JP6189752B2 - 固定化酵素反応器 - Google Patents
固定化酵素反応器 Download PDFInfo
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- JP6189752B2 JP6189752B2 JP2013554526A JP2013554526A JP6189752B2 JP 6189752 B2 JP6189752 B2 JP 6189752B2 JP 2013554526 A JP2013554526 A JP 2013554526A JP 2013554526 A JP2013554526 A JP 2013554526A JP 6189752 B2 JP6189752 B2 JP 6189752B2
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000004442 acylamino group Chemical group 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 125000004453 alkoxycarbonyl group Chemical group 0.000 description 1
- 125000005194 alkoxycarbonyloxy group Chemical group 0.000 description 1
- 125000004947 alkyl aryl amino group Chemical group 0.000 description 1
- 125000003806 alkyl carbonyl amino group Chemical group 0.000 description 1
- 125000004448 alkyl carbonyl group Chemical group 0.000 description 1
- 125000005196 alkyl carbonyloxy group Chemical group 0.000 description 1
- 125000004691 alkyl thio carbonyl group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- UMGDCJDMYOKAJW-UHFFFAOYSA-N aminothiocarboxamide Natural products NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 125000001769 aryl amino group Chemical group 0.000 description 1
- 125000004658 aryl carbonyl amino group Chemical group 0.000 description 1
- 125000005199 aryl carbonyloxy group Chemical group 0.000 description 1
- 125000005110 aryl thio group Chemical group 0.000 description 1
- 125000005200 aryloxy carbonyloxy group Chemical group 0.000 description 1
- 125000004104 aryloxy group Chemical group 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001540 azides Chemical class 0.000 description 1
- 125000000852 azido group Chemical group *N=[N+]=[N-] 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 125000000499 benzofuranyl group Chemical group O1C(=CC2=C1C=CC=C2)* 0.000 description 1
- 125000001164 benzothiazolyl group Chemical group S1C(=NC2=C1C=CC=C2)* 0.000 description 1
- 125000000051 benzyloxy group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])O* 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 229940098773 bovine serum albumin Drugs 0.000 description 1
- QXZGBUJJYSLZLT-FDISYFBBSA-N bradykinin Chemical class NC(=N)NCCC[C@H](N)C(=O)N1CCC[C@H]1C(=O)N1[C@H](C(=O)NCC(=O)N[C@@H](CC=2C=CC=CC=2)C(=O)N[C@@H](CO)C(=O)N2[C@@H](CCC2)C(=O)N[C@@H](CC=2C=CC=CC=2)C(=O)N[C@@H](CCCNC(N)=N)C(O)=O)CCC1 QXZGBUJJYSLZLT-FDISYFBBSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 235000010410 calcium alginate Nutrition 0.000 description 1
- 239000000648 calcium alginate Substances 0.000 description 1
- 229960002681 calcium alginate Drugs 0.000 description 1
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 1
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- GZGREZWGCWVAEE-UHFFFAOYSA-N chloro-dimethyl-octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](C)(C)Cl GZGREZWGCWVAEE-UHFFFAOYSA-N 0.000 description 1
- DBKNGKYVNBJWHL-UHFFFAOYSA-N chloro-dimethyl-octylsilane Chemical compound CCCCCCCC[Si](C)(C)Cl DBKNGKYVNBJWHL-UHFFFAOYSA-N 0.000 description 1
- 239000012501 chromatography medium Substances 0.000 description 1
- 229960002376 chymotrypsin Drugs 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 125000006448 cycloalkyl cycloalkyl group Chemical group 0.000 description 1
- KDUIUFJBNGTBMD-VXMYFEMYSA-N cyclooctatetraene Chemical compound C1=C\C=C/C=C\C=C1 KDUIUFJBNGTBMD-VXMYFEMYSA-N 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010511 deprotection reaction Methods 0.000 description 1
- 125000004986 diarylamino group Chemical group 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 125000002541 furyl group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229930195712 glutamate Natural products 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 230000003100 immobilizing effect Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical group 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- 101150035025 lysC gene Proteins 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- IZXGZAJMDLJLMF-UHFFFAOYSA-N methylaminomethanol Chemical compound CNCO IZXGZAJMDLJLMF-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 125000002950 monocyclic group Chemical group 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000004573 morpholin-4-yl group Chemical group N1(CCOCC1)* 0.000 description 1
- APVPOHHVBBYQAV-UHFFFAOYSA-N n-(4-aminophenyl)sulfonyloctadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NS(=O)(=O)C1=CC=C(N)C=C1 APVPOHHVBBYQAV-UHFFFAOYSA-N 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000002429 nitrogen sorption measurement Methods 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000002971 oxazolyl group Chemical group 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical group [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical group [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 108040002068 peptide-N4-(N-acetyl-beta-glucosaminyl)asparagine amidase activity proteins Proteins 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004344 phenylpropyl group Chemical group 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012514 protein characterization Methods 0.000 description 1
- 230000017854 proteolysis Effects 0.000 description 1
- 125000003373 pyrazinyl group Chemical group 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 125000000714 pyrimidinyl group Chemical group 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 125000005493 quinolyl group Chemical group 0.000 description 1
- 238000007342 radical addition reaction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 125000003718 tetrahydrofuranyl group Chemical group 0.000 description 1
- 125000001412 tetrahydropyranyl group Chemical group 0.000 description 1
- 125000000335 thiazolyl group Chemical group 0.000 description 1
- 125000001544 thienyl group Chemical group 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 238000001946 ultra-performance liquid chromatography-mass spectrometry Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
上記で使用したように、用語「脂肪族基」には、典型的には1から22個の炭素原子を有する直鎖もしくは分枝鎖を特徴とする有機化合物が含まれる。
本技術によるIMER装置、方法およびキットは、ポリマー分析物を含む液体サンプルの高圧連続流運転および分析を達成するために様々な固体固定相、リンカーおよび酵素を利用することができる。1つの例は、BEH(例、Waters Corporation社、米国マサチューセッツ州、BEH 130Å、BEH 200Å、またはBEH 300Å)である。圧力は、実際チャンバー圧(例、固体固定相床1mm当たりの圧力とは対照的に)を意味することができる。
W−[X]−Q 式1
(式中、Xは、シリカコア材料、金属酸化物コア材料、有機−無機ハイブリッドコア材料もしくは一群のこれらのブロックコポリマーを含む表面を有するコア組成物である;Wは、水素もしくはヒドロキシルである;およびQは、非存在、または分析物との静電相互作用、ファン・デル・ワールス(Van der Waals)相互作用、水素結合相互作用または他の相互作用を最小限に抑える官能基である。)によって表されるコア組成物および表面組成物を有する粒子またはモノリスを含んでいる。
a)固定相材料の表面と式3:
(B1)x(R5)y(R6)zSi− 式3
(式中、xは、1から30の整数である、
yは、0から2の整数である、
zは、0から2の整数である、
およびx+y+z=3である、
R5およびR6の各発生は、独立してメチル、エチル、n−ブチル、iso−ブチル、tert−ブチル、iso−プロピル、テキシル、置換もしくは未置換アリール、環状アルキル、分枝状アルキル、低級アルキル、保護もしくは脱保護アルコール、または両性イオンを表す;
B1は、−OR7、−NR7’R7’’、−OSO2CF3、もしくは−Clである;このときR7、R7’およびR7’’は、水素、メチル、エチル、n−ブチル、iso−ブチル、tert−ブチル、iso−プロピル、テキシル、フェニル、分枝状アルキルもしくは低級アルキルである。)の1部分との間の共有結合もしくは非共有結合の形成によって生成された表面付着基;
b)直接炭素−炭素結合形成を通して、またはヘテロ原子、エステル、エーテル、チオエーテル、アミン、アミド、イミド、ウレア、カーボネート、カルバメート、複素環、トリアゾール、もしくはウレタン結合を通してのXの表面ハイブリッド基への直接結合;または
c)固定相材料の表面に共有結合していない吸着基;
d)Wが水素である場合に、固定相材料の表面とビニルもしくはアルキニル基との反応による共有結合の形成によって生成された表面結合基)を表す;
Yは、直接結合;ヘテロ原子結合;エステル結合;エーテル結合;チオエーテル結合;アミン結合;アミド結合;イミド結合;ウレア結合;チオウレア結合;カーボネート結合;カルバメート結合;複素環結合;トリアゾール結合;ウレタン結合;ジオール結合;ポリオール結合;スチレン、エチレングリコール、もしくはプロピレングリコールのオリゴマー;スチレン、エチレングリコール、もしくはプロピレングリコールのポリマー;炭水化物基、多触角炭水化物、デンドリマーもしくはデンドリグラフ、または両性イオン基を表す;および
Aは、
i.)親水性末端基;
ii.)水素、フルオロ、フルオロアルキル、低級アルキル、もしくは基Z;または
iii.)官能化可能基を表す。
A.)親水性表面装飾を生じさせるシラン類
本技術によるIMER装置、方法およびキットは、ポリマー分析物を含む液体サンプルの高圧連続流運転および分析を達成するために様々な酵素を利用することができる。1つの例は、サンプル調製のためにHDX MSにおいて使用されるペプシンである。
本技術によるIMER装置、方法およびキットは、当該の酵素を固体固定相上に固定化するために様々なリンカーを使用することができる。1つの例は、トリエトキシシリルブチルアルデヒド(bALD−TEOS、Gelest社から入手できる。)である。
IMERは、高圧下で、例えば高圧LCシステム内で使用できる。1つの例は、Waters Corporation社製SYNAPT(商標)Q−TOF(商標)質量分析法と結合され、上昇エネルギー質量分析法(MSE)モードで獲得され、Waters Corporation社製ProteinLynx Global SERVER(商標)(PLGS、定量的および定性的プロテオミクス研究のための完全統合化Mass−Informatics(商標)プラットホームである。)を使用して処理される、Waters Corporation社(米国マサチューセッツ州)から入手できるnanoCQUITY UltraPerformance LC(登録商標)(UPLC(登録商標))システムである。
図3Aは、図2Aと結び付けて記載した900psiペプシン消化後のホスホリラーゼbのクロマトグラムを示している。900psiでホスホリラーゼbを消化すると118種の共通ペプチドで、76%の配列包括度が生じたのみである。これとは対照的に、図3Bは、図2Bと結び付けて記載した9,500psiペプシン消化後のホスホリラーゼbのクロマトグラムを示している。9,500psiでホスホリラーゼbを消化すると、無傷タンパク質が全く残留することなく、139種の共通ペプチドで、82%の配列包括度が生じた。このため、高圧消化は、より多数のペプチドおよびより高い配列包括度を生じさせた。
Claims (11)
- 入口および出口を有するチャンバーを規定する壁;
有機官能化シランリンカーを含む共有リンカーによって酵素に共有結合したエチレン架橋粒子を含み、チャンバー内に配置された固体固定相、ここでエチレン架橋粒子は、0.2から1.3cm 3 /gの範囲内の平均細孔容積、130から300Åの範囲内の平均孔径、および1.5から10μmの範囲内の平均径を有するものであり、;および
チャンバーと流体連絡していて、約172barから約2410barの間の圧力下で、ポリマー分析物を含む液体サンプルが入口から固体固定相を通って出口の外へ流れる、当該液体サンプルの連続流を維持するように適合された圧力モジュレーター
を含む装置。 - 圧力は、約552から約1030barの範囲内にある、請求項1に記載の装置。
- 出口から流出する分析物を収集するために構成された捕捉カラム;
収集された分析物を分離するために構成されたクロマトグラフィーカラム;および
分離された分析物を分析するために構成された質量分析計
をさらに含む、請求項1に記載の装置。 - 固体固定相に結合された捕捉基をさらに含む、請求項1に記載の装置。
- 約172barから約2410barの間の圧力下で、有機官能化シランリンカーを含む共有リンカーによって酵素に共有結合したエチレン架橋粒子を含む固体固定相にポリマー分析物を含む液体サンプルを流し、これによりポリマー分析物を酵素的に開裂させることを含む、ここでエチレン架橋粒子は、0.2から1.3cm 3 /gの範囲内の平均細孔容積、130から300Åの範囲内の平均孔径、および1.5から10μmの範囲内の平均径を有するものである、
ポリマー分析物を酵素的に開裂させる方法。 - 有機官能化シランリンカーを含む共有リンカーによって酵素に共有結合したエチレン架橋粒子を含み、ならびに酵素に対する共有結合を維持しながら約172barから約2410barの間の圧力下で操作する耐圧性固体固定相を提供すること、ここでエチレン架橋粒子は、0.2から1.3cm 3 /gの範囲内の平均細孔容積、130から300Åの範囲内の平均孔径、および1.5から10μmの範囲内の平均径を有するものであり、;および
入口および出口を有するチャンバー内に酵素に共有結合した固体固定相を添加すること;および
前記圧力下で入口から固体固定相を通って出口の外へ流れる、ポリマー分析物を含む液体サンプルの連続流を維持するように適合された圧力モジュレーターと流体連絡しているチャンバーを載置することを含む、ポリマー分析物を酵素的に開裂させる装置を提供する方法。 - 共有リンカーは、トリエトキシシリルブチルアルデヒドを含む、請求項5または6に記載の方法。
- 圧力は、約552から約1030barの範囲内にある、請求項5または6に記載の方法。
- 液体サンプルを流動しながら、(i)約172barから約2410barの間の圧力および(ii)約172bar未満の第2の圧力の間を循環させることをさらに含む、請求項6に記載の方法。
- 固体固定相が捕捉基に結合している、請求項5または6に記載の方法。
- 出口から流出する分析物を収集すること;
液体クロマトグラフィーによって収集された分析物を分離すること;および
分離された分析物を質量分析法によって分析することをさらに含む、請求項5または6に記載の方法。
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