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| 精密稱取各多糖樣品約15 mg,置于10 mL具塞試管中,加蒸餾水1 mL,加熱溶解,再加入2 mL,2 mol•L-1三氟乙酸溶液,搖勻,密封。將其放入烘箱中,110℃加熱水解8 h,取出冷卻至室溫后,室溫下離心5 min,轉(zhuǎn)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約7.0,水定容至刻度,搖勻,PMP衍生化,含量測(cè)定。色譜柱:迪馬科技PLATISIL ODS柱(250 mm × 4.6 mm,5 μm);柱溫:35℃;流動(dòng)相:乙腈-20 mmol•L-1醋酸銨緩沖液(22∶78)(PH=5.5);流速:1.0 mL•min-1;紫外檢測(cè)波長:245 nm;進(jìn)樣量:10 μL。 |

木蟲之王 (文學(xué)泰斗)
| 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. |
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