Substances 0.000 claims description 4
- 238000004255 ion exchange chromatography Methods 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 238000001042 affinity chromatography Methods 0.000 claims 1
- 239000000178 monomer Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000005349 anion exchange Methods 0.000 description 5
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 4
- 239000000872 buffer Substances 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910000160 potassium phosphate Inorganic materials 0.000 description 2
- 235000011009 potassium phosphates Nutrition 0.000 description 2
- 108060003951 Immunoglobulin Proteins 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000006167 equilibration buffer Substances 0.000 description 1
- 102000018358 immunoglobulin Human genes 0.000 description 1
- 229940072221 immunoglobulins Drugs 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US51401803P | 2003-10-27 | 2003-10-27 | |
| US60/514,018 | 2003-10-27 | ||
| US52333503P | 2003-11-20 | 2003-11-20 | |
| US60/523,335 | 2003-11-20 | ||
| PCT/US2004/032883 WO2005044856A2 (en) | 2003-10-27 | 2004-10-06 | Removal of high molecular weight aggregates using hydroxyapatite chromatography |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2012013648A Division JP5490156B2 (ja) | 2003-10-27 | 2012-01-26 | ヒドロキシアパタイトクロマトグラフィーを用いる高分子量凝集体の取り出し |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JP2007532477A JP2007532477A (ja) | 2007-11-15 |
| JP2007532477A5 true JP2007532477A5 (enExample) | 2012-03-22 |
| JP5004586B2 JP5004586B2 (ja) | 2012-08-22 |
Family
ID=34576743
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006538022A Expired - Lifetime JP5004586B2 (ja) | 2003-10-27 | 2004-10-06 | ヒドロキシアパタイトクロマトグラフィーを用いる高分子量凝集体の取り出し |
| JP2012013648A Expired - Lifetime JP5490156B2 (ja) | 2003-10-27 | 2012-01-26 | ヒドロキシアパタイトクロマトグラフィーを用いる高分子量凝集体の取り出し |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2012013648A Expired - Lifetime JP5490156B2 (ja) | 2003-10-27 | 2012-01-26 | ヒドロキシアパタイトクロマトグラフィーを用いる高分子量凝集体の取り出し |
Country Status (19)
| Country | Link |
|---|---|
| US (2) | US9469672B2 (enExample) |
| EP (2) | EP1678208B1 (enExample) |
| JP (2) | JP5004586B2 (enExample) |
| KR (2) | KR101321876B1 (enExample) |
| CN (2) | CN1898266B (enExample) |
| AU (1) | AU2004286938B2 (enExample) |
| BR (2) | BR122020007658B1 (enExample) |
| CA (1) | CA2543193C (enExample) |
| CO (1) | CO5690649A2 (enExample) |
| DK (2) | DK2336172T3 (enExample) |
| EC (1) | ECSP066583A (enExample) |
| ES (2) | ES2418830T3 (enExample) |
| IL (1) | IL175229A (enExample) |
| MX (1) | MXPA06004472A (enExample) |
| NZ (1) | NZ547315A (enExample) |
| PL (2) | PL2336172T3 (enExample) |
| PT (2) | PT1678208E (enExample) |
| RU (2) | RU2409591C2 (enExample) |
| WO (1) | WO2005044856A2 (enExample) |
Families Citing this family (71)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0304576D0 (en) * | 2003-02-28 | 2003-04-02 | Lonza Biologics Plc | Protein a chromatography |
| EP1678208B1 (en) * | 2003-10-27 | 2013-05-15 | Wyeth LLC | Removal of high molecular weight aggregates using hydroxyapatite chromatography |
| MX2007011129A (es) | 2005-03-11 | 2007-11-06 | Wyeth Corp | Un metodo de cromatografia de particion debil. |
| CA2611815A1 (en) | 2005-06-17 | 2006-12-28 | Elan Pharma International Limited | Methods of purifying anti a beta antibodies |
| US20070110757A1 (en) * | 2005-06-23 | 2007-05-17 | Ziping Wei | Antibody formulations having optimized aggregation and fragmentation profiles |
| PE20070796A1 (es) * | 2005-10-24 | 2007-08-15 | Wyeth Corp | Metodo de produccion proteica utilizando compuestos anti-senescencia |
| WO2007076062A2 (en) | 2005-12-21 | 2007-07-05 | Wyeth | Protein formulations with reduced viscosity and uses thereof |
| WO2007123242A1 (ja) | 2006-04-25 | 2007-11-01 | Tosoh Corporation | ＩｇＧ精製用分離剤、及びそれを用いたＩｇＧ単量体の精製方法 |
| JP2010510963A (ja) * | 2006-06-14 | 2010-04-08 | グラクソスミスクライン・リミテッド・ライアビリティ・カンパニー | セラミックヒドロキシアパタイトを使用する抗体の精製方法 |
| EP2061802A1 (en) * | 2006-08-28 | 2009-05-27 | Ares Trading S.A. | Process for the purification of fc-fusion proteins |
| JP2010501623A (ja) | 2006-08-28 | 2010-01-21 | アレス トレーディング ソシエテ アノニム | Ｆｃ含有タンパク質の精製法 |
| US7714111B2 (en) * | 2006-09-08 | 2010-05-11 | Wyeth Llc | Arginine derivative wash in protein purification using affinity chromatography |
| CN103276033A (zh) | 2006-09-13 | 2013-09-04 | 雅培制药有限公司 | 细胞培养改良 |
| US8911964B2 (en) | 2006-09-13 | 2014-12-16 | Abbvie Inc. | Fed-batch method of making human anti-TNF-alpha antibody |
| US7691980B2 (en) * | 2007-01-09 | 2010-04-06 | Bio-Rad Laboratories, Inc. | Enhanced capacity and purification of antibodies by mixed mode chromatography in the presence of aqueous-soluble nonionic organic polymers |
| US7999085B2 (en) * | 2007-01-09 | 2011-08-16 | Bio-Rad Laboratories, Inc. | Enhanced capacity and purification of protein by mixed mode chromatography in the presence of aqueous-soluble nonionic organic polymers |
| ES2366593T3 (es) * | 2007-01-26 | 2011-10-21 | Merck Serono S.A. | Purificación de proteínas de fusión taci-fc empleando la tecnología de cuerpos grasos. |
| TW200902708A (en) | 2007-04-23 | 2009-01-16 | Wyeth Corp | Methods of protein production using anti-senescence compounds |
| KR101163307B1 (ko) * | 2007-10-26 | 2012-07-05 | 아사히 가세이 케미칼즈 가부시키가이샤 | 단백질의 정제 방법 |
| EP2265129B1 (en) * | 2008-04-08 | 2015-10-28 | Bio-Rad Laboratories, Inc. | Chromatography purification of antibodies |
| DK2848625T3 (da) † | 2008-08-14 | 2019-10-07 | Genentech Inc | Fremgangsmåder til fjernelse af en kontaminant under anvendelse af ion bytningsmembrankromatografi med forskydning af naturligt forekommende proteiner |
| CN105111309A (zh) * | 2008-10-20 | 2015-12-02 | Abbvie公司 | 使用a蛋白亲和层析分离和纯化抗体 |
| CN104974251A (zh) | 2008-10-20 | 2015-10-14 | Abbvie公司 | 在抗体纯化过程中的病毒灭活 |
| WO2010056550A1 (en) | 2008-10-29 | 2010-05-20 | Wyeth Llc | Methods for purification of single domain antigen binding molecules |
| KR101593285B1 (ko) | 2008-10-29 | 2016-02-11 | 아블린쓰 엔.브이. | 단일 도메인 항원 결합 분자의 제형 |
| US8058407B2 (en) * | 2008-10-31 | 2011-11-15 | Wyeth Llc | Purification of acidic proteins using ceramic hydroxyapatite chromatography |
| RU2011137030A (ru) * | 2009-03-11 | 2013-04-20 | УАЙТ ЭлЭлСи | Способы очистки малых модулярных иммунофармацевтических белков |
| US8481694B2 (en) | 2009-04-29 | 2013-07-09 | Bio-Rad Laboratories, Inc. | Purification of immunoconjugates |
| US9441011B2 (en) | 2009-07-03 | 2016-09-13 | Asahi Kasei Chemicals Corporation | Method for purification of antibody using porous membrane having amino group and alkyl group both bound to graft chain immobilized on porous substrate |
| MX341136B (es) | 2009-10-20 | 2016-08-09 | Abbvie Inc | Aislamiento y purificacion de los anticuerpos anti-il-13 al usar la cromatografia de afinidad con proteina a. |
| ES2982297T3 (es) | 2009-12-18 | 2024-10-15 | Novartis Ag | Método de cromatografía de afinidad |
| EP2519537A4 (en) * | 2009-12-29 | 2013-07-10 | Reddys Lab Ltd Dr | CLEANING PROTEINS |
| CA2787009C (en) | 2010-01-15 | 2018-04-03 | Bio-Rad Laboratories, Inc. | Surface neutralization of apatite |
| ES2613454T3 (es) | 2010-04-14 | 2017-05-24 | F. Hoffmann-La Roche Ag | Eliminación de agregados de inmunoglobulina |
| GB201006753D0 (en) | 2010-04-22 | 2010-06-09 | Biotest Ag | Process for preparing an immunolobulin composition |
| WO2011156073A1 (en) * | 2010-06-08 | 2011-12-15 | Millipore Corporation | Removal of protein aggregates from biopharmaceutical preparations using calcium phosphate salts |
| US8895707B2 (en) * | 2010-08-18 | 2014-11-25 | Bio-Rad Laboratories, Inc. | Elution of proteins from hydroxyapatite resins without resin deterioration |
| EP2635599A1 (en) * | 2010-11-01 | 2013-09-11 | DSM IP Assets B.V. | Single unit ion exchange chromatography antibody purification |
| US9592540B2 (en) | 2011-02-02 | 2017-03-14 | Bio-Rad Laboratories, Inc. | Apatite surface neutralization with alkali solutions |
| SG195306A1 (en) * | 2011-06-08 | 2013-12-30 | Agency Science Tech & Res | Purification of biological products by constrained cohydration chromatography |
| JP2014529330A (ja) * | 2011-06-16 | 2014-11-06 | ディーエスエム アイピー アセッツ ビー．ブイ． | 単一ユニットクロマトグラフィー抗体精製 |
| SG10201701224UA (en) * | 2012-03-12 | 2017-04-27 | Merck Patent Gmbh | Removal of protein aggregates from biopharmaceutical preparations in a flowthrough mode |
| CN104507952B (zh) | 2012-05-30 | 2018-08-10 | 生物辐射实验室股份有限公司 | 基于磷灰石的色谱树脂的原位恢复 |
| WO2014003142A1 (ja) * | 2012-06-27 | 2014-01-03 | 旭化成メディカル株式会社 | 抗体 |
| JP2014105180A (ja) * | 2012-11-27 | 2014-06-09 | Hoya Corp | モノマー化方法 |
| JP6450364B2 (ja) | 2013-03-13 | 2019-01-09 | セセン バイオ， インコーポレイテッド | 眼送達のためのキメラサイトカイン製剤 |
| EP2997041A4 (en) * | 2013-05-13 | 2017-02-15 | Medlmmune, LLC | Separation of recombinant polyclonal antibody multimers with minimal separation of monomers |
| AU2014285971A1 (en) | 2013-07-05 | 2016-02-04 | Laboratoire Francais Du Fractionnement Et Des Biotechnologies | Affinity chromatography matrix |
| JP6479305B2 (ja) * | 2013-07-12 | 2019-03-06 | 株式会社Ｕｍｎファーマ | ウイルス様粒子の精製方法 |
| JP6141524B2 (ja) | 2013-07-12 | 2017-06-07 | メルク パテント ゲーエムベーハー | 活性炭を用いた標的タンパク質含有サンプルからのフラグメントの除去 |
| EP3698870A1 (en) | 2013-12-12 | 2020-08-26 | EMD Millipore Corporation | Protein separations using an acrylamide containing filter |
| US10654933B2 (en) * | 2013-12-27 | 2020-05-19 | Chugai Seiyaku Kabushiki Kaisha | Method for purifying antibody having low isoelectric point |
| WO2015200282A1 (en) | 2014-06-23 | 2015-12-30 | Bio-Rad Laboratories, Inc. | Apatite pretreatment |
| US10092857B2 (en) | 2014-06-23 | 2018-10-09 | Bio-Rad Laboratories, Inc. | Apatite in-situ restoration |
| EP3233230B1 (en) | 2014-12-15 | 2024-06-12 | Merck Patent GmbH | Target molecule capture from crude solutions |
| AU2016233557B2 (en) | 2015-03-13 | 2021-06-24 | Bristol-Myers Squibb Company | Use of alkaline washes during chromatography to remove impurities |
| US11661438B2 (en) | 2015-12-21 | 2023-05-30 | Pfizer, Inc. | Purification of antibody drug conjugates using a sodium phosphate gradient |
| US11919924B1 (en) * | 2016-03-15 | 2024-03-05 | Fresenius Kabi Deutschland Gmbh | Methods of purifying and producing an adalimumab antibody |
| US11186858B1 (en) | 2016-03-15 | 2021-11-30 | Fresenius Kabi Deutschland Gmbh | Methods for increasing biosimilarity |
| CN106977591B (zh) * | 2017-05-04 | 2020-05-05 | 广州康盛生物科技股份有限公司 | 一种分离纯化重组葡萄球菌蛋白a的方法 |
| US11697670B2 (en) | 2017-08-22 | 2023-07-11 | Biogen Ma Inc. | Methods for purifying antibodies having reduced high molecular weight aggregates |
| WO2019116096A1 (en) * | 2017-12-15 | 2019-06-20 | Laboratoire Francais Du Fractionnement Et Des Biotechnologies | Production of fc fragments |
| BR112020015603A2 (pt) * | 2018-02-27 | 2021-01-05 | Pfizer Inc. | Purificação de anticorpo |
| CN119881293A (zh) | 2018-03-21 | 2025-04-25 | 沃特世科技公司 | 基于非抗体高亲和力的样品制备、吸附剂、装置和方法 |
| US20210024573A1 (en) | 2018-04-03 | 2021-01-28 | Merck Patent Gmbh | Cex chromatography media and low salt elution of target proteins from biopharmaceutical feeds |
| JP6951051B2 (ja) * | 2018-05-24 | 2021-10-20 | ＨＯＹＡ Ｔｅｃｈｎｏｓｕｒｇｉｃａｌ株式会社 | 吸着剤の生産方法 |
| JP6704074B2 (ja) * | 2019-02-04 | 2020-06-03 | 株式会社Ｕｍｎファーマ | ウイルス様粒子の精製方法 |
| WO2021099536A1 (en) | 2019-11-22 | 2021-05-27 | Morphosys Ag | Method to increase antibody yield during ion exchange chromatography |
| JP2020099909A (ja) * | 2020-03-17 | 2020-07-02 | ＨＯＹＡ Ｔｅｃｈｎｏｓｕｒｇｉｃａｌ株式会社 | 処理方法、生産方法およびハイドロキシアパタイト充填剤 |
| US20230136595A1 (en) | 2020-03-30 | 2023-05-04 | Ablynx Nv | Method for the production and purification of multivalent immunoglobulin single variable domains |
| JP2023523823A (ja) * | 2020-05-01 | 2023-06-07 | カシーヴ バイオサイエンシズ，リミテッド・ライアビリティ・カンパニー | タンパク質の精製の改善されたプロセス |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US419964A (en) | 1890-01-21 | Transom-lifter | ||
| US428894A (en) | 1890-05-27 | Process of making tool-handles | ||
| US523335A (en) | 1894-07-24 | Air-bolt for flour-mills | ||
| US514018A (en) | 1894-02-06 | Edward j | ||
| US4745183A (en) * | 1984-02-21 | 1988-05-17 | Bio-Rad Laboratories, Inc. | Use of hydroxylapatite for the analysis and preparation of purified monoclonal antibodies |
| JPH03291300A (ja) * | 1989-12-28 | 1991-12-20 | Mitsui Toatsu Chem Inc | ポリクローナル抗体の分離方法 |
| GB9022545D0 (en) * | 1990-10-17 | 1990-11-28 | Wellcome Found | Culture medium |
| TWI255272B (en) * | 2000-12-06 | 2006-05-21 | Guriq Basi | Humanized antibodies that recognize beta amyloid peptide |
| PL374311A1 (en) * | 2001-12-21 | 2005-10-03 | Immunex Corporation | Methods for purifying protein |
| DK1601697T3 (da) | 2003-02-28 | 2007-10-01 | Lonza Biologics Plc | Oprensning af antistof ved protein A- og ionbytningskromatografi |
| EP1678208B1 (en) * | 2003-10-27 | 2013-05-15 | Wyeth LLC | Removal of high molecular weight aggregates using hydroxyapatite chromatography |
-
2004
- 2004-10-06 EP EP04794288.3A patent/EP1678208B1/en not_active Expired - Lifetime
- 2004-10-06 AU AU2004286938A patent/AU2004286938B2/en not_active Expired
- 2004-10-06 KR KR1020117030940A patent/KR101321876B1/ko not_active Expired - Lifetime
- 2004-10-06 JP JP2006538022A patent/JP5004586B2/ja not_active Expired - Lifetime
- 2004-10-06 BR BR122020007658-5A patent/BR122020007658B1/pt active IP Right Grant
- 2004-10-06 NZ NZ547315A patent/NZ547315A/en unknown
- 2004-10-06 EP EP10174366.4A patent/EP2336172B1/en not_active Expired - Lifetime
- 2004-10-06 ES ES04794288T patent/ES2418830T3/es not_active Expired - Lifetime
- 2004-10-06 DK DK10174366.4T patent/DK2336172T3/en active
- 2004-10-06 MX MXPA06004472A patent/MXPA06004472A/es active IP Right Grant
- 2004-10-06 KR KR1020067010375A patent/KR101221862B1/ko not_active Expired - Lifetime
- 2004-10-06 PT PT47942883T patent/PT1678208E/pt unknown
- 2004-10-06 CN CN2004800387536A patent/CN1898266B/zh not_active Expired - Lifetime
- 2004-10-06 US US10/958,595 patent/US9469672B2/en active Active
- 2004-10-06 PL PL10174366T patent/PL2336172T3/pl unknown
- 2004-10-06 PT PT101743664T patent/PT2336172E/pt unknown
- 2004-10-06 PL PL04794288T patent/PL1678208T3/pl unknown
- 2004-10-06 CA CA2543193A patent/CA2543193C/en not_active Expired - Fee Related
- 2004-10-06 CN CN201110221442.5A patent/CN102276717B/zh not_active Expired - Lifetime
- 2004-10-06 ES ES10174366T patent/ES2530446T3/es not_active Expired - Lifetime
- 2004-10-06 BR BRPI0415887-3A patent/BRPI0415887B1/pt not_active IP Right Cessation
- 2004-10-06 WO PCT/US2004/032883 patent/WO2005044856A2/en not_active Ceased
- 2004-10-06 RU RU2006113695/10A patent/RU2409591C2/ru active
- 2004-10-06 DK DK04794288.3T patent/DK1678208T3/da active
-
2006
- 2006-04-26 IL IL175229A patent/IL175229A/en active IP Right Grant
- 2006-05-19 CO CO06048228A patent/CO5690649A2/es not_active Application Discontinuation
- 2006-05-25 EC EC2006006583A patent/ECSP066583A/es unknown
-
2010
- 2010-09-24 RU RU2010139827/10A patent/RU2573910C2/ru active
-
2012
- 2012-01-26 JP JP2012013648A patent/JP5490156B2/ja not_active Expired - Lifetime
-
2013
- 2013-03-14 US US13/803,071 patent/US9822143B2/en not_active Expired - Lifetime
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