摘要:
目的 比较注射用甘露聚糖肽的两种含量测定方法。 方法 分别采用分光光度法和高效液相色谱法测定D-甘露糖的含量。 结果 分光光度法测定中,供试品溶于苯酚溶液和硫酸中,于 490 nm 波长处检测,D-甘露糖衍生物浓度线性范围是 10.2~51 μg/ml(r=0.999 1),平均含量为92.14%, RSD平均值为1.17%。HPLC法测定中,用色谱柱:Gemini C18(250 mm×4.6 mm,5 μm);流动相:乙腈-0.02 mol/L 乙酸铵溶液(20:80),流速:1 ml/min;检测波长:250 nm;柱温:30 ℃;进样量:10 μl。检测结果,平均含量为83.47%, RSD平均值为0.65%,两种方法均能有效测定D-甘露糖的含量。 结论 分光光度法测定的平均含量较高,但检测中使用的苯酚有特殊臭味、有毒、具腐蚀性,对操作者会造成一定的危险性;HPLC法专属性强,色谱图更直观,对操作者的危害性和刺激性较小。同时建立一种测定D-甘露糖的新方法。
Abstract:
Objective To compare two methods in the determination of mannatide for injection. Methods The contents were determined by spectrophotometry and HPLC method. Results In the samples determined by Spectrophotometric Determination,soluble in phenol solution and sulfuric acid, was detected at wavelength 490 nm, D-mannose derivatives linear concentration range is 10.2-51 μg/ml (r=0.999 1), the average content was 92.14%, the average RSD value was 1.17%. In the HPLC determination, with color spectrum column: Gemini C18 (250 mm×4.6 mm, 5 μm), mobile phase acetonitrile -0.02 mol/L ammonium acetate solution (20:80), flow rate:1 ml/min, the detection wavelength was at 250 nm, column temperature: 30 ℃, sample size: 10 μl detection. The average content ws 83.47%, the average RSD value was 0.65%, the content of two kinds of methods could effectively determine the D-mannose. Conclusion The average content for spectrophotometry was higher, but the phenol was used in detection of special odor, poisonous, corrosive, would cause a certain risk.HPLC was exclusive,chromatogram was more intuitive, on the operator harmfulness and less irritating. A new method for the determination of D-mannose was established at the same time.
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