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ᐇ㦂ࡢ㒊

ドキュメント内 茄蔕の細胞致死活性成分に関する研究 (ページ 35-42)

➨୍❶

࠙⣽⬊ࠚ

KB (Human cervical carcinoma)ࠊACC-MESO-1 (Human malignant mesothelioma)ࠊMCF-7 (Human breast cancer)ࠊMia-PaCa-2 (Human pancreatic cancer)ࠊHT-1080 (Human fibrosarcoma) ࡣࠊឡ▱Ꮫ㝔኱Ꮫ⸆Ꮫ㒊⏕య᭷ᶵ໬Ꮫㅮᗙ ⏣୰ ᇶḧ ᩍᤵࡼࡾࠊ HRA (Human ovarian

cancer) ࡣࠊྡྂᒇ኱Ꮫ኱Ꮫ㝔་Ꮫ◊✲⛉⏘፬ே⛉Ꮫศ㔝 ᰘ⏣ Ύ⃈ ඛ⏕ࡼࡾศ୚ࡉࢀ

ࡓࡶࡢࢆ౑⏝ࡋࡓࠋࡑࢀࡽࡢ⣽⬊ࡣࠊ࡟ 10%ศࡢ࢘ࢩ⫾ඣ⾑Ύ㸦FBSࠊSigma Aldrichࠊ St. LouisࠊMOࠊUSA㸧ࠊ࣌ࢽࢩࣜࣥ㸦100 unit/ml㸧ࠊࢫࢺࣞࣉࢺ࣐࢖ࢩࣥ㸦100 mg/ml㸧㸦ࢼ

࢝ࣛ࢖ࢸࢫࢡࠊி㒔㸧ࢆῧຍࡋࡓRPMI 1640ᇵᆅ㸦ࢼ࢝ࣛ࢖㸧࡛ࠊ5% CO2ୗ37Υ࡛ᇵ 㣴ࡋࡓࠋ

⥅௦࡟ࡣࠊ0.25%ࢺࣜࣉࢩࣥ in 0.53 mM EDTA⁐ᾮ㸦ࢼ࢝ࣛ࢖㸧࡛⣽⬊ࢆ3ศ㛫ฎ⌮

ࡍࡿࡇ࡜࡛๤㞳ࡋࡍࡿࡇ࡜࡟ࡼࡾ⾜ࡗࡓࠋ⣽⬊ᩘࡢ ᐃࡣࠊ⾑⌫ィ⟬ᯈࢆ⏝࠸࡚0.5㸣ࢺ

ࣜࣃࣥࣈ࣮ࣝᰁⰍᾮ㸦ࢼ࢝ࣛ࢖㸧࡛ᰁⰍࡍࡿࡇ࡜࡟ࡼࡾ⾜ࡗࡓࠋ

࠙⣽⬊⮴Ṛάᛶࡢ ᐃࠚ

ྛ✀⣽⬊ࢆ96✰ᖹᗏࣉ࣮ࣞࢺ㸦᪥ᮏࢪ࢙ࢿࢸ࢕ࢡࢫ㸧࡟5 × 10cell / 198 μl / well ࡎ ࡘ᧛✀ࡋࠊ24 hᇵ㣴ࡋࡓࠋࡑࡢᚋࠊDMSO࡛10 mg/mlࠊ1 mg/mlࠊ100 μg/mlࠊ10 μg/ml

࡟ㄪ〇ࡋࡓࢧࣥࣉࣝࢆ2 μlࡎࡘῧຍࡋ㸦᭱⤊⃰ᗘ㸸100ࠊ10ࠊ1ࠊ0.1 μg/ml㸧ࠊࡉࡽ࡟72 h ᇵ㣴ࡋࡓࠋࢥࣥࢺ࣮ࣟࣝ࡟ࡣDMSOࢆࠊ㝧ᛶࢥࣥࢺ࣮ࣟࣝ࡜ࡋ࡚adriamycin㸦༠࿴Ⓨ㓝࣭

ࣇ࢓࢖ࢨ࣮ࠊᮾி㸧ࢆ㝶᫬ᕼ㔘ࡋ࡚౑⏝ࡋࡓࠋMTT㸦ࢼ࢝ࣛ࢖㸧ࢆ3 mg/mlࡢ⃰ᗘ࡛20 μlࡎࡘῧຍࡋࠊࡉࡽ࡟4 hᇵ㣴ࡋࡓࠋᇵᆅࢆ㝖ཤᚋࠊDMSO 170 μlࢆῧຍࡋ࡚⏕ᡂࡋࡓ formazanࢆ⁐ゎࡋࠊ570 nm࡛ࡢ྾ගᗘࢆARVO MX 1420 multilabel counter (Perkin Elmerࠊ Winter Street WalthamࠊMAࠊUSA)ࠊࡲࡓࡣiMark Microplate Reader (Bio-RadࠊPhiladelphiaࠊ

PaࠊUSA) ࡟ࡼࡾ ᐃࡋࡓࠋྛ⸆≀ࡢ⃰ᗘ࡟࠾ࡅࡿ⣽⬊ቑṪᢚไ⋡ (%)ࢆ྾ගᗘࡼࡾ⟬

ฟࡋࠊ50%ࢆྵࡴ 3 ࡘࡢ␗࡞ࡿ⃰ᗘࡢᑐᩘ࡟ᑐࡍࡿ⣽⬊⏕Ꮡ⋡ࢆࣉࣟࢵࢺࡋࡓ࡜ࡁࡢ㏆

ఝ┤⥺ࢆ⏝࠸ࠊ50%ࢆ♧ࡍ⃰ᗘࢆIC50࡜ࡋࡓࠋ

࠙ࢼࢫࡀࡃ∦࢚࢟ࢫࡢㄪ〇࡜ศ⏬ࠚ

ᐇ㦂࡟౑⏝ࡋࡓࢼࢫᯝᐇࡣࠊྡྂᒇᕷෆࡢᕷሙ࡛㉎ධࡋࡓࠋ᪂㩭࡞༸ᙧࢼࢫᯝᐇ14 kg

ࢆࠊࡀࡃ∦㒊ศ2.8 kg࡜ࡑࢀ௨እࡢ㒊ศ࡟ศࡅࠊࡀࡃ∦㒊ศࡣ෾⤖஝⇱ࡋࠊ෾⤖஝⇱≀

2.6 x 102 gࢆᚓࡓࠋࡇࢀ࡟࢚ࢱࣀ࣮ࣝ2 lࢆຍ࠼୍࡚ᬌ෭ᾐᢳฟࢆ3ᅇ⾜࠸ࠊᢳฟᾮࢆྜ

ࢃࡏ࡚⃰⦰஝ᅛࡍࡿࡇ࡜࡟ࡼࡾࠊᢳฟ࢚࢟ࢫ7.6 gࢆᚓࡓࠋࡇࢀࢆ80㸣࣓ࢱࣀ࣮ࣝ3.6 l

࡟ᠱ⃮ࡋࠊ࣊࢟ࢧࣥ1.2 l࡛3ᅇ࡛ศ㓄ࡋࠊࡑࢀࡒࢀࡢ⏬ศࢆ⃰⦰஝ᅛࡋࡓࠋḟ࡟80%࣓

30

ࢱࣀ࣮ࣝ⏬ศࢆỈ3.6 l࡟ᠱ⃮ࡋࠊ㓑㓟࢚ࢳࣝ1.2 l࡛3ᅇศ㓄ࡋࠊࡉࡽ࡟Ỉ⏬ศࢆỈ1.2 l

࡛3 ᅇศ㓄ࡋࠊࡑࢀࡒࢀࡢ⏬ศࢆ⃰⦰஝ᅛࡋࡓࠋᚓࡽࢀࡓྛ⏬ศࡢ㔜㔞ࡣࠊ࣊࢟ࢧࣥ⏬

ศ㸦0.8 g㸧ࠊ㓑㓟࢚ࢳࣝ⏬ศ㸦1.3 g㸧ࠊỈ⏬ศ㸦5.2 g㸧࡛࠶ࡗࡓࠋ

ู࡟ࢼࢫᯝᐇࡢࡀࡃ∦ศ௨እࡢ㒊ศ200 gࢆࠊ࢚ࢱࣀ࣮ࣝ2 l࡛ྠᵝ࡟ᢳฟࡋࠊᢳฟ࢚

࢟ࢫ12.5 gࢆᚓࡓࠋ

ࡑࢀࡒࢀࡢࢼࢫࡀࡃ∦࢚ࢱࣀ࣮ࣝᢳฟ࢚࢟ࢫ࠾ࡼࡧࡑࡢྛ⏬ศࡣࠊ10 mg/ml࡜࡞ࡿࡼ

࠺࡟DMSO࡟⁐ゎࡋࠊ–20Υ࡛ಖᏑࡋࡓࠋ

㓑㓟࢚ࢳࣝ⏬ศ1.3 gࢆࠊࢩࣜ࢝ࢤ࣒ࣝ࢝ࣛࢡ࣐ࣟࢺࢢࣛࣇ࢕࣮㸦ࢩࣜ࢝ࢤࣝ60Nࠊ㛵 ᮾ໬Ꮫࠊᮾிࠊ4 cm × 20 cm㸧࡟౪ࡋࠊ࣓ࢱࣀ࣮ࣝ㸸ࢡ࣒ࣟࣟ࣍ࣝ㸸Ỉ㸦2 : 8 : 0.1㸧[13]

࡛⁐ฟࡉࡏࡓࠋ࣒࢝ࣛࡢ୰࡟㢧ⴭⓗ࡞ᅄࡘࡢࣂࣥࢻࢆྲྀࡗ࡚ࠊFr. 1ࠥFr. 4ࢆᚓࡓ㸦ࡑࢀ

ࡒࢀ7.2 mgࠊ683 mgࠊ142 mgࠊ258 mg㸧ࠋFr. 2㸦683mg㸧ࢆODSࢩࣜ࢝ࢤࣝࢡ࣐ࣟࢺࢢ

ࣛࣇ࢕࣮㸦ࢥࢫࣔࢩࣝ140C18-OPNࠊࢼ࢝ࣛ࢖ࠊ4 cm × 20 cm㸧࡟౪ࡋࠊ࣓ࢱࣀ࣮ࣝ㸭Ỉ 㸦1:1ࠊ4:1ࠊ1:0ࠊ300 mlࡎࡘẁ㝵ⓗ㸧࡛⁐ฟࡉࡏࡓࠋFr. 2-1ࠥ2-3㸦ࡑࢀࡒࢀ225.1 gࠊ48 mgࠊ 176 mg㸧ࢆᚓࡓࠋFr. 2-2㸦48 mg㸧ࢆศྲྀHPLC㸦ࢥࢫࣔࢩࣝC18-AR-ϩcolumn 10 × 150 mmࠊ ࢼ࢝ࣛ࢖㸧࡟౪ࡋࠊὶ㏿3 ml/minࠊỈ㸭࢔ࢭࢺࢽࢺࣜࣝ㸦50:50ࠊ0 min㸹30:70ࠊ30 min㸹 0㸸100ࠊ32 min㸧࡛⁐ฟࡉࡏࠊ280 nmࡢUV྾཰࠿ࡽࠊCompound 1㸦19 minࠊ0.13 mg㸧ࠊ

2㸦20 minࠊ0.25 mg㸧ࠊ3㸦24 minࠊ9.1 mg㸧ࠊ4㸦26minࠊ2.2 mg㸧ࢆᚓࡓࠋCompound 3࡜

4ࡢ໬Ꮫᵓ㐀ࡣࠊNMR㸦Bruker ABANCE 600ࠊMAࠊUSA㸧࡜EI-MS㸦᪥ᮏ㟁Ꮚࠊᮾி)

ࢆ ᐃࡋࡓࠋ

Compound 3࡜4ࡢࢼࢫᢳฟᾮ୰ࡢྵ㔞ࡢ ᐃࡣࠊ௨ୗࡢ᮲௳ࡢHPLC࡟ࡼࡾ⾜ࡗࡓ㸸

࣒࢝ࣛࠊࢥࢫࣔࢩࣝ5C18-AR-ϩcolumn 4.6 × 150 mm㸦ࢼࢼ࢝ࣛ࢖㸧㸹⛣ື┦ࠊỈ㸭࢔ࢭࢺࢽ ࢺࣜࣝ㸦50:50ࠊ0 min㸹30:70ࠊ20 min㸹0㸸100ࠊ22 min㸧㸹ὶ㏿ࠊ1 ml/min㸹᳨ฟࠊ UV 280 nmࠊ⁐ฟ᫬㛫ࠊcompound 3㸦19 min㸧ࠊcompound 4㸦20 min㸧ࠋ

࠙ྛ✀ࢼࢫࡀࡃ∦㒊ࠊ㢌㒊ࠊᯝᐇ࢚࢟ࢫࡢㄪ〇ࠚ

ᐇ㦂࡟౑⏝ࡋࡓྛ✀ࡢࢼࢫᯝᐇࡣࠊ᪥ᮏᕷሙရ࡛㉎ධࡋࡓࠋ

ྛ✀᪂㩭࡞ࢼࢫᯝᐇࢆࡀࡃ∦㒊ࠊ㢌㒊ཬࡧᯝᐇࡑࢀࡒࢀศࡅ࡚ࠊ୍ᬌຍ⇕஝⇱ࡋࠊࡑ

ࢀࡒࢀ1 gࢆᐇ㦂ᮦᩱ࡜ࡋ࡚ࠊ㓑㓟࢚ࢳࣝ10 mlࢆຍ࠼࡚minࡢࢯࢽࢣ࣮ࢩࣙࣥ࡟ࡼ

ࡿᢳฟࢆ3ᅇ⾜࠸ࠊᢳฟᾮࢆྜࢃࡏ࡚⃰⦰஝ᅛࡍࡿࡇ࡜࡟ࡼࡾࠊྛᢳฟ࢚࢟ࢫࢆᚓࡓࠋ

඲࡚ࡢᢳฟ࢚࢟ࢫࢆ࣓ࢱࣀ࣮࡛ࣝ10 mg/ml࡟ㄪ〇ࡋࡓࠋࡑࡢᚋࠊྛ⃰ᗘ㸦6.25ࠊ12.5ࠊ

25ࠊ50 μg/ml㸧ࡢ9-EE-KODEࢆ⏝࠸᳨࡚㔞⥺ࢆసᡂࡋࡓࠋࡑࢀࡒࢀࡢࢼࢫࡢྛ㒊఩ࡢᢳ

ฟ࢚࢟ࢫࢆHPLC࡛9-EE-KODE ࡢྵ᭷㔞ࢆ ᐃࡋࡓࠋ

➨஧❶

࠙9-EE-KODEࡢྜᡂࠚ

31

ྜᡂ࠾ࡼࡧ☜ㄆ᪉ἲ࡟ࡘ࠸࡚ࡣࠊᮏᩥ࡟グ㍕ࡋࡓࠋ

࠙MTTἲ࡟ࡼࡿ9-EE-KODEࡢ⣽⬊⮴Ṛస⏝ࡢ ᐃࠚ

9-EE-KODEῧຍᚋࠊ24 hᚋ࡟MTT⁐ᾮࢆῧຍࡋࡓ஦ࢆ㝖ࡁࠊ➨୍❶࡟‽ࡌ࡚⾜ࡗࡓࠋ

࠙BrdUἲ࡟ࡼࡿ9-EE-KODEࡢ⣽⬊⮴Ṛస⏝ࡢ ᐃࠚ

5-Bromo-2'-deoxyuridine Labeling & Detection Kit Ϫ㸦Roche Applied,ScienceࠊMannheimࠊ Germany㸧ࢆ౑⏝ࡋࡓࠋMTTἲ࡜ྠᵝ࡟᧯సࡋࠊMTT⁐ᾮࡢ௦ࢃࡾ࡟10 μlࡢBrdUᶆ㆑⁐

ᾮࢆῧຍࡋࠊ37Υ࡛ 2 h ࢖࣮ࣥ࢟ࣗ࣋ࢺࡋ࡚ࠊ᪂ࡓ࡟ྜᡂࡉࢀࡿDNA࡟ྲྀࡾ㎸ࡲࡏࡓࠋ ᇵᆅࢆ྾ᘬ㝖ཤᚋࠊ⣽⬊࡟200 μl/well ࡢ FixDenat ࢆῧຍࡋ࡚30 minࠊ25°C࡛ฎ⌮ࡍࡿ

ࡇ࡜࡟ࡼࡾᅛᐃࡋࡓࠋࡑࡢᚋࠊ100 μl/well ࡢPODᶆ㆑ᢠBrdU ᢠయ཯ᛂᾮࢆῧຍࡋ࡚ࠊ

15°C ࠊ90 minฎ⌮ࡋࡓࠋὙίᾮ࡛Ὑίᚋࠊ࣌ࣝ࢜࢟ࢩࢲ࣮ࢮࡢᇶ㉁ࢆຍ࠼ࠊ25°C࡛3 min

࢖࣮ࣥ࢟ࣗ࣋ࢺᚋࠊ405/490nmࡢ྾ගᗘࢆ࣐࢖ࢡࣟࣉ࣮ࣞࢺ࣮ࣜࢲ࣮ࢆ⏝࠸࡚ ᐃࡋࡓ

࠙࢔࣮࢞ࣟࢫࢤࣝ㟁ẼὋື࡟ࡼࡿ࢔࣏ࢺ࣮ࢩࢫࡢ᳨ฟࠚ

ᇵ㣴ࣇࣛࢫࢥ㸦50 mlࠊ᪥ᮏࢪ࢙ࢿࢸ࢕ࢡࢫࠊ᪥ᮏ㸧࡟2 × 106 ಶࡢHRA⣽⬊ࢆ᧛✀ࡋࠊ 24 h ᇵ㣴ᚋࠊᇵᆅࢆDMSO㸦Control㸧ࡲࡓࡣ9-EE-KODEࢆ1ࠊ5ࠊ10ࠊ100 μg/ml ྵࡴᇵ ᆅ࡜஺᥮ࡋࠊࡉࡽ࡟24 hᇵ㣴ࡋࡓࠋ⣽⬊ࢆᅇ཰ࡋࠊ⁐ゎࣂࢵࣇ࢓࣮㸦100 mM Tris-HClࠊ pH 8.5㸹5 mM EDTAࠊ0.2 M NaClࠊ0.2% SDSࠊ0.2 mg/ml proteinase K㸧ࢆ330 μlຍ࠼࡚37Υ

୍࡛ᬌ࢖࣮ࣥ࢟ࣗ࣋ࢺࡍࡿࡇ࡜࡟ࡼࡾࠊ⣽⬊ࢆ⁐ゎࡋࡓࠋ㐲ᚰศ㞳㸦1.5 x 104 rpmࠊ10 min㸧 ᚋࠊỿẊ࡟5 M NaCl 141 μlࢆຍ࠼ࠊ㍍ࡃᨩᢾࡋࡓᚋࠊࡉࡽ࡟㐲ᚰศ㞳ࡋࡓ㸦1.5 x 104 rpmࠊ 20 min㸧ࠋୖΎࢆ᪂ࡓ࡞ࢳ࣮ࣗࣈ࡟⛣ࡋ࡚ࠊ࢚ࢱࣀ࣮ࣝ470 μlࢆຍ࠼ࠊ㍍ࡃᨩᢾࡋࡓᚋࠊ 㐲ᚰศ㞳ࡋࡓ㸦1.5 x 104 rpmࠊ20 min㸧ࠋୖΎࢆ྾ᘬ㝖ཤࡋࠊỿẊ࡟70%࢚ࢱࣀ࣮ࣝ 400 μl

ࢆຍ࠼ࡓᚋࠊ㍍ࡃᨩᢾࡋ࡚ࠊ㐲ᚰศ㞳ࡋࡓ㸦1.5 x 104 rpmࠊ20 min㸧ࠋୖΎࢆ྾ᘬ㝖ཤࡋࠊ ỿẊ࡟Ỉࢆ15 μlῧຍࡋ࡚⁐ゎࡋࠊRNase A (10 mg/mL in Tris-EDTA buffer) ࢆ1 μlῧຍࡋࠊ 37ΥỈᾎ୍࡛ᬌ࡛࢖࣮ࣥ࢟ࣗ࣋ࢺࡋࡓࠋࡑࡢᚋࠊ㐲ᚰ㸦3 x 103 rpmࠊ20 min㸧ࡉࡏ࡚ࠊୖ

Ύࢆ㝖ཤࡋࠊỿẊࢆTris-EDTA buffer 20 μl࡛⁐ゎࡋࠊ2%࢔࣮࢞ࣟࢫࢤࣝࢆ⏝࠸࡚㟁ẼὋ

ືࡋࡓࠋศ㞳ࡋࡓDNA ࡣࠊ࢚ࢳࢪ࣒࢘ࣈ࣑ࣟࢻ࡛ࢤࣝࢆᰁⰍࡋࡓᚋࠊUV ࢺࣛࣥࢫ࢖ࣝ

࣑ࢿ࣮ࢱ࣮࡟ࡼࡾྍど໬ࡋࡓࠋ

࠙ࢾࢡࣞ࢜ࢯ࣮࣒࡟ࡼࡿDNA᩿∦ࡢ᳨ฟࠚ

Cell death detection ELISAPLUS㸦Roche Applied ScienceࠊPenzbergࠊUpper BavariaࠊGermany㸧

ࢆ⏝࠸࡚ ᐃࡋࡓࠋ96✰ࣉ࣮ࣞࢺ࡟HRA⣽⬊ࢆ1.5 × 104 cells/well᧛✀ࡋࠊ24 hᇵ㣴ᚋࠊ

9-EE-KODEࢆῧຍࡋ࡚ࡉࡽ࡟24 hࢆᇵ㣴ࡋࡓࠋࡑࡢᚋࠊ࢟ࢵࢺࡢㄝ᫂᭩࡟ᚑࡗ࡚ ᐃࡋ

ࡓࠋ⤖ᯝࡣࠊᮍฎ⌮㸦ᑐ↷㸧⣽⬊࡜9-EE-KODE࡛ฎ⌮ࡋࡓ⣽⬊࠿ࡽࡢ྾ගᗘࡢẚ࠿ࡽࠊ ௨ୗࡢᘧ࡟ࡼࡾィ⟬ࡋࡓenrichment factor࡜ࡋ࡚⾲ࡋࡓࠋ

32

࠙࢔ࢿ࢟ࢩࣥV ᰁⰍࠚ

ᇵ㣴ࣇࣛࢫࢥ㸦50 ml㸧࡟HRA⣽⬊ࢆ1.5 × 104 cells/wellࡢHRA⣽⬊ࢆ᧛✀ࡋࠊ6 hᇵ 㣴ࡋࡓᚋࠊྛ⃰ᗘࡢ9-EE-KODEࢆῧຍࡋࡓࠋ24 hᇵ㣴ᚋࠊPBS࡛Ὑίࡋࠊ⣽⬊࡟࢔ࢿ

࢟ࢩࣥV-ࣇࣝ࢜ࣞࢭࣜࣥ㸦Medical & Biological Laboratoriesࠊྡྂᒇ㸧ࢆ10 μlῧຍࡋࡓࠋ ᬯᡤᐊ ࡛15 min࢖࣮ࣥ࢟ࣗ࣋ࢺࡋࡓᚋࠊPBS ࡛Ὑίࡋࠊ⺯ග㢧ᚤ㙾࡛ほᐹࡋࡓࠋ

࠙Caspase-3/-7ࡢ ᐃࠚ

96✰ࣉ࣮ࣞࢺ࡟HRA⣽⬊ࢆ2 × 104 cells/well᧛✀ࡋࠊ24 hᇵ㣴ᚋࠊ9-EE-KODEࢆῧ ຍࡋ࡚24 hᇵ㣴ࡋࡓࠋᇵᆅࢆ྾ᘬ㝖ཤᚋࠊCaspase-3/7 reagent㸦PromegaࠊMadisonࠊWIࠊ USA㸧ࢆ100 μlῧຍࡋ࡚ᐊ ࡛1 hᇵ㣴ࡋࡓᚋࠊບ㉳Ἴ㛗498 nmࠊ྾཰Ἴ㛗521 nmࡢ⺯

ගࢆ࣑ࣝࣀ࣓࣮ࢱ࣮㸦Perkin ElmerࠊWinter Street WalthamࠊMAࠊUSA㸧࡛ ᐃࡋࡓࠋ

࣑࠙ࢺࢥࣥࢻࣜ࢔⭷㟁఩ࡢ ᐃࠚ

96✰㯮Ⰽࣉ࣮ࣞࢺ࡟HRA⣽⬊ࢆ1.5 × 104 cells/well᧛✀ࡋࠊ24 hᇵ㣴ᚋࠊ9-EE-KODE ࢆ ῧຍࡋ࡚12 hᇵ㣴ࡋࡓࠋࡑࡢᚋࠊCell MeterTM JC-10 Mitochondrial Membrane Potential࢟ࢵ

ࢺ㸦BiomolࠊHamburgࠊGermany㸧ࢆ౑⏝ࡋ࡚ࠊບ㉳Ἴ㛗490 nmࠊ྾཰Ἴ㛗535(⥳)/590(㉥) ࡢ⺯ගࢆ ᐃࡋࡓࠋ

࣑࠙ࢺࢥࣥࢻࣜ࢔ࡢBcl-2 ࢧࣈࣇ࢓࣑࣮ࣜࢱࣥࣃࢡ㉁ࡢ᳨ฟࠚ

6✰ࣉ࣮ࣞࢺ࡟HRA⣽⬊ࢆ1.5 × 104 cells/well᧛✀ࡋࠊ9-EE-KODEࢆῧຍࡋ࡚ࠊ24 hᇵ㣴 ࡋࡓࠋ⣽⬊ࢆࢺࣜࣉࢩࣥฎ⌮࡟ࡼࡾ᥇ྲྀࡋࠊ㐲ᚰศ㞳㸦2 x 103 rpmࠊ20 min㸧ᚋࠊỿẊ࡟

lysis buffer㸦50 M Tris-HCl, pH8.0ࠊ0.15 M NaClࠊ0.5% sodium deoxycholateࠊ0.1% SDS, 1.0 %

NP-40 substitute㸧ࢆ100 μlῧຍࡋࠊ㉸㡢Ἴ࡛⣽⬊ࢆ◚○ࡋࡓࠋࢱࣥࣃࢡ㉁⃰ᗘࡣࠊBCA ࣉ

ࣟࢸ࢖ࣥ࢔ࢵࢭ࢖࢟ࢵࢺ㸦Thermo ScientificࠊRockfordࠊILࠊUSA㸧࡛ ᐃࡋࡓࠋ25 μgࡢ

ྛࢧࣥࣉࣝࢆ12%࢔ࢡࣜࣝ࢔࣑ࢻࢤࣝࢆ౑⏝ࡋࡓSDS-PAGE࡟౪ࡋࡓࠋศᏊ㔞࣐࣮࣮࢝࡜

ࡋ࡚ࠊPrecision Plus ProteinTM Standards Dual Color㸦Bio-Rad㸧 ࢆ⏝࠸ࡓࠋ㟁ẼὋືᚋࡢࢤ

ࣝࡣࠊࢭ࣑ࢻࣛ࢖ᘧࣈࣟࢵࢸ࢕ࣥࢢ⿦⨨㸦ATTO AE-6687 HorizBLOT 2MࠊATTOࠊᮾி㸧

ࢆ⏝࠸࡚ࠊImmobilonTM-P Transfer Membrane㸦MilliporeࠊBillericaࠊMAࠊUSA㸧࡟㌿෗ࡋ ࡓࠋ⭷ࢆὙίᾮ㸦20 mM Tris-HClࠊpH 7.5ࠊ170 mM NaClࠊ0.05% Tween20㸧࡟࡚Ὑίࡋࠊ

10%ࣈࣟࢵࢡ࢚࣮ࢫ㸦DS ࣇ࢓࣮࣐ࣂ࢖࣓࢜ࢹ࢕࢝ࣝࠊ኱㜰㸧୰࡛ᐊ ࡛2 h࢖ࣥ࢟ࣗ࣋

࣮ࢺࡋࡓࠋḟ࡟10%ࣈࣟࢵࢡ࢚࣮ࢫ࡛ᕼ㔘ࡋࡓ௨ୗࡢ୍ḟᢠయᾮ࡛࣓ࣥࣈࣞࣥࢆ4°C୍࡛

33

ᬌ཯ᛂࡉࡏࠊὙίᾮ࡛3ᅇὙίᚋࠊ10%ࣈࣟࢵࢡ࢚࣮ࢫ࡛ᕼ㔘ࡋࡓ࣌ࣝ࢜࢟ࢩࢲ࣮ࢮᶆ㆑

ᢠ࣐࢘ࢫIgG㸦1:1 x 104ࠊJackson Immuno ResearchࠊRestonࠊVAࠊUSA㸧ࢆ⏝࠸࡚ᐊ ࡛1 h཯ᛂࡉࡏࡓࠋὙίᾮ࡛3ᅇὙίࡋࠊLuminateTM Forte Western HRP Substrate (Merck KGaA, Darmstadt, Germany㸧ᾮ࡟5 minᾐࡋࠊ໬ᏛⓎග᳨ฟჾ㸦LAS3000ࠊᐩኈࣇ࢕࣒ࣝࠊᮾி㸧

ࢆ౑⏝ࡋ࡚Ⓨගࢆ᳨ฟࡋࡓࠋⓎග⏬ീࡢゎᯒࡣIMAGE J1.46㸦ᐩኈࣇ࢖࣒ࣝ㸧ࢆ⏝࠸ࡓࠋ

᧜ᙳᚋࡢ࣓ࣥࣈࣞࣥࡣࠊWB-stripping solution㸦ࢼࢼ࢝ࣛ࢖㸧࡛37°Cࠊ9ศ㛫Ὑίࡋࠊ෌ࡧࣈ

ࣟࢵ࢟ࣥࢢࢆ⾜࠺ࡇ࡜ู࡛ࡢࢱࣥࣃࢡ㉁ࡢ᳨ฟ࡟⏝࠸ࡓࠋ

࣑࠙ࢺࢥࣥࢻࣜ࢔ෆ࡜⣽⬊㉁ෆࡢCytochrome cࡢ ᐃࠚ

6✰ࣉ࣮ࣞࢺ࡟HRA⣽⬊ࢆ1.5 × 104 cells/well᧛✀ࡋ࡚24 hᇵ㣴ࡋࠊ9-EE-KODE࡛ 24 hᇵ㣴ࡋࡓࠋ⣽⬊ࢆࢺࣜࣉࢩࣥฎ⌮࡟ࡼࡾ᥇ྲྀࡋࠊMitochondria/Cytosol Fractionation Kit 㸦AbcamࠊCambridgeࠊUK㸧࡛࣑ࢺࢥࣥࢻࣜ࢔࡜⣽⬊㉁ࢆศ㞳ࡋࠊ๓⠇࡜ྠᵝࡢ᪉ἲ࡛

᳨ฟࡋࡓࠋ

࠙౑⏝ࡋࡓᢠయࠚ

ศᏊ✀ ࣓࣮࣮࢝ ᕼ㔘ẚ⋡ kDa

Bcl-2 Cell Signaling㸦DanversࠊMAࠊUSA㸧 1:1000 26

Bcl-xL Cell Signaling 1:1000 30

Bax Cell Signaling 1:1000 20

Cytochrome c Abcam 1:500 12

β-actin Santa Cruz Biotechnology㸦Santa CruzࠊCAࠊUSA㸧 1:500 43

34

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ドキュメント内 茄蔕の細胞致死活性成分に関する研究 (ページ 35-42)

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