甘露聚糖肽片剂中氨基酸成分HPLC指纹图谱研究  

Determination of Fingerprint in Mannatide Tablets by Derivation HPLC

作　　者：张轲易 毛跟年[1] 毛瑞娟[1] 吕婧[1] 杜磊[1] 

机构地区：[1]陕西科技大学生命科学与工程学院,陕西西安710021

出　　处：《食品研究与开发》2015年第4期115-119,共5页Food Research and Development

基　　金：陕西省自然科学基金项目(2012JZ3002)

摘　　要：采用HPLC法建立甘露聚糖肽片剂中氨基酸类成分的指纹图谱。选用异硫氰酸苯酯进行柱前衍生,色谱柱为Diamonsil C18柱,采用2种流动相进行梯度洗脱,流动相A为乙腈-水(80∶20),流动相B为0.1 mol/L醋酸钠-乙腈(93∶7,用乙酸调p H至6.4);流速:1.0 m L/min;检测波长:254 nm;柱温:25℃;进样量10μL;分析时间45 min。对来自3厂家共10批甘露聚糖肽片剂建立了氨基酸成分的指纹图谱,发现精密度、重现性、稳定性试验RSD均不大于3%,未水解甘露聚糖肽片剂指纹图谱共有峰9个,水解后共有峰9个,且水解后样品色谱图与对照色谱图之间的相似度相差不大均在0.938以上。研究结果表明,所用方法准确可靠,适用于甘露聚糖肽片剂的质量评价。To set up a fingerprint for amino acid in mannatide tablets by High performance liquid chromatography. The samples were investigated by pre-column derivation with Phenylisothiocyanate. Chromatographic conditions： Separations were performed on a DiamonsilC18 column, Gradient elution was used with two mobile phase. Mobile phase A ： acetonitrile-water （80 ： 20）, mobile phase B ： 0.1mol/L acetate- acetonitrile （93 ： 7, adjust pH to 6.4 with acetic acid） ; flow rate： 1.0 mL/min;detection wavelength：254 nm; column temperature：25 ℃ ;Incoming sample amount：10 μL;time analysis：45 min. The fingerprint of ten samples from different mannatide tablets of three factory was established. The relative standard deviation （RSD） of precision and reproducibility was not more than 3 %. There were 9 common peaks in non-hydrolyzed sample of fingerprint, 9 common peaks in hydrolyzed sample. There was little difference in the similarity between hydrolyzed sample chromatograms and the standard spectrum （similarity above 0.938） . The result showed that the method is accurate, convenient and the chromatographic fingerprints can be served as a tool for the quality evaluation of mannatide tablets.

关 键 词：甘露聚糖肽片剂 氨基酸 高效液相色谱 衍生 指纹图谱 

分 类 号：O657.72[理学—分析化学] TQ464[理学—化学]