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wangshengchao金虫 (正式写手)
学徒
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[交流]
那位高手测定过甘露醇的含量?
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| 那位高手测定过甘露醇的含量?用什么柱子?溶剂?不胜感激! |
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9楼2008-10-10 16:56:05
2楼2008-10-08 11:03:41
wangshengchao
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3楼2008-10-10 15:45:10
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HPLC-ELSD不是药典推荐的方法，ELSD检测器现在好多地方都有，我们公司也有；但测定甘露醇含量仍然是采用药典推荐的示差折光检测器： Assay— Mobile phase— Use degassed water. Resolution solution— Dissolve sorbitol and USP Mannitol RS in water to obtain a solution having concentrations of about 4.8 mg per mL of each. Standard preparation— Dissolve an accurately weighed quantity of USP Mannitol RS in water, and dilute quantitatively with water to obtain a solution having a known concentration of about 4.8 mg per mL. Assay preparation— Transfer about 0.24 g of Mannitol, accurately weighed, to a 50-mL volumetric flask, dissolve in 10 mL of water, dilute with water to volume, and mix. Chromatographic system (see Chromatography 621)—The liquid chromatograph is equipped with a refractive index detector that is maintained at a constant temperature and a 4-mm × 25-cm column that contains packing L19. The column temperature is maintained at a temperature between 30 and 85 controlled within ±2 of the selected temperature, and the flow rate is about 0.5 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the relative standard deviation for replicate injections is not more than 2.0%. In a similar manner, chromatograph the Resolution solution: the resolution, R, between the sorbitol and mannitol peaks is not less than 2.0. Procedure— Separately inject equal volumes (about 20 µL) of the Assay preparation and the Standard preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in mg, of C6H14O6, in the Mannitol taken by the formula: 50C(rU / rS) in which C is the concentration, in mg per mL, of USP Mannitol RS in the Standard preparation; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively. 你也可以建立HPLC-ELSD方法，但需要做研究。你是沈药的，在你们学校找一个ELSD还不容易？ [ Last edited by 脂质体 on 2008-10-10 at 16:08 ] |
6楼2008-10-10 16:05:59
