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| 精密称取各多糖样品约15 mg，置于10 mL具塞试管中，加蒸馏水1 mL，加热溶解，再加入2 mL，2 mol•L-1三氟乙酸溶液，摇匀，密封。将其放入烘箱中，110℃加热水解8 h，取出冷却至室温后，室温下离心5 min，转速12000 r•min-1，移出上清液至10 mL容量瓶中，用2 mol•L-1 NaOH中和至PH约7.0，水定容至刻度，摇匀，PMP衍生化，含量测定。色谱柱：迪马科技PLATISIL ODS柱（250 mm × 4.6 mm，5 μm）；柱温：35℃；流动相：乙腈-20 mmol•L-1醋酸铵缓冲液（22∶78）（PH=5.5）；流速：1.0 mL•min-1；紫外检测波长：245 nm；进样量：10 μL。 |
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LifePursuit
木虫之王 (文学泰斗)
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80后的末班车: 金币+30, 翻译EPI+1, ★★★★★最佳答案, 非常感谢 2014-12-01 20:05:50
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| A precise quantity (~15 mg) of polysaccharide sample was weighed and put in a 10 mL test tube with a plug, to which 1 mL distilled water was added. The test tube was heated such that the polysaccharide sample was dissolved, and 2 mL trifluoroacetic acid (2 mol•L-1) was added. The mixed solution was shaken uniformly and sealed. The test tube was then placed in an oven, where it was heated at 110 ℃ for hydrolysis. After 8 h it was taken out, cooled to ambient temperature, and centrifuged at 12000 r•min-1 for 5 min. The supernatant was collected and transferred to a 10 mL volumetric flask, where it was neutralized by NaOH (2 mol•L-1) to pH = ~7.0, diluted with water to volume, and shaken uniformly for PMP derivation and content measurement. The chromatographic column is a PLATISIL ODS column (250 mm × 4.6 mm, 5 μm) made by Dikma Technologies Inc. The column temperature is 35℃. The mobile phase is acetonitrile - 20 mmol•L-1 ammonium acetate buffer（22∶78） with pH = 5.5. The flow rate is 1.0 mL•min-1. The UV detection wavelength is 245 nm. The injection volume is 10 μL. |
2楼2014-12-01 19:41:37
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