Method for separating hemporfin isomer and separated isomer
A technology of isomers and hydroxyethyl groups, applied in the field of photosensitizers for photodynamic therapy, can solve problems such as single molecular structure
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Embodiment 1
[0075] Embodiment 1: the preparation of hemporfin
[0076] 1.3 (8)-(1-methoxyethyl)-8(3)-(1-hydroxyethyl) hypoporphyrin IX crude product preparation
[0077] In a 50L acid-resistant glass-lined reaction pot, add 30L of methanol / water mixed solution with a volume ratio of 3:1, slowly drop it in from a liquid dropper under stirring, and prepare 3 , 8-bis-(1-bromoethyl)-hypoporphyrin IX hydrobromide glacial acetic acid saturated solution 10L, control the rate of addition to keep the temperature of the reaction mixture at 10-20°C. After the dropwise addition, the reaction solution continued to stir for 2h and left for 4h. Then add 10N NaOH aqueous solution dropwise under stirring until the reaction liquid is strongly alkaline (pH13 or so), let stand for more than 10h, add acetic acid to neutralize to pH4~5, add 5 times the volume of water to dilute, stand overnight, the precipitate will naturally precipitate, After decanting the supernatant, the precipitate was collected by suct...
Embodiment 2
[0080] Example 2: HPLC Separation of Hemporfin Positional Isomers
[0081] Instrument: Agilent1100 high performance liquid chromatography; DAD detector, detection wavelength: 395nm
[0082] Mobile phase: methanol—1.5M acetic acid—ammonium acetate buffer (pH4.76) (65:35V / V)
[0083] Chromatographic column: MOS—Hypersil (C 8 ), 10×250mm
[0084] Flow rate: 2mL / min
[0085] Column pressure: 125Bar
[0086] Take 100 mg of the hemporfin sample prepared in Example 1 above, dissolve it in HPLC mobile phase, prepare a sample solution with a concentration of 5 mg / mL, and filter it before injection. Each injection of 400 microliters of the above solution, after injection, according to the HPLC chromatogram (see figure 1 ) to collect fraction A respectively, the retention time is 11.94 minutes and the fraction B retention time is 14.35 minutes. Accumulated 40 times, a total of 136ml of fraction A and 133ml of fraction B were collected. Pour the collected solution into ethyl acetat...
Embodiment 3
[0090] Example 3: Preparative Separation of Hemporfin Positional Isomers
[0091] The separation system adopts Flash150M, built-in pre-installed C 8 The chromatographic column (150mm ID×30cm) is produced by Biotage Company (USA), the silica gel particle size is 35-70 μm, and the pore size is 60A.
[0092] Sample preparation: get 3 (or 8)-(1-methoxyethyl)-8 (or 3)-(1-hydroxyethyl) hypoporphyrin IX pure product (content>95%) prepared in Example 1 30 g was dissolved in tetrahydrofuran and filtered, and 100 g of C8 reversed-phase silica gel was added, concentrated under reduced pressure, evaporated to dryness, and added to the loading column SIM for sample loading.
[0093] Sample loading and collection: Using methanol-1.5M acetic acid-ammonium acetate buffer (pH4.76) (65:35V / V) as the mobile phase, the above sample is passed through the loading column SIM and brought into the chromatographic column for separation , the flow rate is controlled at 200ml / min, the detector waveleng...
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