| 柱前衍生高效液相色谱法分析海洋褐藻多糖药物的糖醛酸组成 |
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| 引用本文： | 王金霞,赵峡,于广利,李广生,郝翠. 柱前衍生高效液相色谱法分析海洋褐藻多糖药物的糖醛酸组成[J]. 分析化学, 2009, 37(5) |
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| 作者姓名： | 王金霞 赵峡 于广利 李广生 郝翠 |
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| 作者单位： | 中国海洋大学医药学院,教育部海洋药物重点实验室,青岛,266003 |
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| 基金项目： | 国家高技术研究发展计划(863计划) |
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| 摘 要： | 采用三氟乙酸(TFA)分别将藻酸双酯钠(PSS)、甘糖酯(PMS)和古糖酯(PGS)3种海洋褐藻多糖药物进行降解,再与1-苯基-3-甲基-5-吡唑啉酮(PMP)进行柱前衍生,建立了3种药物糖醛酸组成分析的高效液相色谱方法.结果表明:PSS、PMS、PGS的最适降解条件:在110 ℃下降解6 h,TFA浓度3 mol/L;最适衍生条件:反应温度70 ℃,反应90 min,PMP与供试品的摩尔比为12∶ 1,NaOH与供试品的摩尔比为2∶ 1;色谱条件为:0.1 mol/L 磷酸盐(pH 6.7)缓冲液-乙腈(82∶ 18,V/V),检测波长:245 nm,流速:1 mL/min.在此色谱条件下,甘露糖醛酸(M)和古罗糖醛酸(G) 分离良好,测得PSS、PMS、PGS的M/G分别为2.37±0.05、6.60±0 22和0.22±0 03,该方法具有良好的精密度和重现性,灵敏度高,适合于海洋褐藻多糖类药物的微量分析.
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| 关 键 词： | 海洋褐藻多糖 柱前衍生 高效液相色谱法 1-苯基-3-甲基-5-吡唑啉酮 |
Analysis of Uronic Acid Compositions in Marine Brown Alga Polysaccharides by Precolumn Derivatization High Performance Liquid Chromatography |
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| WANG Jin-Xia,ZHAO Xia,YU Guang-Li,LI Guang-Sheng,HAO Cui. Analysis of Uronic Acid Compositions in Marine Brown Alga Polysaccharides by Precolumn Derivatization High Performance Liquid Chromatography[J]. Chinese Journal of Analytical Chemistry, 2009, 37(5) |
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| Authors: | WANG Jin-Xia ZHAO Xia YU Guang-Li LI Guang-Sheng HAO Cui |
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| Affiliation: | Key Laboratory of Marine Drugs;Ministry of Education;School of Medicine and Pharmacy;Ocean University of China;Qingdao 266003 |
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| Abstract: | A high performance liquid chromatography method has been established to determine the uronic acid comopositions of three marine brown alga polysaccharide drugs,namely propylene glycol alginate sodium sulfate(PSS),polymannuronate sulfate(PMS) and polyguluronate sulfate(PGS).This method is based on precolumn derivatization with 1-phenyl-3-methyl-5-pyrazolone(PMP),after three drugs are degraded by trifluoroacetic acid(TFA).The results show that the optimum degradation conditions of PSS,PMS and PGS are as follo... |
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| Keywords: | Marine brown alga polysaccharides precolumn derivatization high performance liquid chro-matography 1-phenyl-3-methyl-5-pyrazolone |
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