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 (https=) | 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 (https=) |
| EP (2) | EP2336172B1 (https=) |
| JP (2) | JP5004586B2 (https=) |
| KR (2) | KR101221862B1 (https=) |
| CN (2) | CN1898266B (https=) |
| AU (1) | AU2004286938B2 (https=) |
| BR (2) | BR122020007658B1 (https=) |
| CA (1) | CA2543193C (https=) |
| CO (1) | CO5690649A2 (https=) |
| DK (2) | DK2336172T3 (https=) |
| EC (1) | ECSP066583A (https=) |
| ES (2) | ES2530446T3 (https=) |
| IL (1) | IL175229A (https=) |
| MX (1) | MXPA06004472A (https=) |
| NZ (1) | NZ547315A (https=) |
| PL (2) | PL1678208T3 (https=) |
| PT (2) | PT1678208E (https=) |
| RU (2) | RU2409591C2 (https=) |
| WO (1) | WO2005044856A2 (https=) |
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 |
| EP2336172B1 (en) * | 2003-10-27 | 2014-12-10 | Wyeth LLC | Removal of high molecular weight aggregates using hydroxyapatite chromatography |
| AU2006223180B2 (en) * | 2005-03-11 | 2011-11-24 | Wyeth Llc | A method of weak partitioning chromatography |
| TWI372763B (en) * | 2005-06-17 | 2012-09-21 | Wyeth Llc | Methods of purifying anti a beta antibodies |
| EP1893647A2 (en) * | 2005-06-23 | 2008-03-05 | MedImmune, Inc. | Antibody formulations having optimized aggregation and fragmentation profiles |
| AR058140A1 (es) * | 2005-10-24 | 2008-01-23 | Wyeth Corp | Metodo de produccion proteica utilizando compuestos anti-senescencia |
| BRPI0620316A2 (pt) * | 2005-12-21 | 2011-11-08 | Wyeth Corp | formulações de proteìnas com viscosidades reduzida e seus usos |
| EP2012118A4 (en) | 2006-04-25 | 2009-12-16 | Tosoh Corp | ISOLENT FOR IGG PURIFICATION AND METHOD FOR PURIFYING AN IGG MONOMER THEREFOR |
| US20100234577A1 (en) * | 2006-06-14 | 2010-09-16 | Smithkline Beecham Corporation | Methods for purifying antibodies using ceramic hydroxyapatite |
| DK2061803T4 (da) | 2006-08-28 | 2022-12-05 | Ares Trading Sa | Fremgangsmåde til oprensning af fc-holdige proteiner |
| EA017733B1 (ru) * | 2006-08-28 | 2013-02-28 | Арес Трейдинг С.А. | СПОСОБ ОЧИСТКИ Fc-СЛИТЫХ БЕЛКОВ |
| WO2008031020A2 (en) * | 2006-09-08 | 2008-03-13 | Wyeth | Arginine wash in protein purification using affinity chromatography |
| TWI456062B (zh) | 2006-09-13 | 2014-10-11 | Abbvie Inc | 細胞培養改良 |
| 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 |
| CA2674213A1 (en) * | 2007-01-26 | 2008-07-31 | Merck Serono S.A. | Purification of fc-taci fusion proteins using the oilbody technology |
| TW200902708A (en) | 2007-04-23 | 2009-01-16 | Wyeth Corp | Methods of protein production using anti-senescence compounds |
| CA2703086C (en) * | 2007-10-26 | 2014-11-25 | Asahi Kasei Chemicals Corporation | Method for purifying protein |
| US8188242B2 (en) | 2008-04-08 | 2012-05-29 | Bio-Rad Laboratories, Inc. | Chromatography purification of antibodies |
| MX2011001506A (es) † | 2008-08-14 | 2011-03-15 | Genentech Inc | Metodos para eliminar un contaminante utilizado cromatografia de membrana de intercambio de ion en desplazamiento de proteina indigena. |
| MX2011004201A (es) | 2008-10-20 | 2011-05-24 | Abbott Lab | Desactivacion viral durante purificacion de anticuerpos. |
| AU2009347206C1 (en) | 2008-10-20 | 2016-12-08 | Abbvie Inc. | Isolation and purification of antibodies using Protein A affinity chromatography |
| BRPI0919879A2 (pt) * | 2008-10-29 | 2016-02-16 | Wyeth Llc | métodos para purificação de moléculas de ligação a antígeno de domínio único |
| EP2362767B1 (en) | 2008-10-29 | 2017-12-06 | Ablynx N.V. | Formulations of single domain antigen binding molecules |
| EP2350130B1 (en) * | 2008-10-31 | 2018-10-03 | Wyeth LLC | Purification of acidic proteins using ceramic hydroxyapatite chromatography |
| CN102395597A (zh) * | 2009-03-11 | 2012-03-28 | 惠氏有限责任公司 | 纯化小模块免疫药物蛋白的方法 |
| US8481694B2 (en) | 2009-04-29 | 2013-07-09 | Bio-Rad Laboratories, Inc. | Purification of immunoconjugates |
| JPWO2011001963A1 (ja) | 2009-07-03 | 2012-12-13 | 旭化成ケミカルズ株式会社 | 多孔質基材に固定されたグラフト鎖に結合しているアミノ基及びアルキル基を有する多孔膜を用いた抗体の精製方法 |
| ES2813398T3 (es) | 2009-10-20 | 2021-03-23 | Abbvie Inc | Aislamiento y purificación de anticuerpos anti-IL-13 usando cromatografía de afinidad a Proteína A |
| EP2513134B1 (en) | 2009-12-18 | 2017-09-06 | Novartis AG | Wash solution and method for affinity chromatography |
| WO2011090720A2 (en) * | 2009-12-29 | 2011-07-28 | Dr. Reddy's Laboratories Ltd | Purification of proteins |
| WO2011088225A1 (en) | 2010-01-15 | 2011-07-21 | Bio-Rad Laboratories, Inc. | Surface neutralization of apatite |
| RU2012146448A (ru) | 2010-04-14 | 2014-05-20 | Ф.Хоффманн-Ля Рош Аг | Удаление агрегатов иммуноглобулинов |
| 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 |
| CA2814781A1 (en) | 2010-11-01 | 2012-05-10 | Diderik Reinder Kremer | Single unit ion exchange chromatography antibody purification |
| JP5881744B2 (ja) * | 2011-02-02 | 2016-03-09 | バイオ−ラッド ラボラトリーズ インコーポレーティッド | アルカリ溶液でのアパタイトの表面中和方法 |
| SG195306A1 (en) * | 2011-06-08 | 2013-12-30 | Agency Science Tech & Res | Purification of biological products by constrained cohydration chromatography |
| US20140187749A1 (en) | 2011-06-16 | 2014-07-03 | Dsm Ip Assets B.V. | Single unit chromatography antibody purification |
| SG10201701224UA (en) * | 2012-03-12 | 2017-04-27 | Merck Patent Gmbh | Removal of protein aggregates from biopharmaceutical preparations in a flowthrough mode |
| US9815695B2 (en) | 2012-05-30 | 2017-11-14 | Bio-Rad Laboratories, Inc. | In situ restoration of apatite-based chromatography resins |
| 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 |
| SG10201707477SA (en) | 2013-03-13 | 2017-10-30 | Eleven Biotherapeutics Inc | Chimeric cytokine formulations for ocular delivery |
| CA2909969A1 (en) * | 2013-05-13 | 2014-12-31 | Medimmune, Llc | Separation of recombinant polyclonal antibody multimers with minimal separation of monomers |
| MX384222B (es) | 2013-07-05 | 2025-03-14 | Lab Francais Du Fractionnement | Matriz de cromatografia de afinidad. |
| WO2015005960A1 (en) | 2013-07-12 | 2015-01-15 | Emd Millipore Corporation | Removal of fragments from a sample containing a target protein using activated carbon |
| 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 |
| WO2015088677A1 (en) | 2013-12-12 | 2015-06-18 | Emd Millipore Corporation | Protein separations using an acrylamide containing filter |
| BR112016014824A2 (pt) * | 2013-12-27 | 2017-09-19 | Chugai Pharmaceutical Co Ltd | Método para purificar anticorpo que tem ponto isoelétrico baixo |
| CN105392569B (zh) * | 2014-06-23 | 2019-08-20 | 生物辐射实验室股份有限公司 | 磷灰石预处理 |
| US10099157B2 (en) | 2014-06-23 | 2018-10-16 | 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 |
| KR102490956B1 (ko) | 2015-03-13 | 2023-01-19 | 브리스톨-마이어스 스큅 컴퍼니 | 불순물을 제거하기 위한 크로마토그래피 동안의 알칼리성 세척의 용도 |
| 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 |
| WO2019040671A1 (en) * | 2017-08-22 | 2019-02-28 | Biogen Ma Inc. | METHODS OF PURIFYING ANTIBODIES HAVING REDUCED AGGREGATES OF HIGH MOLECULAR WEIGHT |
| WO2019116096A1 (en) * | 2017-12-15 | 2019-06-20 | Laboratoire Francais Du Fractionnement Et Des Biotechnologies | Production of fc fragments |
| MX2020008931A (es) * | 2018-02-27 | 2020-10-01 | Pfizer | Purificacion de anticuerpos. |
| CN111902720B (zh) * | 2018-03-21 | 2025-02-07 | 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 |
| JP2021519339A (ja) | 2018-04-03 | 2021-08-10 | メルク パテント ゲーエムベーハー | Ｃｅｘクロマトグラフィー媒体及び生物製剤供給原料からの標的タンパク質の低塩溶出 |
| WO2019224660A1 (ja) * | 2018-05-24 | 2019-11-28 | 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 |
| IL293047A (en) | 2019-11-22 | 2022-07-01 | Morphosys Ag | A method for increasing 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 |
| IL296767A (en) | 2020-03-30 | 2022-11-01 | Ablynx Nv | A method for the production and purification of single variable multivalent immunoglobulin sites |
| EP4142792A4 (en) * | 2020-05-01 | 2024-11-27 | Kashiv Biosciences, LLC | An improved process of purification of protein |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | ||
| US419964A (en) | 1890-01-21 | Transom-lifter | ||
| 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 |
| WO2003059935A2 (en) | 2001-12-21 | 2003-07-24 | Immunex Corporation | Methods for purifying protein |
| AU2004215653B2 (en) | 2003-02-28 | 2011-03-17 | Lonza Biologics Plc. | Antibody purification by protein A and ion exchange chromatography |
| EP2336172B1 (en) * | 2003-10-27 | 2014-12-10 | Wyeth LLC | Removal of high molecular weight aggregates using hydroxyapatite chromatography |
-
2004
- 2004-10-06 EP EP10174366.4A patent/EP2336172B1/en not_active Expired - Lifetime
- 2004-10-06 CN CN2004800387536A patent/CN1898266B/zh not_active Expired - Lifetime
- 2004-10-06 KR KR1020067010375A patent/KR101221862B1/ko not_active Expired - Lifetime
- 2004-10-06 DK DK10174366.4T patent/DK2336172T3/en active
- 2004-10-06 BR BR122020007658-5A patent/BR122020007658B1/pt active IP Right Grant
- 2004-10-06 CN CN201110221442.5A patent/CN102276717B/zh not_active Expired - Lifetime
- 2004-10-06 JP JP2006538022A patent/JP5004586B2/ja not_active Expired - Lifetime
- 2004-10-06 DK DK04794288.3T patent/DK1678208T3/da active
- 2004-10-06 BR BRPI0415887-3A patent/BRPI0415887B1/pt not_active IP Right Cessation
- 2004-10-06 KR KR1020117030940A patent/KR101321876B1/ko not_active Expired - Lifetime
- 2004-10-06 PT PT47942883T patent/PT1678208E/pt unknown
- 2004-10-06 PL PL04794288T patent/PL1678208T3/pl unknown
- 2004-10-06 EP EP04794288.3A patent/EP1678208B1/en not_active Expired - Lifetime
- 2004-10-06 PT PT101743664T patent/PT2336172E/pt unknown
- 2004-10-06 ES ES10174366T patent/ES2530446T3/es not_active Expired - Lifetime
- 2004-10-06 NZ NZ547315A patent/NZ547315A/en unknown
- 2004-10-06 ES ES04794288T patent/ES2418830T3/es not_active Expired - Lifetime
- 2004-10-06 US US10/958,595 patent/US9469672B2/en active Active
- 2004-10-06 WO PCT/US2004/032883 patent/WO2005044856A2/en not_active Ceased
- 2004-10-06 AU AU2004286938A patent/AU2004286938B2/en not_active Expired
- 2004-10-06 MX MXPA06004472A patent/MXPA06004472A/es active IP Right Grant
- 2004-10-06 PL PL10174366T patent/PL2336172T3/pl unknown
- 2004-10-06 CA CA2543193A patent/CA2543193C/en not_active Expired - Fee Related
- 2004-10-06 RU RU2006113695/10A patent/RU2409591C2/ru 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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