海南黎药海巴戟多糖含量测定及其测量不确定度评估

研究和探讨海南黎药海巴戟多糖含量,并对多糖含量测量过程中引入的不确定因素进行评估。采用苯酚-硫酸法测定海巴戟药材中多糖含量,并根据苯酚-硫酸法建立数学模型,找出影响不确定的因素,最终确定测量结果的合成不确定度和扩展不确定度。以D-葡萄糖作为对照品,浓度在0.002 5～0.012 5 g/L范围内线性关系良好(R~2=0.999 4),重现性试验RSD=1.84%,4 h内显色稳定,加样回收率为98.05%(n=9,RSD=2.32%);16批海巴戟药材多糖含量为5.53%～12.63%,其多糖含量测定方法的合成不确定度为0.029 4～0.093 8,扩展不确定度为0.059 0～0.187 6。影响测量不确定度的主要因素有称量、浓度配制和吸光度。本研究建立的海南黎药海巴戟多糖含量测定方法适应性广、灵敏度高,若将测量结果不确定度纳入标准制定有助于对海巴戟药材含量分析方法的建立和质量标准的制定,有利于对海巴戟药材资源的开发。

Polysaccharide content determination and measurement uncertainty evaluation of Morindae Citrifoliae Fructus

The content of polysaccharide was determined with phenol?sulfuric acid method, and the uncertainty factors introduced in the measurement process were also evaluated. The polysaccharide content of Morindae Citritolia Fructus was determined by phenol?sulfuric acid method, the mathematical model has been established according to the phenol sulfuric acid method to find out the factors that affect uncertainty, and the combined uncertainty and extended uncertainty of the measurement result were determined. The result showed that the polysaccharide content of Morindae Citritolia Fructus was a good linear relationship in 0.002 5~0.012 5 g/L (R²=0.999 4), reproducibility test of RSD=1.84%, the color stability in 4 hours, and the recovery rate 98.05% (n=9, RSD=2.32%). The combined uncertainty of the method for determination of polysaccharide in Morindae Citritolia Fructus was 0.029 4~0.093 8, and the extended uncertainty was 0.059 0~0.187 6. The three main factors affecting the uncertainty were weighing, concentration preparation and absorbance. Using phenol?sulfuric acid method, this study established determination method for polysaccharide content of Morindae Citritolia Fructus, and showed wide adaptability and high sensitivity. The uncertainty may be fitted into the standard formulation, which would be helpful to establish the quality standard for the content analysis of Morindae Citritolia Fructus.