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| 高效液相色谱法测定油茶饼粕多糖组成 |
| Determination of polysaccharide composition of oil-tea camellia seed cake by high performance liquid chromatography |
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| DOI：10.12166/j.zgyz.1003-7969/2020.12.024 |
| 中文关键词: 油茶饼粕多糖 单糖 1-苯基-3-甲基-5-吡唑啉酮 柱前衍生 高效液相色谱 |
| 英文关键词:oil-tea camellia seed cake polysaccharide monosaccharide 1-phenyl-3-methyl-5-pyrazolone pre-column derivation high performance liquid chromatography |
| 基金项目:广东省林业科技创新项目（2017 KJCX 003） |
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| 中文摘要: |
| 提出并对比了3种分析油茶饼粕多糖组成的高效液相色谱方法——氨基柱-折光示差检测器法、氨基柱-串级质谱法、1-苯基-3-甲基-5-吡唑啉酮柱前衍生-C18柱-紫外检测器法（柱前衍生法）。综合考虑分离效果、灵敏度、仪器成本等因素，最终选定柱前衍生法。柱前衍生法可同时测定油茶饼粕多糖中的鼠李糖、甘露糖、葡萄糖、半乳糖、木糖、阿拉伯糖、葡萄糖醛酸、半乳糖醛酸，线性关系良好（线性系数>0.99），检出限为0.02~0.29 mg/L，定量限为0.06~0.96 mg/L；单糖及糖醛酸的加标回收率分别为77.2%~111.9%、60.1%~87.0%；峰面积日内精密度为0.08%~3.77%，日间精密度为0.39%~17.15%。利用柱前衍生法检测油茶饼粕多糖样品，结果显示所检的4个样品中均含有5种或6种单糖及2种糖醛酸，且含量最高的组分均为葡萄糖。 |
| 英文摘要: |
| Three high performance liquid chromatography methods for the determination of polysaccharide composition of oil-tea camellia seed cake were put up and compared, which were NH2 column- refractive index detector (RID) method, NH2 column- tandem mass spectrometry (MS/MS) method, 1-phenyl-3-methyl-5-pyrazolone (PMP) pre-column derivation- C18 column- ultra-violet detector (UV) method (pre-column derivation method), respectively. Considering the separation effect, sensitivity, instrument cost and other factors, the pre-column derivation method was selected.The method could be used for determination of rhamnose, mannose, glucose, galactose, xylose, arabinose, glucuronic acid and galacturonic acid simultaneously. The correlation coefficients were higher than 0.99, with limits of detection 0.02-0.29 mg/L and limits of quantification 0.06-0.96 mg/L.The recoveries of standard addition of monosaccharides and uronic acids were 77.2%-111.9% and 60.1%-87.0% respectively. Intra-day relative standard deviations (RSD) of the peak area were 0.08%-377% while inter-day RSD were 0.39%-17.15%.The established method was then applied to detect four polysaccharide samples of oil-tea camellia seed cake. The results showed that all the polysaccharide samples consisted of five or six monosaccharides and two uronic acids, and glucose content was the highest. |
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