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| Synthesis of meso-5,10,15,20-Tetrakis(4-N-methylpyridiniumyl)porphyrinato Manganese(III) Pentachloride (Mn−PyP). Mn−PyP was synthesized according to literature methods (Scheme S1, Supporting Information).20 Briefly, porphyrin tetratosylate (101 mg, 0.074 mmol) and manganese(II) chloride tetrahydrate (16 mg, 0.081 mmol) were added to 15 mL of methanol. The mixture was refluxed with stirring under N2 atm. UV−vis absorption spectroscopy was used to monitor the reaction, and it was stopped when the Soret band completely shifted from 422 to 463 nm. Subsequently, the tosylate anion was exchanged by chloride ion on 5 g anion-exchange resin (DOWEX 1 × 8−200) for 24 h with slow stirring. The solution was filtered, and the resin was washed with methanol. The methanol solution was concentrated to 1−2 mL, and the product was precipitated by the addition of Et2O. The precipitate was filtered, washed with Et2O, dried, and dissolved in 4 mL of water. Finally, the manganese salt was allowed to precipitate at 4 °C, and the aqueous phase was filtered and then evaporated. After drying under vacuum, Mn−PyP was obtained as a purple solid. The product was characterized by electrospray ionization mass spectrometry (ESI-MS) (Figure S1). The ESI-MS analysis provided a m/z value of 182.9, whereas the calculated m/z value for [C44H36MnN8]4+ was 182.8, which confirmed the identity and purity of the probe. Assay Procedures. The VEGF luminol CL assay was performed at an ambient temperature. Briefly, 980 μL of Tris− HCl solution (20 mM, pH 9.0) containing 50 nM VEGF165 aptamer 1 (or 80 nM VEGF165 aptamer 2), 10 nM Mn−PyP, 25 μM luminol, 2 mM H2O2, 0.05% Triton X-100, and VEGF of different concentrations were mixed. Then, 20 μL of H 2O2 stock solution (100 mM) was quickly added. The CL signal at 1 min was collected by the MCDR-A system. The photomultiplier tube (PMT) voltage was set at 500 V. The biological fluid analysis was conducted in the sample mixtures containing 0.1%, 1% human serum, or 1% human serum with albumin and IgG removed (Figures S9−S11). The procedures were the same as described above. |
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jiangguofeng
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| 内消旋5,10,15,20 -四（4 - N -甲基吡啶基）卟啉锰(III)五氯化物( Mn - PyP)的合成。Mn - PyP是根据文献方法（图S1,支持信息）合成的。20 简单地说就是,将卟啉四对甲苯磺酸酯( 101毫克，0.074毫摩尔）和氯化锰四水合物( 16毫克, 0.081毫摩尔）加到15毫升甲醇中。混合物于N2气压下搅拌回流。用紫外-可见吸收光谱法监控反应,当索瑞氏光谱带完全地由422移至463nm时停止反应。随后,缓慢搅拌的同时于５克阴离子交换树脂（道威克斯1?8 - 200)上用氯离子对甲苯磺酸盐阴离子进行交换24小时。过滤溶液,用甲醇洗涤树脂。将甲醇溶液浓缩至1-２毫升，添加Et2O使产物析出。滤出沉淀物用Et2O洗涤、干燥再溶于４毫升水中。最后,于4℃使锰盐沉淀,过滤水相然后蒸发。 真空干燥后得到紫色固体Mn-PyP。 产物通过电喷雾质谱( ESI - MS)进行表征(图S1)。电喷雾质谱分析给出[C44H36MnN8]4+的m/Z值为182.9,而计算的m／Z值为182.8，这就证明了试样的同一性和纯度。 VEGF鲁米诺CL含量测定于常温中进行。简言之,将含有50nM的VEGF165适配体1(或80nM的VEGF165适配体2）、10 nM的Mn-PyP、25μΜ的鲁米诺、2mM的H2O2、0.05%的曲拉通X-100和不同浓度的VEGF的980μL的盐酸溶液（20mM, pH值9.0)进行混合。然后, 将20μL的H 2O2储备溶液( 100 mM)迅速地加进。通过MCDR - A系统收集于1分钟的CL信号。光电倍增管(PMT)电压设置为500 V。使用含有0.1%、1%人体血清或1%除去白蛋白和IgG的人体血清的混合物样品进行生物流体分析（图S9 - S11）。具体程序如上所述。 |
2楼2015-11-09 09:43:10